1800-8110-OM-R310-2001 Operating Manual - SRU

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1800-8110-OM-R310-2001

SRU UNIT
OPERATING
MANUAL PETRORabigh REV F1

Client’s Name: Rabigh Refining and Petrochemical Company (PETRORABIGH)

Project Title: REFINING PLANTS PROJECT

Project Location: Rabigh, Saudi Arabia

REVISION O1 F1
DATE 22/05/07 27/11/07
ORIG. BY IBM/JJA IBM/JJA
APP. BY JLT JLT
QA REVIEW LPG LPG

Approved for Aramco Sumitomo JV


Signature / Date Name Signature / Date Name

Revision Status
Revision Comment
O1 ISSUED FOR COMMENTS
F1 FINAL ISSUE

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INDEX

1 INTRODUCTION.................................................................................................................................................. 7

2 GLOSSARY............................................................................................................................................................ 8

3 DESIGN AND OPERATING DATA ................................................................................................................. 10

3.1 Basis of Design ................................................................................................................................................. 10


3.1.1 Purpose of the Facilities ................................................................................................................................ 10
3.1.2 Process Overview.......................................................................................................................................... 11
3.1.3 Design Feed Characteristics .......................................................................................................................... 12
3.1.4 Product Specification .................................................................................................................................... 14
3.1.5 Material Balances.......................................................................................................................................... 15
3.1.6 Battery Limit Conditions............................................................................................................................... 16

3.2 General Description......................................................................................................................................... 17


3.2.1 Process Description ....................................................................................................................................... 17
3.2.1.1 Process Chemistry ................................................................................................................................ 17
3.2.2 Description of Unit Flow............................................................................................................................... 20
3.2.2.1 Process Flow Description ..................................................................................................................... 20
3.2.2.2 Operating Conditions............................................................................................................................ 27
3.2.2.3 Effect of Main Process Variables ......................................................................................................... 27
3.2.2.4 Drawings (PFD’s & P&ID’s, Plot Plan)............................................................................................... 34
3.2.2.5 Line Schedule Tables............................................................................................................................ 39
3.2.3 Utilities and Chemicals ................................................................................................................................. 40
3.2.3.1 Utility Consumption Summary............................................................................................................. 40
3.2.3.2 Chemicals and Catalysts....................................................................................................................... 40
3.2.4 Control Systems ............................................................................................................................................ 43
3.2.4.1 Distributed Control System (DCS)....................................................................................................... 43
3.2.4.2 Emergency Shutdown (ESD)................................................................................................................ 45
3.2.4.3 Logic Description for Start-up and Shutdown ...................................................................................... 47
3.2.5 Overview Drawings....................................................................................................................................... 48
3.2.5.1 Electrical One Line Diagrams .............................................................................................................. 48
3.2.5.2 Area Classification Diagrams ............................................................................................................... 48
3.2.5.3 Material Selection Diagrams ................................................................................................................ 48
3.2.6 General HSE Systems and Equipment .......................................................................................................... 49
3.2.6.1 Pressure Relief Devices ........................................................................................................................ 49
3.2.6.2 Fire & Gas Systems .............................................................................................................................. 49
3.2.6.3 Fire Fighting Equipments ..................................................................................................................... 49
3.2.6.4 Material Safety Data Sheets (MSDS) ................................................................................................... 49
3.2.6.5 Operational Safety Issues ..................................................................................................................... 49

3.3 Operating Instructions .................................................................................................................................... 55

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3.3.1 Preparation for Start-up ................................................................................................................................. 55


3.3.2 Start-up Procedure......................................................................................................................................... 62
3.3.2.1 Drying Out and Initial Heating Up ....................................................................................................... 62
3.3.2.2 Handling, storage and loading of Catalyst............................................................................................ 69
3.3.2.3 Treatment of catalyst ............................................................................................................................ 77
3.3.2.4 Heating Up after Shutdown .................................................................................................................. 82
3.3.2.5 Check List and Preparation before Feed Gas Intake............................................................................. 86
3.3.2.6 Feed Gas Intake .................................................................................................................................... 88
3.3.2.7 Taking the SUPERCLAUS® Stage into operation............................................................................... 90
3.3.2.8 Start-up of Sulphur Degassing System ................................................................................................. 91
3.3.3 Normal Operation.......................................................................................................................................... 93
3.3.3.1 Operating Variables and Control .......................................................................................................... 93
3.3.3.2 Ammonium Salt Plugging .................................................................................................................... 99
3.3.3.3 Plugging of Sulphur Locks ................................................................................................................. 100
3.3.3.4 Temperature Runaways ...................................................................................................................... 100
3.3.3.5 Poor Sulphur Recovery....................................................................................................................... 101
3.3.3.6 Pressure Drop ..................................................................................................................................... 102
3.3.3.7 Operational Hazards ........................................................................................................................... 103
3.3.4 Shut-down Procedure .................................................................................................................................. 106
3.3.5 Emergency Shutdown and Restart Procedures............................................................................................ 112
3.3.5.1 Automatic Shutdown (Trip)................................................................................................................ 112
3.3.5.2 Restart after an Automatic Shutdown (Trip) ...................................................................................... 112
3.3.5.3 Critical Areas In Sulphur Recovery Plant Operation.......................................................................... 114
3.3.6 Special Operations....................................................................................................................................... 120
3.3.6.1 Operational procedure for draining sour water pumps ....................................................................... 120
3.3.6.2 Maintenance ....................................................................................................................................... 121
3.3.7 Analytical Requirements ............................................................................................................................. 127

3.4 Equipment and Instrument Lists ................................................................................................................. 128


3.4.1 Equipment List ............................................................................................................................................ 128
3.4.2 Instrument List ............................................................................................................................................ 128

4 OUTLINE FOR INDIVIDUAL MAJOR EQUIPMENT ............................................................................... 129

5 SUPPORT SYSTEMS ....................................................................................................................................... 130

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ANNEX I

1.1 PFD’s AND STREAM DATA


1.2 P&ID’s
1.3 PLOT PLAN
1.4 LINE SCHEDULE

ANNEX II

2.1 UTILITIES SUMMARY

ANNEX III

3.1 DISTRIBUTED CONTROL SYSTEMS (DCS)


3.2 CONTROL NARRATIVE
3.3 CAUSE AND EFFECT DIAGRAM
3.4 EMERGENCY SHUTDOWN (ESD)
3.5 LOGIC DESCRIPTION FOR START-UP AND SHUTDOWN

ANNEX IV

4.1 ELECTRICAL ON-LINE DIAGRAMS


4.2 ELECTRICAL HAZARDOUS CLASSIFICATION AREAS
4.3 MATERIAL SELECTION DIAGRAMS
4.4 FIRE HAZARDOUS CLASSIFICATION AREAS
4.5 EMERGENCY MUSTER AREAS, WINDSOCKS, ESCAPE ROUTES AND SAFETY SHOWERS
DIAGRAMS
4.6 UNDERGROUND PIPING LAYOUT

ANNEX V

5.1 PRESSURE RELIEF DEVICES

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5.2 FIRE AND GAS DETECTION LAYOUTS


5.3 FIRE FIGHTING EQUIPMENT LIST
5.4 MATERIAL SAFETY DATA SHEETS (MSDS)

ANNEX VI

6.1 START-UP FIGURE


6.2 PLANT OPERATING LOG
6.3 ANALITICAL REQUIREMENTS

ANNEX VII

7.1 EQUIPMENT LIST

ANNEX VIII

8.1 INSTRUMENT LIST

ANNEX IX

9.1.- MAIN BURNER (R310-FR-1001/2001)


9.1.1- Purpose of the equipment
9.1.2- Operating Manual

9.2.- REACTION FURNACE (R310-FR-1002/2002)


9.2.1- Purpose of the equipment
9.2.2- Operating Manual

9.3.- THERMAL OXIDISER BURNER (R310-FR-1003/2003)


9.3.1- Purpose of the equipment
9.3.2- Operating Manual

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9.4.- THERMAL OXIDISER (R310-FR-1004/2004)


9.4.1- Purpose of the equipment
9.4.2- Operating Manual

ANNEX X

10.1. WASTE HEAT BOILER (R310-E-1003/2003)


10.1.1- Purpose of the equipment
10.1.2- Operating Manual

10.2.- WASTE HEAT BOILER STEAM DRUM (R310-E-1003D/2003D)


10.2.1- Purpose of the equipment
10.2.2- Operating Manual

ANNEX XI

11.1 SUPPORT SYSTEMS GENERAL

ANNEX XII

12.1 SUPPORT SYSTEMS TELECOMMUNICATIONS

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1 INTRODUCTION
This Operation and Maintenance Manual, prepared by “TÉCNICAS REUNIDAS S.A.” and based in Jacobs
Engineering basic engineering package data, intends to prepare and assist operators for the start-up,
operation, shutdown and maintenance of the Sulphur Recovery Unit at Rabigh Refinery, Saudi Arabia.

This document will allow personnel to operate the plant in an efficient and safe manner as long as smooth
and stable operation is being carried out. Severe or modified guarantee conditions may lead to lack of
accuracy or of applicability in correlations and guidelines stated in this operation manual.

This Manual describes the procedures that are required to start, operate and stop the sulphur recovery
process. The instructions contained herein are presented as a general guide to aid in safe start-up and
operation of the unit. Operating experience will indicate where a procedure should be modified to improve
the performance of the unit.

Descriptions for the Process, the Chemicals and Utilities, the Control Philosophy, the Operating instructions,
the major Equipment and the Health, Safety and Environmental issues, will be given throughout the
following pages.

The SRU consists of two identical trains that shall be operated in the exact same way. Only explanations for
train 1 are compiled in this manual, but they are also applicable to train 2 by simply modifying the tag
numbers for the equipment and instrumentation.

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2 GLOSSARY
BEDD – Basic Engineering Design Data

BFW – Boiler Feed Water

DGA – Di-gycolamine

EIVs: Emergency Isolation Valves

HP- High Pressure

HPU – Hydrogen Production Unit

LP – Low Pressure

MP – Medium Pressure

PFD – Process Flow Diagram

P&ID – Piping and Instrumentation Diagram

PWHT – Postweld Heat Treatment

SAP – Sulfuric Acid Plant

SWS – Sour Water Stripper

SRU- Sulphur Recovery Unit

VDU – Vacuum Distillation Unit

VGO - Vacuum Gas Oil

VGO HDT - Vacuum Gas Oil Hydrotreater

ZVs: Emergency Shutdown Valves

PRECOMMISSIONING - is the period when conformity, non-operational checks and verifications that the
installation conforms to plans, specifications, and drawings, are carried out. It includes the calibration of
instruments, cold-alignment checks of rotating machinery, testing of safety devices, etc. This phase leads to
the project milestone mechanical completion, or ready for commissioning.

COMMISSIONING - is the period in the project when the dynamic verification of the functioning equipment,
the simulated action of control loops and safety systems, and the operational tests are carried out.
Commissioning includes also a variety of activities such as flushing/cleaning and drying-out of piping

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systems, tightness tests, loading of chemicals, desiccants and catalysts, running-in of pumps, turbines, and
compressors, with inert fluid (generally water and Nitrogen).

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3 DESIGN AND OPERATING DATA


3.1 BASIS OF DESIGN

The design intent of the SRU is to recover the sulphur coming from the two Amine regeneration treaters
(ARU 2 and ARU 3) and two Sour Water Strippers (SWS 2 and SWS 3) with a minimum recovery of 99.2%.

The SRU shall consist of two 50% trains each rated at 276 metric tons per day (mtpd). The unit is designed
to have a high on stream factor. The equipment sparing is such that an unscheduled downtime is not
exceeding 1%.

Each sulphur recovery train is able to operate in a stable manner at 40% (98 t/d sulphur inlet) of the design
case based on the feed gasses as specified in section II.A.3.1.

There are two cases that are defined for operation of the SRU, these are:

The design case is Sour Gas Case, that is the gas from the ARU2, ARU3, SWS2 and SWS3.

The Turndown Case, that is 20% of the gas from ARU2, ARU3, SWS2 and SWS3 for one sulphur recovery
train.

3.1.1 Purpose of the Facilities

A new Sulphur Recovery Unit is required for the PetroRabigh Project. The purpose of this Unit is to convert
the Hydrogen Sulfide produced from the ARU and the SWS into elemental sulphur and thermally
decompose ammonia from the SWSU. The sulphur produced in these facilities is in its liquid state. It is
thereafter sent to a Sulphur Forming Unit where it is cooled to form solid pastilles and loaded into trucks.

The Unit will process a high ammonia content, sour water stripper acid gas. An important feature will be the
ability to destroy all the ammonia in the feed and thereby to eliminate formation and deposition of
ammonium salts.

The process design for the SRU is included in the Jacobs Engineering Licensor’s package.

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3.1.2 Process Overview

In the SRU2, sour gases coming from Amine Regeneration 2&3 units and Sour Water Stripping 2&3 units,
are routed to two Knock Out drums. Amine acid gas is then heated and mixed with the Sour Water Stripper
gas and then the process gas feed is sent to the reactor furnace, where the thermal stage occurs. In this
thermal stage the H2S is partially burnt with air in a reaction furnace burner. The heat from this combustion
is used to produce High Pressure Steam, which may be used in this one unit to preheat the process
streams before entering each step of the catalytic stage.

When the thermal stage has been already carried out, some elemental sulphur has been generated. In
order to separate this sulphur, process gas is conducted to a condenser in which, liquid sulphur is
withdrawn from the process gas and LP steam is generated.

The thermal stage is followed by two catalytic Claus stages, a catalytic Euroclaus® stage and a catalytic
Superclaus® stage. Before entering each one of the four converters, process gas is reheated to reach
optimum temperature for the catalytic conversion of hydrogen sulfide. The tail gas from the last condenser
is conducted to a coalescer in order to eliminate possible liquid sulphur droplets.

The elemental sulphur that has been generated in each converter is then routed to a condenser in which
Sulphur is removed from the gas stream by cooling. The liquid sulphur withdrawn in the four condensers
and the coalescer is collected in the sulphur pit, where sulphur is first cooled to reach the appropriate
viscosity. After that, it passes through the degassing section to eliminate the occluded gases in the liquid
mass.

The tail gas from the coalescer, from the degassing section and from the venting of the sulphur pit is routed
to the thermal oxidiser to eliminate polluting gasses before discharging them to atmosphere. Flue gas
release is carried out through a dedicated stack, which is common to the two trains.

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3.1.3 Design Feed Characteristics

Feestock
Flow rate, composition and battery limit conditions are as follows:

(Note 5) ARU2 ARU3 SWS2 SWS3


Composition (mol.%)
H2S 94.76 2.97 38.45 66.9
N2 - - - -
SO2 - - - -
2)
CO2 - 91.28 - -
NH3 - - 40.15 9.366
H2 0.164 - - -
C1 0.033 0.1 - -
C2 0.009 0.48 - -
C3 0.004 0.1 - -
C4 0.001 - - -
C5+ trace - - -
H2O 5.02 5.05 21.4 23.73
DGA - trace - -

Total 100 100 100 100


Flow kmol/h 615.1 62.8 132 0.57
Average
MW 33.2 42.3 23.8 28.67
Battery Limit Conditions
Pressure kg/cm2g 0.8 0.8 0.8 0.8
Notes

1. Deleted.
2. ARU3 CO2 content is a maximum value.
3. Temperature and pressure are at SRU battery limit.
4. Deleted.
5. Data showed based in latest Heat & Material Balances for units ARU2, ARU3, SWS2 and SWS3
supplied by Shaw Stone & Webster Limited, 1800-8110-DS-R291-0034, 1800-8110-DS-R291-0035, 1800-
8110-21-R301-0001, 1800-8110-21-R302-0001, respectively.

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Vent streams to Thermal Incinerator

The vent gasses coming from the SWS degassing drums is routed to the Thermal Incinerator.
Compositions, flow rate and battery limit conditions are as follows:

(Note 1) SWS2 vent gas SWS3 vent gas


Composition (mol %)
H2S 0.03 2.41
N2 - -
SO2 - -
CO2 - -
NH3 - -
H2 - -
C1 9.09 35.08
C2 56.74 20.72
C3 9.05 12.74
C4 6.39 10.33
C5 1.29 8.28
C6 0.93 -
H2O 16.48 10.43
DGA trace -
Phenol - trace

Total 100 100


Flow kmol/h 7.42 4.82
Average MW 30.94 31.11
Battery Limit Conditions
Pressure kg/cm2g 0.15 0.15
Temperature °C 65.5 53.9

Data showed based in latest Heat & Material Balances for units ARU2, ARU3, SWS2 and SWS3 supplied
by Shaw Stone & Webster Limited, 1800-8110-21-R301-0001, 1800-8110-21-R302-0001, respectively.

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3.1.4 Product Specification

Liquid Sulphur
The product sulphur will have the following specification:

Specification Required limit


Purity (dry basis) 99.8 wt.% min.
Appearance (as solid) Bright Yellow
Carbon 500 ppm wt. max.
H2S in liquid sulphur 10 ppm wt. max
Ash 500 ppm wt. max.
Arsenic 0.25 ppm wt. max.
Tellurium 1 ppm wt. max.
Selenium 1 ppm wt. max.

Condensate
Condensate is produced by the preheaters, reheaters and plant heating system of the unit and is send to
the unit battery limit.

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3.1.5 Material Balances

The material balance for the “Sour Design Case” is included in the Process Flow Diagrams. For the “Design
Case” and 40% Turndown Case”, refer to the following documents from Jacobs Basic Engineering:

Maximum Design Case: 1613-8110-PD-R310-0004 rev A1

Turndown Case: 1613-8110-PD-R310-0005 rev A1

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3.1.6 Battery Limit Conditions

The operating and design conditions for the process streams (as stated in the Process Design Basis) are as
follows. Operating conditions relate to Maximum Design Case throughput. The conditions of feeds and
products are at grade at the SRU battery limit.

Operating
Operating
System Pressure
Temperature (°C)
(kg/cm2g )
Amine acid gas condensate to ARU2 as produced 7.3
Amine acid gas condensate to ARU3 as produced 7.3
SWS gas condensate to SWS2 as produced 4.5
SWS gas condensate to SWS3 as produced 4.5
Cooled blowdown 60 2.15
Liquid sulphur 135 - 150 10.5
Steam condensate to plant utility system 95 – 100 6

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3.2 GENERAL DESCRIPTION

3.2.1 Process Description

3.2.1.1 Process Chemistry

Thermal Stage
The applied sulphur recovery process, known as the EUROCLAUS® process, is based upon the partial
combustion of hydrogen sulphide (H2S) with a ratio-controlled flow of air. The air flow is maintained
automatically to accomplish the complete oxidation of all hydrocarbons and ammonia present in the acid
gas feed, and to obtain an H2S percentage of 0.6 vol.% at the outlet of the third reactor (EUROCLAUS®
reactor).

In the conventional Claus process the 'air - to - acid gas ratio' is maintained to produce an H2S - to - SO2
ratio of exactly 2/1 in the catalytic effluent gases. This is the optimum ratio of H2S - to - SO2 for the Claus
reaction. The EUROCLAUS® process operates according to a different philosophy. In this process the 'air -
to - acid gas' ratio is adjusted to achieve an H2S concentration at the inlet of the fourth reactor
(SUPERCLAUS® reactor). In order to accommodate this requirement, the front-end combustion step is
operated off-Claus-ratio (higher than H2S - to - SO2 = 2/1).

In other words, the front-end combustion step is operated on H2S control rather than the customary
'H2S/SO2' ratio control. A process gas analyser measures the H2S concentration in the effluent gas stream
from the EUROCLAUS® reactor. The analyser controller corrects the air flow to the main burner to achieve
the desired H2S concentration at this point in the process.

From an overview standpoint, the control philosophy may be summarized as:

If the H2S concentration entering the SUPERCLAUS® reactor is too high, more air is supplied to the main
burner, or

1. If the H2S concentration entering the SUPERCLAUS® reactor is too low, less air is supplied to the
main burner.
The main
reaction in the main burner and reaction furnace is:

3
H2 S + O 2 → SO 2 + H2 O + heat
2

The major percentage of the residual H2S combines with the SO2 to form sulphur, according to equilibrium
reaction:

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3
2H 2 S + SO 2 ↔ S 2 + 2H2 O - heat
2

By this reaction, known as the Claus reaction, sulphur is formed in vapour phase in the main burner and
reaction furnace.

Catalytic Claus Stage

The downstream catalytic reaction stage further increases the overall conversion to sulphur. In the first and
second reactor the following reaction takes place:

2 H2S + SO2 ↔ 3/x Sx + 2 H2O + heat

The Claus equilibrium is shifted to the sulphur side by making use of a Claus catalyst. Condensation and
removal of sulphur after the first and second reactor enables further conversion of sulphur in the next
catalytic stage.

EUROCLAUS® Stage
The process gas from the first and second reactor contains SO2 as the Claus reaction equilibrium does not
fully shift to the sulphur side. As SO2 does not react in the final SUPERCLAUS® stage, the SO2 represents
a loss of recovery. Therefore, the SO2 has to be converted to H2S for conversion to sulphur in the
SUPERCLAUS® stage. This is achieved by the catalytic reduction of SO2 in the EUROCLAUS® reactor.
The SO2 is reduced to sulphur vapour and H2S by reaction with H2 and CO over the EUROCLAUS®
catalyst. The H2 and CO are already present in the Claus process gas and react with SO2 according to the
following reactions:

SO2 + 2 H2 → 1/x Sx + 2 H2O


SO2 + 3 H2 → H2S + 2 H2O

SO2 + 2 CO → 1/x Sx + 2 CO2

SUPERCLAUS® Stage
The The process gas from the EUROCLAUS® reactor is mixed with air. In the selective oxidation reactor
(or SUPERCLAUS® reactor), a special catalyst for selective oxidation of H2S to elemental sulphur is
applied. The following reaction takes place:

H2S + 0.5 O2 → 1/x Sx + H2O

This reaction is thermodynamically complete and therefore high conversion levels to elemental sulphur can
be obtained.

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Sulphur Degassing Process


The sulphur produced in the SRU contains about 300 ppm wt H2S, partly chemically bound as
polysulphides (H2Sx) and partly physically dissolved. To remove H2S and H2Sx from liquid sulphur,
eliminating potential toxic and explosion hazard associated with handling, transport and storage of liquid
sulphur, the ‘Shell Sulphur Degassing Process’ has been developed. Degasification by means of the Shell
degassing process reduces the H2S content to less than 10 ppm wt.

Degasification is obtained by injecting air via spargers in the liquid sulphur, thereby partly stripping the
dissolved H2S from the sulphur and partly oxidizing it to elemental sulphur. Furthermore, the removal of H2S
from the sulphur promotes the decomposition of the polysulphides into H2S and sulphur.

H2Sx → H2S + Sx-1

H2S + ½ O2 → 1/x Sx + H2O

Thermal Oxidiser
The tail gas resulting from the SUPERCLAUS® stage and vent gas from the sulphur degassing still
contains traces of sulphur compounds. These sulphur compounds are oxidized in the thermal oxidiser at
elevated temperatures. The main reactions are:

H2S + 3/2 O2 → SO2 + H2O

1/x Sx + O2 → SO2

COS + 3/2 O2 → SO2 + CO2

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3.2.2 Description of Unit Flow

3.2.2.1 Process Flow Description

The sulphur recovery unit SRU 2 consists of two identical trains, Train 1 and Train 2 each with its own
dedicated equipment. The Main air blower and stack are common for both trains. This section describes
only train 1, since both trains are identical.

Feed Gas

Feed gas to the SRU consists of two different streams:

Amine feed gas from ARU 2,3

SWS feed gas from SWS 2,3

Each feed gas has its own knock-out drum. In the Knock-out Drums the entrained water is separated from
the feed gases. The sour water is intermittently pumped to the originating ARU or SWS.

The amine feed gas is preheated to 230°C before it is combined with the SWS feed gas stream after which
the combined feed gas is routed to the Main Burner FR-1001.

Thermal Stage

Main Air Blower K-0001A/B/C supplies the air to the main burner. The main air blower also supplies air to
the SUPERCLAUS® stage and the sulphur degassing system. There is a common stand by blower for both
trains. The air to the main burner is heated by the Air Preheater E-1002 to 230°C to get a temperature
(1250°C) high enough for NH3 destruction in the reaction furnace. Eventually also fuel gas will be co-fired
in the main burner to reach this temperature. The air to the main burner is exactly sufficient to accomplish
the complete oxidation of all hydrocarbons and ammonia present in the feed gases and to burn as much
H2S as required to obtain a 0.6 %vol. H2S at the outlet of the EUROCLAUS® reactor.

The combustion air to the main burner is controlled by the Advanced Burner Control system (ABC system).
This system consists of two parts: a feed forward and a feed back part. Reference is made to the control
description, doc. no. 1613-8120-PD-R310-0001.

The required quantity of air is calculated by measuring the amine feed gas flow, the SWS feed gas flow and
fuel gas flow and multiplying each flow with its own individual air demand (feed forward control). This results
in a total air demand and this signal sets the flow control system in the air supply. The flow control system
adjusts the position of two control valves.

The system adjusts immediately a small control valve in the trim air line, after which the bigger main valve
follows with a delay. The final situation is that the flow through the control valve in the trim air line is again in

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the optimum of its range to cope quickly with flow changes. Then the total air flow through the main air and
the trim air lines corresponds with the total amount of acid gas feed.

The flow control system is also adjusted by the H2S analyser controller (feed back control) located in the
process line upstream of the SUPERCLAUS® reactor stage. It ensures the required H2S content in the
process gas, in order to obtain the optimum sulphur recovery efficiency of the unit.

The combustion temperature has to be sufficiently high (1250°C minimum) to obtain a proper destruction of
NH3. The feed gas does not contain sufficient combustibles to obtain this temperature. Therefore preheating
of the acid gas and air by HP steam is required. When even with preheating this temperature is not met,
fuel gas has to be co-fired in the main burner. The fuel gas supplied at the battery limit has a certain
composition range, which can vary during operation. Therefore, a fuel gas analyser is provided to measure
the fuel gas composition to be sure that always the correct amount of air is supplied for burning the fuel gas.

To remove the heat generated in the main burner, the gas passes through the tube bundle located in Waste
Heat Boiler E-1003. The gas is cooled, thereby generating saturated high pressure steam, which is
collected in Waste Heat Boiler Steam Drum E-1003-D, which is a part of the waste heat boiler. The high-
pressure steam is partly supplied to the reheaters and preheaters. The surplus is let down in pressure and
routed to the refinery LP steam system. Boiler feed water is introduced to the steam drum of the waste heat
boiler on level control.

The process gas is cooled further in the First Sulphur Condenser E-1004. The sulphur vapour in the
process gas is condensed and separated from the gas. Liquid sulphur from the first sulphur condenser is
directed to the Sulphur Pit TK-1001 via its Sulphur Seal D-1005A. A demister pad is installed in the outlet
channel of the first sulphur condenser to recover liquid sulphur, entrained as mist with the process gas.

In the sulphur condenser low pressure steam is generated.

Claus Stage
The gas stream from the first sulphur condenser is heated again in the First Reheater E-1005, to obtain the
optimum temperature for the catalytic conversion in the First Claus Reactor R-1001. The first Claus reactor
contains a top layer of alumina oxide type catalyst and a bottom layer of titanium oxide catalyst to obtain a
high COS and CS2 conversion in the bottom the bed. The steam flow to the first reheater is adjusted by a
temperature controller at the inlet of the reactor.

In the reactor, the H2S and SO2 in the process gas react over the catalyst until equilibrium is reached. The
inlet temperature of the reactor is maintained at 240°C to favour COS and CS2 conversion. The process gas
from the reactor passes into the Second Sulphur Condenser E-1006, is cooled and the sulphur in the gas is
condensed and separated from the gas. Liquid sulphur from the second sulphur condenser is directed to
the sulphur pit via its Sulphur Seal D-1005B. A demister pad is installed in the outlet channel of the second
sulphur condenser to recover liquid sulphur, entrained as mist with the process gas. Like in the first sulphur

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condenser low pressure steam is generated.

The first and second sulphur condensers are combined in one shell. Boiler feed water is introduced to the
shell side of the condensers on level control. The condensers generate low pressure steam which is used
for plant heating, the surplus is exported to the refinery steam network.

The gas stream from the second sulphur condenser is heated again in the Second Reheater E-1007, to
obtain the optimum temperature (210°C) for the catalytic conversion in the Second Claus Reactor R-1002,
which contains an alumina oxide type catalyst. The steam flow to the second reheater is adjusted by a
temperature controller at the inlet of the reactor. The inlet temperature is lower than in the first reactor to
promote a high conversion of H2S and SO2 into sulphur.

In the reactor, the H2S and SO2 in the process gas react over the catalyst until equilibrium is reached. The
process gas from the reactor passes into the Third Sulphur Condenser E-1008, is cooled and the sulphur in
the gas is condensed and separated from the gas. Liquid sulphur from the third sulphur condenser is
directed to the sulphur pit via its Sulphur Seal D-1005C. A demister pad is installed in the outlet channel of
the third sulphur condenser to recover liquid sulphur, entrained as mist with the process gas.

EUROCLAUS® Stage
The gas stream from the third sulphur condenser is heated again in the Third Reheater E-1009, to obtain
the optimum temperature (195°C) for the catalytic conversion in the EUROCLAUS® Reactor R-1003.

This reactor contains three different types of catalyst. The top layer consists of alumina oxide type catalyst
to promote a conversion of H2S and SO2 into sulphur. As the final SUPERCLAUS® stage does not convert
components other than H2S, these components present a loss of recovery when routed to the
SUPERCLAUS® stage. Therefore the second layer is the EUROCLAUS® catalyst, a hydrogenation
catalyst. This catalyst reduces SO2 to H2S and sulphur vapour. Finally, the bottom layer consists of titanium
oxide catalyst to hydrolyse undesired components as COS.

The steam flow to the third reheater is adjusted by a temperature controller at the inlet of the reactor; the
inlet temperature is lower than in the first two reactors to promote a high conversion of H2S and SO2 into
sulphur.

The process gas from the EUROCLAUS® reactor passes to the Fourth Sulphur Condenser E-1010, is
cooled and sulphur in the gas is condensed and separated from the gas. Liquid sulphur is directed to the
sulphur pit via its Sulphur Seal D-1005D. A demister pad is installed in the outlet channel of the fourth
sulphur condenser to recover liquid sulphur, entrained as mist with the process gas.

The third and fourth sulphur condensers are combined in one shell. Boiler feed water is introduced to the
shell side of the condensers on level control. The condensers generate low pressure steam which is used
for plant heating and the surplus is exported to the refinery steam network.

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SUPERCLAUS® Stage
To obtain a high sulphur recovery the process gas is passed to the 4th and final catalytic stage, the
SUPERCLAUS® stage. Preheated air supplied by the main air blower is injected into the process gas
upstream of the Fourth Reheater E-1011. The process gas is heated in the fourth reheater, to obtain the
optimum temperature (200°C – 210°C) for the catalytic conversion in the SUPERCLAUS® Reactor R-1004.
The steam flow to the fourth reheater is adjusted by a temperature controller at the inlet of the reactor.

H2S is selectively oxidized into sulphur in the SUPERCLAUS® reactor. The reactor contains a special
selective oxidation catalyst. The air is supplied in excess in order to maintain oxidizing conditions in the
reactor to prevent sulphiding of the catalyst. Therefore, the air supply is flow controlled. The set point of the
flow controller is determined by the relative load of the unit (based on calculated air demand for main
burner), the reaction stoichiometry, the excess of oxygen and the H2S concentration in the tail gas upstream
the SUPERCLAUS® stage.

The gas from the SUPERCLAUS® Reactor passes to the Fifth Sulphur Condenser E-1012. In order to
condense as much sulphur as possible the fifth sulphur condenser operates at a low temperature. This is
obtained by generating steam at low pressure of around 2 kg/cm2 (abs). The steam is condensed in Steam
Condenser E-1013 by means of an air cooler. The steam pressure is maintained by a pressure controller
adjusting the speed and pitch of the air fans to the steam condenser. The pressure of 2 kg/cm2 (abs)
corresponds with a steam temperature of 120°C, which is slightly above the solidification temperature of the
sulphur. The control system ensures a safe margin above the sulphur solidification temperature.

The liquid sulphur from the fifth sulphur condenser is sent to the sulphur pit via its Sulphur Seal D-1005E. A
demister pad is installed in the outlet channel of the fifth sulphur condenser to recover liquid sulphur,
entrained as mist with the process gas.

The process gas flows from the fifth sulphur condenser into the downstream Coalescer D-1006, provided
with a demister pad, in which the last traces of liquid sulphur are separated from the gas and the liquid
sulphur is sent to the sulphur pit via its Sulphur Seal D-1005F.

In case of malfunctioning, the SUPERCLAUS® stage can be bypassed without taking the Claus and
EUROCLAUS® sections out of operation. In this case the process gas from the third reactor is routed via
the SUPERCLAUS® bypass to the Thermal Oxidiser FR-1004.

Sulphur Degassing
The liquid sulphur from the condensers is first cooled in the Sulphur Cooler E-1016 which is installed in the
sulphur pit.

The sulphur as it is produced in the sulphur recovery train contains about 300 ppm wt H2S. Sulphur
stripping has been incorporated to reduce the H2S content to less than 10 ppm wt. It takes place in the
stripping section of the sulphur pit.

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Two bubble columns Z-1001A/B are located in the stripping section. They are identical and have a
rectangular cross section. The top and bottom parts are open. Air distribution spargers are provided at their
bottom sides.

The stripping air to the spargers is supplied by the main air blower. The function of the air is to obtain forced
sulphur circulation in and around the bubble columns, to strip the dissolved hydrogen sulphide from the
liquid sulphur and to oxidize the major part of the H2S to sulphur. Furthermore, the removal of H2S from the
sulphur promotes the decomposition of polysulphides into dissolved H2S and sulphur. In this way, sulphur
with a H2S content of less than 10 ppm wt is obtained.

Besides the stripping air, an additional amount of sweep air is added via the air inlets, located on the cover
of the degassing section. The sweep air is preheated by means of low pressure steam. The total air,
together with the H2S released from the sulphur, is drawn off by steam driven Steam Ejector EJ-1001A/B.

The off-gas from the sulphur pit is discharged to the thermal oxidiser.

The sulphur level in the stripping section is kept constant by means of an overflow weir between the
stripping compartment and the downstream storage compartment. The degassed sulphur is pumped by the
Sulphur Pump P-1006A/B from the storage compartment to the solidification unit.

The storage compartment of the pit can contain 5 days sulphur production. The pump is automatically
stopped when the level drops too much.

Both parts of the pit are equipped with steam coils to maintain the temperature of the sulphur.

Thermal Oxidiser
The SUPERCLAUS® tail gas (or in case of bypass operation, the EUROCLAUS® tail gas) and the vent gas
from the sulphur pit contain residual H2S and other sulphur compounds, which cannot be released directly
to the atmosphere. These gases are therefore thermally oxidised in thermal oxidiser to convert residual H2S
and sulphur compounds into SO2. Additionally the vent gasses from the SWS buffer tanks are also fed to
the thermal oxidizer.

The gases to be oxidised are heated by mixing with hot flue gas, obtained by combustion of fuel gas in
Thermal Oxidiser Burner FR-1003.

The fuel gas flow to the burner is adjusted by control of the temperature in the flue gas leaving the
incinerator. The combustion air for the fuel gas is provided by the Thermal Oxidiser Air Blower K-1002A/B.

The air supply to the thermal oxidiser is divided in three stages:

1. Primary air used for substoichiometric combustion of fuel gas


2. Staged air for supply of air to the flue gas from the burner to obtain overstoichiometric combustion
of the fuel gas.
3. Secondary air for combustion (oxidation) of the process gas

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The primary air flow is ratio controlled by the fuel gas flow. The resulting primary air flow rate is 80% of the
amount required for stoichiometric combustion of the fuel gas. This reduces the formation of NOx in the
burner.

The staged air flow is also ratio controlled by the fuel gas and amounts to 30% of the air flow rate required
for stoichiometric combustion of the fuel gas.

An oxygen analyser is situated in the oxidiser flue gas and is provided with an oxygen controller. The signal
from the oxygen controller is the setpoint of the flow controller of the secondary air. The staged air flow and
secondary air flow rates are therefore adequate to supply sufficient oxygen to burn the un-burnt fuel gas
and to incinerate the combustibles in the process gas. It results in an oxygen excess of 2.1 vol.% in the
incinerator flue gas. The oxygen excess ensures that the flue gas contains less than 10 ppm vol. H2S.
Finally, the incinerator flue gas is routed to the common Stack SK-0001.

When maintenance works have to be carried out in one train while the other one is in operation, the manual
sliding valve that connects the thermal oxidiser (FR-1004 / FR-2004) to the stack SK-0001 shall be closed,
ensuring a hermetic isolation. Besides the isolation provided by the sliding valve, the stack draft ensures
that the gas flows through the stack and not towards the thermal oxidiser, avoiding the entrance of gases in
the train under maintenance works.

Before carrying out maintenance works, the following steps shall be carried out:

1. Shut down the train that needs to be repaired. Maintain the thermal oxidiser in operation by
feeding air from the blower and fuel gas. Make sure that all other connections to the
thermal oxidiser are closed (especially important is closing line SWS VENT GAS FROM
SWS3, SWS2).

2. Take a sample from sample connexion/ analyser and make sure that there is no H2S.

3. Shut down the burners of the thermal oxidiser and flow only air until cooling down.

4. Stop the blower.

5. Close the manual sliding valve to isolate the train that has to be repaired

6. Take a sample from sample connexion/ analyser and make sure that there is no H2S.

7. Open the man way.

After the train is well isolated, maintenance works can be carried out in one train, while the other one is in
operation. When works are finished, the sliding valve shall be opened again and both trains will be
connected to the stack.

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UTILITY SYSTEMS

High Pressure (HS) Steam

Saturated HS steam is generated in the waste heat boiler. It is utilized as heating medium for the air and
feed gas preheaters and the steam reheaters. Surplus HS steam is let down in pressure and submitted to
the LP steam system.

During startup and shutdown when the waste heat boiler produces insufficient HS steam it might be
necessary to import HS steam from the refinery system to supply steam to the reheaters.

Low Pressure (LS) Steam

Saturated LS steam is generated in the sulphur condensers and used for plant heating (e.g. for degassing,
tracing/jacketing of pipelines). The remainder is discharged into the LS steam system.

During hot standby LS steam is supplied to the main burner for cooling of the fuel gas flame, as air cooling
is not allowed under these circumstances.

Discontinuous steam purges may be required as smothering medium during a temperature run-away in the
sulphur pit.

When the equipment in the unit is cold (below 100°C), steam should not be introduced into the main burner,
neither for cooling nor for purging.

Boiler feed water

Boiler feed water is supplied to the waste heat boiler and the sulphur condensers, high pressure boiler feed
water is used for the waste heat boiler and medium pressure boiler feed water is used for the condensers.

Fuel gas

Fuel gas is fired in the thermal oxidiser burner. During startup, hot standby and shutdown or in the case that
the flame temperature is lower then 1250°C, like in the design case, it is also supplied to the main burner.

Nitrogen

A continuous small nitrogen purge is required for the flame scanners, sight glasses and pyrometer of the
main burner and the relief line of the SWS gas knock out drum. During startup it is also used for purging the
main burner and the reaction furnace.

Condensate recovery

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All the steam used for heating within the plant shall be recovered. Each item is first routed to a steam trap,
to take care of the correct conditions within the item where the heating takes place.

HS steam condensate and LS steam condensate are routed to the Condensate Flash Drum D-1007. Here
the condensate is completely flashed to almost atmospheric pressure. The steam is condensed by the
Flash Steam Condenser

E-1015 and drained back to the flash drum. The condensate water is pumped by Steam Condensate Pump
P-1005A/B on level control to the plant utility system.

Blow down recovery

The blow down of the waste heat boiler and the sulphur condensers is recovered. The blow down is routed
to the Blow Down Drum D-1004, where it is completely flashed to atmospheric pressure. The blow down
water is pumped to the battery limit by Blow Down Pump P-1004A/B. Downstream the pump an air cooler
cools the blow down water to approx. 60°C. A part of the cooled blow down water is recycled to the top of
the blow down drum to surpress the steam plume coming from the flashing blow down.

3.2.2.2 Operating Conditions

For detailed information about operating conditions, refer to Process Flow Diagrams (1800-8110-20-R310-
0189, 0190, 0191, 0192, 0193 and 1800-8110-21-R310-0194S1, 0194S2, 0195S1, 0195S2) included in
Section II.B.2.d.

3.2.2.3 Effect of Main Process Variables

The main process variables and the deviations that may lead to significant effects in the process successful
completion, are to be described subsequently. The information is presented separately for each of the main
piece of equipment. For the Claus Reaction Area the main variables to consider are temperature and
oxygen concentration. Pressure is not to be included as long as it is not a critical variable in Claus process
performance.

Main Burner (R310-FR-1001)

Temperature in the Main Burner is an important issue, as long as it may affect the performance of the
downstream equipment.

It is imperative that the combustion temperature in the main burner is at least, 1250 ºC to destroy the NH3
present in the Sour Water Stripper acid gas. If this figure is not accomplished, incomplete conversion of
ammonia will occur, causing plugging of lines and downstream equipment by ammonium salts on the
coldest spots. For proper ammonia conversion, it is also desirable that a good residence time is obtained in
the main burner.

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When the feed gas contains not sufficient combustibles to maintain the required flame temperature,
additional heat is supplied. This is obtained by preheating both the air and the amine gas feed. The feed
gas preheater will also be maintained in operation when no SWS feed gas is supplied to avoid water
condensation in the acid gas feed line. If due to shortage of combustibles in the feed gas the temperature
tends to drop below 1250°C with the heaters on, fuel gas should be co-fired in the main burner.

If the oxygen concentration in the process gas mixture is too low, combustion of H2S in the thermal stage
may be insufficient, increasing the hydrogen sulfide that reaches the Superclaus catalyst. In this case,
because of the thermodynamics for Superclaus main reaction, there may be a temperature runaway in the
bed, resulting in possible catalyst damage.

A major deficiency of air at fuel gas firing might result in deposition of soot on the first catalyst bed resulting
in a higher pressure drop and less sulphur conversion.

When the unit is still hot, an air excess might lead to equipment damage due to fire inside de equipment. It
might also cause sulphation of the Claus catalyst in the 2nd reactor resulting in less sulphur conversion.

1st and 2nd Claus Reactors (R310-R-1001/R-1002)

When the reactor inlet temperatures are according to the design values the conversion to sulphur is
maximum.

At a lower inlet temperature of the first reactor, consequently the outlet temperature is also lower. It may be
less than 300°C, which leads to insufficient conversion of COS and CS2. This is not recovered in the
downstream part of the unit and results in an increased SO2 emission from the stack.

At a lower inlet temperature of the second and third reactors, sulphur vapour may condense on the catalyst
beds, resulting in reduced catalyst activity. At higher temperatures, less H2S is converted as the equilibrium
shifts to H2S and SO2.

At high throughput, the reactor inlet temperatures are 240°C, 210°C and 195°C, respectively. When the unit
operates at low throughput (below 40% of design), it is advised to increase the inlet temperature of the
second and third reactor by 10°C, to compensate for heat losses. This prevents sulphur condensation on
the catalyst beds. The reactor inlet temperatures are automatically controlled: the controllers adjust control
valves in the steam supply lines to the reheaters.

The difference between the inlet and bottom temperature of the reactor is a measure for the conversion rate
in the catalyst bed.

As soon as a decline in temperature difference across the second and third reactor becomes noticeable
from the daily operating figures, the inlet temperature should be temporarily increased. In this way
condensed sulphur is evaporated from the catalyst bed. It is pointed out that condensation of sulphur on the
catalyst is the most likely reason for deterioration of the catalyst.

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At high temperatures and high partial pressure of oxygen, SO2, Alumina (present in the catalyst) and
oxygen (whether it is present or not) might interact together causing aging in the catalyst by superficial
sulfates formation (sulfation). This situation leads to a decrease in sulphur recovery. This process usually
occurs during shut-down operation.

In case the H2S concentration in the process gas leaving this converter increases above 1.5% vol. the
temperature in the third converter can reach so high that the catalyst may be damaged

Euroclaus® Reactor (R310-R-1003)

A low inlet temperature in the 3rd reactor will lead to a lower reactor outlet temperature. A low reactor
temperature will give insufficient conversion of SO2 in the reactor. A high inlet temperature in the reactor will
lead to a higher reactor outlet temperature. The outlet temperature should not be allowed to exceed 250°C

as above this temperature the main reversible reaction shifts (


S + O2 → SO2 ). This leads to a decrease in
sulphur production as less SO2 is converted and sulphur is converted to H2S.

Once in the EUROCLAUS® reactor off-gas, the sulphur associated with the SO2 cannot be recovered and
part of the sulphur transformed into H2S will also not be recovered. The difference in between the inlet and
bottom temperature of the EUROCLAUS® reactor is a measure for the conversion rate in the catalyst bed.

As soon as a decline in temperature difference across the reactor becomes noticeable from the daily
operating figures, the inlet temperature should be temporarily increased (at least 24 hours). In this way
condensed sulphur is evaporated from the catalyst bed. It is pointed out that condensation of sulphur on the
catalyst is the most likely reason for deterioration of the catalyst (see 3.3.2.3)

At high throughput, the reactor inlet temperature is 195°C. When the unit operates at low throughput (below
40% of design), it is recommended that the reactor inlet temperature will be increased by 10°C to
compensate for increased heat losses to obtain a safe dew point margin. This prevents sulphur
condensation on the bed.

Superclaus® Reactor (R310-R-1004)

The SUPERCLAUS® reactor inlet temperature is controlled similarly to the other reactor stages.

At high throughput the SUPERCLAUS® reactor inlet temperature is 210°C, maximum 220°C. The reactor
outlet temperature should however not exceed 280°C. Above this temperature the sulphur yield decreases
due to an increase in SO2 formation. This is shown in figure 1.

It is imperative to maintain oxidizing conditions to prevent sulfiding of the catalyst, which would decrease
the sulphur yield. Therefore, the oxidation air control system has been designed to maintain an excess of
oxygen in the reactor. In this way the catalyst is protected against reduction of the iron oxide. The intent of
the control system for the oxidation air is to maintain an oxidizing environment on the SUPERCLAUS®

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catalyst, to ensure the maximum conversion of H2S to sulphur and to prevent consecutive oxidation of
sulphur to SO2.

The two feed gas flows to the main burner are measured and used to calculate the relative load of the unit.

The H2S concentration in the EUROCLAUS® tail gas is measured by the tail gas analyser and this
measurement, together with the relative load are used to calculate the required oxidation air flow. Since the
tail gas flow has some time lag with respect to the incoming flow, the calculated oxidation air flow is delayed
by a lag block. The calculated oxidation air flow is used as the set point of the oxidation air flow controller.
This flow controller is provided with minimum set point limit and minimum output limit to prevent a too low
concentration of oxygen downstream the SUPERCLAUS® reactor.

In this way the oxygen content in the process gas leaving the SUPERCLAUS® reactor stage is kept at
0.5 vol.%. Only at low throughput the oxygen content increases as the minimum stop in the controller output
overrules the actions of the control system.

Remarks
In contrast with the Claus reactors, no sulphur is absorbed in the pores of the SUPERCLAUS® catalyst.
Therefore, no sulphur fires can occur in the SUPERCLAUS® reactor.

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Figure 1: Relative SO2 formation

SUPERCLAUS® condenser (R310-E-1012)

The steam pressure in the condenser is low in order to condense as much sulphur vapour as possible, but
not so low that the water temperature causes solidification of sulphur (approx. 115°C).

During the first days after admitting EUROCLAUS® tail gas to the SUPERCLAUS® stage, the condenser is
operated at an increased steam pressure, similar to the other condensers. This is because during start-up
of the SUPERCLAUS® section the catalyst is very active and low levels of SO3 are formed. The SO3 will
form H2SO4 and this can react with NH3, to form ammonia salts causing plugging of the condenser. Also
plugging by solidification of sulphur can take place. Operating at increased steam pressure may also be
done at low throughput operation.

Thermal Oxidiser Burner (R310-FR-1003)

The function of the thermal oxidiser is to convert the residual H2S and other sulphur compounds, present in
the SUPERCLAUS® off-gas and the vent gas from the sulphur pit, into SO2. The maximum allowable H2S
content in the flue gas from the thermal oxidiser is 10 ppm vol.

The gas to be oxidized is heated by mixing with hot flue gas. The hot flue gas is produced in the thermal
oxidizer burner by combustion of fuel gas with air.

The combustion air for the fuel gas is supplied by the thermal oxidiser air blower. The air required for
oxidizing the sulphur compounds is partly supplied as vent air from the sulphur pit at a constant quantity.
The remainder is supplied by the thermal oxidiser air blower. The fuel gas is burnt in two stages.

The first stage is the primary air, supplied to the burner. The primary air flow is ratio controlled by the fuel
gas flow. It is important to operate the primary air at substoichiometric conditions (between 80% and 90% of
stoichiometry) to prevent NOx formation.

The next stage is the "staged" air, supplied after the flame zone. The staged air flow is also ratio controlled
by the fuel gas flow, but moreover the output of the oxygen controller is added to the air flow rate,
calculated from the fuel gas flow. As the staged airflow corresponds with 50% of stoichiometric combustion
of the fuel gas, the fuel gas is actually burnt with approximately 130% of the stoichiometric air quantity.

Secondary air is supplied to the thermal oxidizer chamber to obtain an oxidizing environment. The
secondary airflow controller is adjusted by the output of the oxygen controller. Consequently, free oxygen is
available for the incineration of non-recovered sulphur components.

The flue gas leaving the thermal oxidiser is discharged via the stack to the atmosphere.

The operating temperature in the thermal oxidiser is 750°C and the oxygen concentration is 2.1 vol.%

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during the SUPERCLAUS® mode. It is obtained from:

a. Combustion of fuel gas in the thermal oxidiser burner.


b. Combustion of the combustibles present in the tail gas, which is however small in the
SUPERCLAUS® mode.

At lower temperatures than 750°C the H2S content in the flue gas will increase. This might be partly
compensated by increasing the O2 concentration. A higher temperature will result in higher fuel gas
consumption. In the Claus mode, the tail gas contains considerably more H2S. In order to keep the H2S
content in the flue gas below 10 ppm vol, the operating temperature should be increased.

A low O2 concentration has the same effect as a low temperature: the H2S content increases. More O2
means that too much air is supplied, resulting in high fuel gas consumption.

In the Claus mode, more air is required for oxidation of the tail gas than in the SUPERCLAUS® mode as
the tail gas from the SRU contains more combustibles.

The flue gas leaving the thermal oxidiser is discharged via the stack to the atmosphere.

Apart from at initial start-up, the thermal oxidiser should be started before the main burner at subsequent
start-ups. Then poisonous gas with sulphur combustibles that might still be present in the unit, is converted
and released via the stack.

When Oxygen concentration decreases in the Thermal Oxidiser Burner, incomplete oxidation of the tail
gases might occur, leading to high H2S content in the flue gas. For diminishing this, higher temperatures
must be accomplished in the burner. If the oxygen concentration gets even lower, danger of soot formation
and flame extinguishing might be created.

On the other hand, when oxygen concentration increases up to stoichiometric (or higher) ratio in the
Thermal Oxidiser Burner (too high the primary air flow), there is a high risk of NOX formation and emission
to atmosphere.

A low temperature in the combustion of tail gases might lead to the same consequences as the low oxygen
concentration, this is: incomplete oxidation causing high H2S content in the flue gas. In this case, the
mitigation procedure should be increasing the oxidation airflow in order to build up the oxygen concentration
in the combustion mixture.

Sulphur Degassing

The air (with the released H2S) leaving the bubble columns is drawn off by the steam ejector. The capacity
of the ejector is higher than the stripping air flow, so that an additional amount of sweep air is drawn in via
an air intake on the pit cover.

Initially the pit contains undegassed sulphur. At start-up, i.e. after opening the air supply to the bubble

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columns, the released H2S is more than at normal operation. To prevent the creation of an explosive gas
mixture (H2S with air), an additional amount of sweep air flows into the pit by having the second ejector in
operation during at least one hour after start-up.

The sulphur temperature in the stripping section of the pit should be maintained between 125°C and 155°C.
Below 125°C the margin between operating and solidification temperature of 115°C would become too
small. Please note that the melting temperature is 119°C. Above 155°C degasification is less effective due
to the increased sulphur viscosity.

In order to operate the stripping section below 150°C, the incoming sulphur is cooled. The sulphur passes
through the sulphur cooler, located inside the pit. The cooling medium is boiler water from the
SUPERCLAUS® condenser with a temperature of 117°C.

The sulphur is cooled to 159°C in the cooler. Further cooling takes place by heat losses from the sulphur
pit.

When the temperature in the storage compartment exceeds 155°C, problems in the sulphur pumps
bearings may occur as the viscosity of the degassed sulphur rises excessively.

It is expected that during normal operation the steam coils in the stripping section will be switched off.

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3.2.2.4 Drawings (PFD’s & P&ID’s, Plot Plan)

See ANNEX I
Attached in this point are the following Process and Flow Diagrams (PFD´s):

Dwg. Nº Description
1800-8110-20-R310-0189 Claus Section
1800-8110-20-R310-0190 Euroclaus/Superclaus Section
1800-8110-20-R310-0191 Sulphur Pit
1800-8110-20-R310-0192 Thermal Oxidiser
1800-8110-20-R310-0193 Feed Section, Main Blowers and Condensate System
1800-8110-21-R310-0194S1 Stream Data – Sheet 1 of 2
1800-8110-21-R310-0194S2 Stream Data – Sheet 2 of 2
Table 1. PFD Index
NOTE 1: Both Trains are represented via tag numbers

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Attached in this point are the following Process Piping and Instrumentation Diagrams (P&ID´s) for Train 1:

Dwg. Nº
1800-8110-25-R310-0151 AMINE ACID GAS KO DRUM
1800-8110-25-R310-0152 SWS GAS KO DRUM
1800-8110-25-R310-0154 ACID GAS HEATING/ FEED CONTROL
1800-8110-25-R310-0155 S1 MAIN AIR BLOWER
1800-8110-25-R310-0155 S2 MAIN AIR BLOWER
1800-8110-25-R310-0155 S3 THERMAL OXIDISER AIR BLOWER
1800-8110-25-R310-0156 COMBUSTION AIR HEATING/ CONTROL
1800-8110-25-R310-0157 MAIN BURNER
1800-8110-25-R310-0158 WASTE HEAT BOILER
1800-8110-25-R310-0159 1st REACTOR STAGE
1800-8110-25-R310-0160 2nd REACTOR STAGE
1800-8110-25-R310-0161 3rd REACTOR STAGE (EUROCLAUS)
1800-8110-25-R310-0162 SUPERCLAUS REACTOR
1800-8110-25-R310-0163 5th CONDENSER & COALESCER
1800-8110-25-R310-0164 SULPHUR SEALS
1800-8110-25-R310-0165 SULPHUR PIT DEGASSING SECTION
1800-8110-25-R310-0166 SULPHUR PIT STORAGE COMPARTMENT
1800-8110-25-R310-0167 S1 THERMAL OXIDISER AIR BLOWERS
1800-8110-25-R310-0167 S2 THERMAL OXIDISER AIR BLOWERS
1800-8110-25-R310-0168 THERMAL OXIDISER
1800-8110-25-R310-0169 COMMOM STACK
1800-8110-25-R310-0170 FUEL GAS KO DRUM & DISTRIBUTION
1800-8110-25-R310-0171 CONDENSATE SYSTEM
1800-8110-25-R310-0172 BLOW DOWN
1800-8110-25-R310-0178 FLARE SYSTEM
1800-8110-25-R310-0179 SAMPLE CONNECTION DETAILS
Table 2. Process P&ID Index.

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Attached in this point are the following Utilities Piping and Instrumentation Diagrams (P&ID´s) for Common
Section and Train 1:

Dwg. Nº Description
1800-8110-25-R310-0173S1 HP STEAM SHEET 1 OF 2
1800-8110-25-R310-0173S2 LP STEAM SHEET 2 OF 2
1800-8110-25-R310-0174 NITROGEN/IA/PA DISTRIBUTION
1800-8110-25-R310-0175 S1 BFW & UTILTY WATER SHEET 1 OF 2
1800-8110-25-R310-0175 S2 DW, CWS & CWR SYSTEMS SHEET 2 OF 2
1800-8110-25-R310-0180 PUMP AUXILIARY DETAILS
1800-8110-25-R310-0181 ANALYSER AUXILIARY DETAILS
Table 3. Utilities P&ID Index.

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Attached in this point are the following Process Piping and Instrumentation Diagrams (P&ID´s) for Train 2:

Dwg. Nº
1800-8110-25-R310-0851 AMINE ACID GAS KO DRUM
1800-8110-25-R310-0852 SWS GAS KO DRUM
1800-8110-25-R310-0854 ACID GAS HEATING/ FEED CONTROL
1800-8110-25-R310-0856 COMBUSTION AIR HEATING/ CONTROL
1800-8110-25-R310-0857 MAIN BURNER
1800-8110-25-R310-0858 WASTE HEAT BOILER
1800-8110-25-R310-0859 1st REACTOR STAGE
1800-8110-25-R310-0860 2nd REACTOR STAGE
1800-8110-25-R310-0861 3rd REACTOR STAGE (EUROCLAUS)
1800-8110-25-R310-0862 SUPERCLAUS REACTOR
1800-8110-25-R310-0863 5th CONDENSER & COALESCER
1800-8110-25-R310-0864 SULPHUR SEALS
1800-8110-25-R310-0865 SULPHUR PIT DEGASSING SECTION
1800-8110-25-R310-0866 SULPHUR PIT STORAGE COMPARTMENT
1800-8110-25-R310-0867 S1 THERMAL OXIDISER AIR BLOWERS
1800-8110-25-R310-0867 S2 THERMAL OXIDISER AIR BLOWERS
1800-8110-25-R310-0868 THERMAL OXIDISER
1800-8110-25-R310-0870 FUEL GAS KO DRUM & DISTRIBUTION
1800-8110-25-R310-0871 CONDENSATE SYSTEM
1800-8110-25-R310-0872 BLOW DOWN
1800-8110-25-R310-0877 S1 MAIN AIR BLOWER AND COMMON SPARE
1800-8110-25-R310-0877 S2 MAIN AIR BLOWER AND COMMON SPARE
1800-8110-25-R310-0877 S3 MAIN AIR BLOWER AND COMMON SPARE
1800-8110-25-R310-0877 S4 MAIN AIR BLOWER AND COMMON SPARE
1800-8110-25-R310-0878 FLARE SYSTEM
1800-8110-25-R310-0879 SAMPLE CONNECTION DETAILS
Table 2. Process P&ID Index.

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Attached in this point are the following Utilities Piping and Instrumentation Diagrams (P&ID´s) for Common
Section and Train 2:

Dwg. Nº Description
1800-8110-25-R310-0873S1 HP STEAM SHEET 1 OF 2
1800-8110-25-R310-0873S2 LP STEAM SHEET 2 OF 2
1800-8110-25-R310-0874 NITROGEN/IA/PA DISTRIBUTION
1800-8110-25-R310-0875 S1 BFW & UTILTY WATER SHEET 1 OF 2
1800-8110-25-R310-0875 S2 DW,CWS & CWR SYSTEMS SHEET 2 OF 2
1800-8110-25-R310-0880 PUMP AUXILIARY DETAILS
Table 3. Utilities P&ID Index.

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Attached in this point are the following Plot Plans:

Dwg. Nº Description
1800-8230-01-R310-0001 (Sh 01 & 02) Facility Plot Plan Sulphur Recovery Train 1
1800-8230-01-R310-0001 (Sh 02 & 02) Facility Plot Plan Sulphur Recovery Train 2
Table 4. Plot Plan Index
See ANNEX I

3.2.2.5 Line Schedule Tables

See ANNEX I

Attached in this point is the Line Schedule Tables:

Doc. Nº Description
1800-8110-26-R310-2001 Line List for Sulphur Recovery Unit Train 1
1800-8110-26-R310-2002 Line List for Sulphur Recovery Unit Train 2
Table 5. Line List Index

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3.2.3 Utilities and Chemicals

See ANNEX II

3.2.3.1 Utility Consumption Summary

The utilities Balances for SRU are included in this section. The following balances are included:

9 Sea Cooling Water consumption


9 Utility Water Consumption
9 Utility Air Consumption
9 Instrument Air consumption
9 Nitrogen Consumption
9 Fuel Gas Consumption
9 Steam Balance

3.2.3.2 Chemicals and Catalysts

Catalyst for Claus Converters

The following quantities are net quantities per Sulphur Recovery Unit Train. The new Sulphur Plant contains
two identical Sulphur Recovery Unit Trains.

Axens CRS-31 Catalyst

Size: 3-4 mm extrudates

Bulk density: 900-1100 kg/m3

Quantity required: 14.2 m3

Total: 28.4 m3

Axens CR-3S Catalyst

Size: 3-6 mm balls

Bulk density: 680-740 kg/m3

Quantity required: 76.2 m3

Total: 152.4 m3

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Packing of Claus Catalyst

Packing type: Big bags

Packing quality: Seaworthy

Catalyst for Euroclaus® Converter

The following quantities are net quantities per Sulphur Recovery Unit Train. The new Sulphur Plant contains
two identical Sulphur Recovery Unit Trains.

The Euroclaus® catalyst type is Ketjenfine 756 (KF-756).

Euroclaus® Catalyst

Size: 1.3 mm dia

Shape: quadralobe

Bulk density: Approximately 620 kg/m3

Quantity required: 3.1 m3

Total: 6.2 m3

Packing of Euroclaus® Catalyst

Packing type: Drums

Packingquality: Seaworthy

Catalyst for Superclaus® Converter

The following quantities are net quantities per Sulphur Recovery Unit Train. The new Sulphur Plant contains
two identical Sulphur Recovery Unit Trains.

The Superclaus® catalyst type is JCSC-12, equivalent to D -1651. It consists of a mixture of α-Alumina and
Silica catalyst. The two catalyst types (α-Alumina and Silica) are premixed on a 25%/75% volume basis by
the manufacturer.

Superclaus® Catalyst

Size: 1.80 ± 0.15 mm dia

Shape: extrudates

Bulk density: Approximately 560 kg/m3

Quantity required: 25.6 m3

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Total: 51.2 m3

Packing of Superclaus® Catalyst

Packing type: Drums

Packing quality: Seaworthy

Ceramic balls

The Claus Reactor contain a 100 mm support layer of ceramic balls with a diameter of 6 mm. The support
layer is situated on top of the gauze on the support grid.

The Euroclaus® Reactor contains a 100 mm. support layer of the catalyst. The support layer consists of
chemically inert ceramic balls with a diameter of 6 mm.

The Superclaus® Reactor contains a 50 mm. holddown layer on top of the catalyst. The holddown layer
consists of chemically inert ceramic balls with a diameter of 6 mm. The support layer consist of two types of
chemically inert ceramic balls. The upper support layer has a height of 50 mm and consists of 3 mm balls.
The lower support layer also has a height of 50 mm and consists of 6 mm balls.

Supplier: Denstone 57

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3.2.4 Control Systems

3.2.4.1 Distributed Control System (DCS)

See ANNEX III

Control Narrative
See ANNEX III

1. Process Alarms List and Settings

L H HH
Loop Name Tag Number Alarm Alarm Trip Units P&ID
R310-AT-1184A - 1.2 2 %vol 1800-8110-25-R310-0161
R310-AT-1184C - 1.2 %vol 1800-8110-25-R310-0161
R310-AT-1282 1 3 %vol 1800-8110-25-R310-0168
R310-AT-1284 0.2 %vol 1800-8110-25-R310-0168
R310-FT-0050 vendor kg/h 1800-8110-25-R310-0155
R310-FT-0055 vendor kg/h 1800-8110-25-R310-0155
R310-FT-1086 588 kg/h 1800-8110-25-R310-0157
R310-FT-1201 756 kg/h 1800-8110-25-R310-0162
R310-FT-1237 182 kg/h 1800-8110-25-R310-0165
R310-FT-1250 725 kg/h 1800-8110-25-R310-0166
R310-FT-1253 8539 14800 kg/h 1800-8110-25-R310-0166
R310-FT-1717 vendor kg/h 1800-8110-25-R310-0167
R310-FT-1767 vendor kg/h 1800-8110-25-R310-0167
R310-FT-3023 vendor kg/h 1800-8110-25-R310-0155
R310-LT-1001 300 1900 mm 1800-8110-25-R310-0151
R310-LT-1013 300 1250 mm 1800-8110-25-R310-0152
R310-LT-1126 750 950 mm 1800-8110-25-R310-0158
R310-LT-1145 1700 1900 mm 1800-8110-25-R310-0159
R310-LT-1167 1700 1900 mm 1800-8110-25-R310-0160
R310-LT-1217 1300 1450 mm 1800-8110-25-R310-0163
R310-LT-1253 500 4000 mm 1800-8110-25-R310-0166
R310-LT-1308 100 500 mm 1800-8110-25-R310-0170
R310-LT-1316 1350 1950 mm 1800-8110-25-R310-0171
R310-LT-1326 1150 2150 mm 1800-8110-25-R310-0172
R310-LT-3025 vendor mm 1800-8110-25-R310-0155
R310-PDT-0054 vendor kg/cm2 1800-8110-25-R310-0155
R310-PDT-0059 vendor kg/cm2 1800-8110-25-R310-0155
R310-PDT -1107 0.5 kg/cm2 1800-8110-25-R310-0157
R310-PDT -1295 0.002 kg/cm2 1800-8110-25-R310-0168
R310-PDT -1714 vendor kg/cm2 1800-8110-25-R310-0167
R310-PDT -1764 vendor kg/cm2 1800-8110-25-R310-0167
R310-PDT -3019 vendor kg/cm2 1800-8110-25-R310-0155

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R310-PDT -3029 vendor kg/cm2 1800-8110-25-R310-0155


R310-PT-1077 0.5 kg/cm2g 1800-8110-25-R310-0156
R310-PT-1089 1.44 kg/cm2g 1800-8110-25-R310-0157
R310-PT-1090 1.16 kg/cm2g 1800-8110-25-R310-0157
R310-PT-1217 0.5 1.84 kg/cm2g 1800-8110-25-R310-0163
R310-PT-1304 2 3 kg/cm2g 1800-8110-25-R310-0170
R310-PT-1327 1.5 kg/cm2g 1800-8110-25-R310-0172
R310-PT-1330 42 45.5 kg/cm2g 1800-8110-25-R310-0173S1
R310-PT-1332 5 6 kg/cm2g 1800-8110-25-R310-0173S2
R310-PT-1342 1.5 3 kg/cm2g 1800-8110-25-R310-0174
R310-PT-3026 vendor kg/cm2g 1800-8110-25-R310-0155
R310-PT-3027 vendor kg/cm2g 1800-8110-25-R310-0155
R310-PT-3028 vendor kg/cm2g 1800-8110-25-R310-0155
R310-TT-0002 300 ºC 1800-8110-25-R310-0169
R310-TT-0003 250 ºC 1800-8110-25-R310-0169
R310-TT-1039 225 ºC 1800-8110-25-R310-0154
R310-TT-1077 225 ºC 1800-8110-25-R310-0156
R310-TT-1104 900 1350 ºC 1800-8110-25-R310-0157
R310-TT-1105 900 1350 ºC 1800-8110-25-R310-0157
R310-TT-1106 900 1350 ºC 1800-8110-25-R310-0157
R310-TT-1127 350 ºC 1800-8110-25-R310-0158
R310-TT-1133 220 ºC 1800-8110-25-R310-0158
R310-TT-1145 220 250 ºC 1800-8110-25-R310-0159
R310-TT-1159 210 ºC 1800-8110-25-R310-0159
R310-TT-1167 200 220 ºC 1800-8110-25-R310-0160
R310-TT-1181 210 ºC 1800-8110-25-R310-0160
R310-TT-1184 180 210 ºC 1800-8110-25-R310-0161
R310-TT-1190 210 ºC 1800-8110-25-R310-0161
R310-TT-1201 190 230 ºC 1800-8110-25-R310-0162
R310-TT-1219 240 ºC 1800-8110-25-R310-0163
R310-TT-1220 120 135 ºC 1800-8110-25-R310-0163
R310-TT-1223 100 ºC 1800-8110-25-R310-0163
R310-TT-1235 170 ºC 1800-8110-25-R310-0165
R310-TT-1236 130 160 ºC 1800-8110-25-R310-0165
R310-TT-1250 170 ºC 1800-8110-25-R310-0166
R310-TT-1251 130 160 ºC 1800-8110-25-R310-0166
R310-TT-1252 170 ºC 1800-8110-25-R310-0166
R310-TT-1254 130 160 ºC 1800-8110-25-R310-0166
R310-TT-1281 700 800 ºC 1800-8110-25-R310-0168
R310-TT-1315 80 ºC 1800-8110-25-R310-0171
R310-TT-1336 150 170 ºC 1800-8110-25-R310-0173S2
R310-TT-3030 vendor ºC 1800-8110-25-R310-0155
R310-TT-3031 vendor ºC 1800-8110-25-R310-0155
R310-TX-1150 350 ºC 1800-8110-25-R310-0159
R310-TX-1151 350 ºC 1800-8110-25-R310-0159
R310-TX-1152 350 ºC 1800-8110-25-R310-0159
R310-TX-1153 350 ºC 1800-8110-25-R310-0159

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R310-TX-1172 350 ºC 1800-8110-25-R310-0160


R310-TX-1173 350 ºC 1800-8110-25-R310-0160
R310-TX-1174 350 ºC 1800-8110-25-R310-0160
R310-TX-1175 350 ºC 1800-8110-25-R310-0160
R310-TX-1185 350 ºC 1800-8110-25-R310-0161
R310-TX-1186 350 ºC 1800-8110-25-R310-0161
R310-TX-1187 350 ºC 1800-8110-25-R310-0161
R310-TX-1188 350 ºC 1800-8110-25-R310-0161

3.2.4.2 Emergency Shutdown (ESD)

See ANNEX III

1. Cause and Effect Diagrams


See ANNEX III

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2. Process Trip List and Settings

Loop L H LL HH
Name Tag Number Alarm Alarm Trip Trip Units P&ID
R310-AT-1184B - 1.2 - 2 %vol 1800-8110-25-R310-0161
R310-FT-1039 1890 1680 kg/h 1800-8110-25-R310-0154
R310-FT-1046 385 342 kg/h 1800-8110-25-R310-0154
R310-FT-1078 3633 3229 kg/h 1800-8110-25-R310-0156
R310-FT-1080 1417 1259 kg/h 1800-8110-25-R310-0156
R310-FT-1087 661 588 kg/h 1800-8110-25-R310-0157
R310-FT-1202 672 kg/h 1800-8110-25-R310-0162
R310-FT-1238 205 182 kg/h 1800-8110-25-R310-0165
R310-FT-1251 644 kg/h 1800-8110-25-R310-0166
R310-FT-1286 616 kg/h 1800-8110-25-R310-0168
R310-LT-1003 2700 mm 1800-8110-25-R310-0151
R310-LT-1015 1800 mm 1800-8110-25-R310-0152
R310-LT-1125 750 600 mm 1800-8110-25-R310-0158
R310-LT-1306 500 600 mm 1800-8110-25-R310-0170
R310-LT-1317 750 mm 1800-8110-25-R310-0171
R310-LT-1325 1150 200 mm 1800-8110-25-R310-0172
R310-LT-1328 300 mm 1800-8110-25-R310-0166
R310-PT-1074 0.5 0.2 kg/cm2g 1800-8110-25-R310-0156
R310-PT-1086A 1.16 1.66 kg/cm2g 1800-8110-25-R310-0157
R310-PT-1086B 1.16 1.66 kg/cm2g 1800-8110-25-R310-0157
R310-PT-1086C 1.16 1.66 kg/cm2g 1800-8110-25-R310-0157
R310-PT-1287 0 kg/cm2g 1800-8110-25-R310-0168
R310-PT-1305 2 2 kg/cm2g 1800-8110-25-R310-0170
R310-TT-1204A 280 300 ºC 1800-8110-25-R310-0162
R310-TT-1204B 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1204C 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1204D 320 350 ºC 1800-8110-25-R310-0162
R310-TT-1205A 280 300 ºC 1800-8110-25-R310-0162
R310-TT-1205B 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1205C 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1205D 320 350 ºC 1800-8110-25-R310-0162
R310-TT-1206A 280 300 ºC 1800-8110-25-R310-0162
R310-TT-1206B 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1206C 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1206D 320 350 ºC 1800-8110-25-R310-0162
R310-TT-1207A 280 300 ºC 1800-8110-25-R310-0162
R310-TT-1207B 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1207C 300 320 ºC 1800-8110-25-R310-0162
R310-TT-1207D 320 350 ºC 1800-8110-25-R310-0162
R310-TT-1282 700 800 ºC 1800-8110-25-R310-0168
R310-TT-1335 170 180 ºC 1800-8110-25-R310-0173S2

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3.2.4.3 Logic Description for Start-up and Shutdown

See ANNEX III

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3.2.5 Overview Drawings

3.2.5.1 Electrical One Line Diagrams

See ANNEX IV

3.2.5.2 Area Classification Diagrams

See ANNEX IV

3.2.5.3 Material Selection Diagrams

See ANNEX IV

Attached in this point are following Material Selection Diagrams:

Dwg. Nº Description

1800-8110-23-R310-0001 Feed Section, Main Blowers and Condensate System


1800-8110-23-R310-0002 Claus Section
1800-8110-23-R310-0003 Euroclaus/Superclaus Section
1800-8110-23-R310-0004 Sulphur Pit
1800-8110-23-R310-0005 Thermal Oxidiser
1800-8110-23-R310-0006
Table 1. MSD Index
NOTE 1: Both Trains are represented via tag numbers

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3.2.6 General HSE Systems and Equipment

3.2.6.1 Pressure Relief Devices

See ANNEX V

Pressure relief devices list for SRU is included hereinafter

3.2.6.2 Fire & Gas Systems

See ANNEX V

3.2.6.3 Fire Fighting Equipments

See ANNEX V

3.2.6.4 Material Safety Data Sheets (MSDS)

See ANNEX V

3.2.6.5 Operational Safety Issues

The following information deals with the prevention of possible dangerous situations encountered in the
Sulphur Recovery Unit.

1. H2S monitor equipment


H2S is a very toxic gas. For protection of the operating personnel, an H2S monitor system is installed.

The monitor is a multi-channel system specific for continuous monitoring of H2S in the ambient air.

The system consists of several local sensors and a common solid state monitor. Each sensor has its own
channel. The individual channels are independent and each channel continuously reads the H2S gas
concentration at its remote sensor location.

Manual override switching is included to permit a read out of any given channel without interrupting
automatic response of alarm circuits.

Meter range: 0 – 100 ppm vol. H2S.

The complete system consists of one monitor, local sensors, an indicator situated on the control room panel
and a warning alarm system in the unit as well as in the control room.

The alarm is audible and visible.

When the concentration of H2S in the atmosphere, after the alarm is actuated, appears to increase

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considerably, the unit has to be shutdown manually to stop all incoming streams.

The alarm is set at a value of 15 ppm vol. H2S.

It is advised to check the sensors every six months.

Process gas leaks of minor nature can be detected by means of cotton waste soaked in ammonia. If this is
brought into the vicinity of the leak, white fumes of ammonium salts will be formed. In addition, filter paper
wetted with lead acetate solution can be used. The lead acetate turns black when exposed to H2S.

2. First aid measures


If a person has lost consciousness by inhalation of H2S or SO2 gas, the following procedure is advised:

1. Remove the patient to fresh air or a well ventilated room and loosen any restrictive clothing.

2. In conjunction with 1 above, contact the medical department, and call immediately a doctor,
stressing the nature of the accident.

3. A person familiar with the use of oxygen inhalation apparatus should only carry out application
of oxygen to a patient. An attempt to apply oxygen by a person not familiar with the use of the
apparatus may result in the loss of valuable time and may harm the patient.

4. Keep the patient comfortably warm, but not hot. If the patient regains consciousness during this
period, keep him as calm as possible as he might be in a state of shock.

5. If, however, respiration of the patient has stopped, commence artificial respiration treatment at
once and continue until professional assistance arrives.

6. It should not be attempted to give anything to eat or to drink to an unconscious patient.

Note
Do not attempt to enter a gaseous area to render assistance before putting on a compressed air breathing
apparatus or air hose mask.

Toxicological data

Tables of H2S and SO2 effects are given below, followed by a summary of some of their properties.

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3. Physiological Effects of H2S

Effect ppm1) vol. vol.%

1. Limit for odour detection 0.14

2. Weak odour hardly noticeable 0.77

3. Noticeable odour 4.6

4. Obnoxious odour 7.0

5. MAC2) 10 0.001

6. Slight signs of inflammation of the eyes after one hour 50 - 100 0.005 - 0.010

Limit that can be stood for six hours without adverse


7. 78 - 128 0.008 - 0.013
effects

Limit that can be stood for one hour without


8. 170 - 255 0.017 - 0.026
consequences

9. Odour no longer disagreeable 198 - 283 0.020 - 0.028

Distinct signs of inflammation of the eyes after one


10. 200 - 300 0.02 - 0.03
hour

11. Danger to life within thirty to sixty minutes 355 - 496 0.036 - 0.050

12. Fatal within thirty to sixty minutes 425 - 580 0.043 - 0.058

13. Fatal after half an hour 500 - 700 0.05 - 0.07

14. Causing immediate fainting 700 - 1000 0.07 - 0.10

15. Immediately fatal 850 - 1980 0.085 - 0.2

1)
ppm =
volume parts of H2S per million parts of air
1 ppm =1 cm3/m3
2) MAC =
Maximum allowable concentration for an eight hours working day

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Physiological Effects of SO2

Effect ppm 1) vol. vol.%

1. Limit for odour detection 3-5

2. MAC 2) 5

Smallest amount causing immediate irritation of


3. 20 0.002
the eyes and throat

Maximum allowable concentration for


4. 50 - 100 0.005 - 0.010
30 - 60 minutes

5. Danger even with short exposure more than 400 0.040

1
) ppm = volume parts of H2S per million parts of air
1 ppm = 1 cm3/m3

H2S Properties and Toxic Effects

H2S is a colourless, inflammable and very toxic gas having an offensive odour and sweetish taste. It has a
specific gravity 1.17 times that of air.

The offensive odour, like that of rotten eggs, is not reliable as a warning of dangerous concentrations, as
persons differ greatly in the ability to detect smells, and furthermore the sense of smell deteriorates and is
of little help in noting higher increased concentrations.

H2S is almost as toxic as hydrogen cyanide and six times as toxic as carbon monoxide.

The toxic effects vary considerably with the concentration and to some extent with individual susceptibility.

At low concentrations, it has an irritant action on the respiratory tract, which could result in sickness,
vomiting and a feeling of pressure on the chest. Simultaneously it affects the nervous system.

At high concentrations, H2S paralyses the nervous system. Consequently, the respiration fails and death
will follow immediately by suffocation.

Even at low concentrations, H2S affects the cornea of the eye.

SO2 Properties and Toxic Effects


Sulphur dioxide is a colourless gas, with a specific gravity 2.2 times that of air.

In the presence of mist or water, this gas forms sulphurous acid.

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The gas has a sour taste. It irritates the respiratory tracts because it forms, with the water present,
sulphurous acid and further sulphuric acid.

This acid etches the human tissue.

At low concentrations, it irritates the mucous membranes. Inhalation of higher concentrations causes
hoarseness, pain and a feeling of pressure on the chest and bronchitis. It is sometimes impossible to speak
or to swallow.

Very high concentrations cause acute bronchitis, tightness of the chest and a quick start of perturbation of
consciousness. Instant death by poisoning seldom occurs.

Suffocation, however, can cause death quickly.

SO2 also causes an increase of haemoglobin in the blood.

The toxic effects vary to some extent with individual susceptibility.

A certain immunization to SO2 is possible, to a maximum of 30 to 50 ppm vol.

Human beings can withstand a maximum of 20 ppm vol. without adverse effects.

Higher concentrations can give the victim a pale appearance, cause an unpleasant taste in the mouth and
can even make the gustatory nerves insensitive.

Additional effects are loss of appetite and constipation.

Sulphur Dust
Sulphur dust in the atmosphere has a highly irritating effect upon the human eye. Therefore, safety goggles
should be worn when working in an atmosphere where dust contaminates the air. This cannot be
overemphasized.

Fire and explosivity data

H2S
The lower and upper limits for inflammability in a gas air mixture are 4.3 and 45.5 vol.%, respectively. In the
stoichiometric ratio with oxygen, it explodes violently when ignited.

It is therefore necessary to handle hydrogen sulphide by excluding all sources of ignition, open flames,
sparks (including static discharges) and heat producing equipment from contact with this gas when mixed
with air.

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The auto-ignition of H2S in air will occur at a temperature of approximately 260°C.

SO2
This is a non-inflammable gas.

Sulphur liquid
At a temperature of approximately 230°C, auto-ignition of liquid sulphur will occur when in contact with air.

Therefore, attention must be paid to ensure that the liquid sulphur temperature is maintained below the
above-mentioned value.

Ignition of the sulphur will also occur when exposed in the area of an open flame, resulting in the formation
of SO2.

Sulphur dust
As stated above, liquid sulphur has a relatively low ignition point, 230°C; however, sulphur dust clouds will
already ignite at a temperature of approximately 190°C.

See ANNEX IX

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3.3 OPERATING INSTRUCTIONS

3.3.1 Preparation for Start-up

A systematic program of start-up preparations must be drawn up and carried out to ensure that the start-up
properly proceeds with the minimum delay. This is particularly important when the unit has to be brought on
stream together with other units within a limited period.

The construction of the plant as a whole must be checked in detail against design and equipment
specifications.

The unit area should be cleaned of all unnecessary construction materials that might burn, and the area
around the unit should be cleared sufficiently to provide complete safety of movement for operating and fire
fighting personnel. This should be carried out before the introduction of fuel gas into the plant equipment. All
fire fighting and gas protection facilities within the unit should be available for immediate use.

Some of the items are construction details, but operations must confirm that they have been performed. It
will not be necessary to repeat all of these items on subsequent start-ups. The attention devoted to
preliminary preparations for start-up contributes greatly to a safe and successful start-up.

Cleaning Of Waste Heat Boiler

During the construction period of the unit, the inside of the equipment is exposed to grease and oil. These
have to be removed from the steam side of the waste heat boilers before the initial start-up takes place, as
they decrease the heat transfer at the tubes.

Also scales have been formed on the metal walls. These have to be removed to avoid dirt accumulation
inside the boiler and to avoid harm to the downstream steam piping and equipment. Following procedure
can be executed to clean the boilers or alternatively a procedure from the boiler manufacturer should be
used.

Before starting the cleaning procedure, make sure that all flanges of the boiler are blinded and keep the
blind list register updated. The cleaning of the waste heat boilers takes place in two steps. In the first step
grease and oil are removed and in the second step scale.

First step (removal of grease and oil)

1. Prepare a quantity of Na3PO4, corresponding with 0.3 wt.% and NaOH, corresponding with
0.025 wt.% in the boiler water.

2. Supply boiler feed water to the boiler until normal level is reached. Keep the vent open.

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3. Add the above mentioned chemicals to the water content via a manhole etc. and close the
manhole. The vent remains open.

4. Supply LP steam to the boiler. Keep the water boiling for 24 hours at atmospheric pressure.
Maintain the water level by blowing-down some boiler water each 1-2 hours.

5. Close the steam supply and drain the total boiler content.

Second step (removal of scale and rust)

1. Prepare a quantity of Na3PO4, corresponding with 0.5 wt.% in the boiler water.

2. Supply boiler feed water to the boiler until normal level is reached. Keep the vent open.

3. Add the Na3PO4 to the water content via a manhole etc. and close the manhole. The vent
remains open.

4. Supply LP steam to the boiler. Close the vent when steam is supplied. Let the pressure rise to
LP steam refinery pressure and close the steam supply. Maintain the water level by blowing-
down some boiler water if required. Wait until the pressure has dropped to 1 kg/cm2g and
repeat this step at least 5 times.

5. After the 5th time of supplying LP steam tot the boiler, wait until the pressure has dropped to 1
kg/cm2g. Then open the vent. Drain the total boiler content.

6. Clean the boiler by supplying boiler feed water to normal level and drain the contents. Repeat
this several times until the water is clear and has obtained a pH of approximately 9. If scaling
material still comes out of the boiler after several water washes, it is advised to repeat the
scaling removal procedure (step 2). Make sure that no air can enter the boiler after the cleaning
(new rust formation). Air ingress can be prevented by keeping the boiler under nitrogen
pressure or steam pressure. During cleaning with water, special attention should be paid to
removal of scale and rust at instrument connections.

Cleaning of Sulphur Condensers

Removal of scale is not required. Therefore, only the removal of oil and grease is applicable. Follow the
method as described in Step 1 for the Waste Heat Boiler. LP steam should be used instead of MP steam.
All connected instruments shall be removed.

On conclusion, clean the condenser by supplying boiler feed water to normal level and drain the contents.
Repeat this several times until the water is clear and has obtained a pH of approximately 9.

Commissioning of Utility and Instrument Systems

The following recommendations are suggested for the commissioning phase of the Sulphur Recovery Unit

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and can be utilized for subsequent start-ups after routine major overhauls.

1. It is assumed at this stage that:


• Cleaning of lines and vessels has been carried out.
• All isolating valves located within the unit are closed and the necessary blinds at the battery limit
installed.
• Power and utilities are available.
• P-1002, P-1001, P-1006 and E-1013 have been checked for lubrication and correct rotation.
• Acid gas lines and fuel gas lines are cleaned, purged and filled with nitrogen.
• The sulphur pit has been cleaned and is ready to receive product.
• All hand valves in the steam and condensate lines at the steam preheaters and the steam
reheaters are closed.
• The steam and condensate systems are available.
• The SUPERCLAUS® stage is bypassed.
2. Personnel from the Instrumentation Department will check out in detail the Instrumentation of the
Unit to ensure that:
• Safeguarding systems function correctly by simulation of abnormal conditions.
• The DCS is properly programmed and contains correct parameters.
• All alarms function correctly by simulation of abnormal conditions.
• All controllers function correctly by simulation of operating conditions and are already tuned where
possible.
• All instruments are commissioned.
3. Testing of the air blowers K-0001A/B/C and K-1002 A/B is advised at this stage so that any
mechanical defects may be rectified. Reference is made to the manufacturer's instruction for
blowers for testing and commissioning.
4. Simultaneously with the blower testing the unit is blown-through for 60 hours as the air flow
through the plant equipment will remove traces of dust etc., which has possibly remained in the
pipe work from the construction period. In addition, the air flow will help to pre-dry the fire bricks
and refractory linings.

Main burner

a. Open the air supply to the main burner with HS-1115. Adjust an initial air flow rate of 30% on FC-
1081. Gradually increase the air flow to maximum. Both control valves FV-1081 and XV-1077 can
be used.
b. By actuating HS-1202 the air stream from the Claus reactor stages can be routed to the
®
SUPERCLAUS stage. When the blow-through/testing operation is completed, the air supply to
the burner is closed with HS-1115. Shutdown the blowers.

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5. Check the positions of all non-return valves located in the steam pipe work, associated with the
boiler, condensers and steam heaters. Grease and exercise all valves, especially plug valves.
Ensure that all level gauge glasses and instruments are clean.
6. It is strongly advised to strip down the burner and ignition lance for cleaning. Check the burner
sight glasses.
7. Check if the ignitor functions properly by testing it outside the burner.
8. Slowly supply LP steam to the plant heating system. However, before systematically
commissioning each individual steam trap, open all low drain points, thereby flushing any dirt out
of the pipe work. When the condensate emitting from the above mentioned drain points run clean,
the steam traps are commissioned and the drain valves are closed, thereby directing all
condensate to the condensate system. Ensure that the condensate disposal system has been
commissioned.
9. Check all steam traced and steam jacketed equipment and lines for heating efficiency, using
thermal crayon or a lump of sulphur.
10. Ensure all valves downstream of the isolating blinds of the boiler feed water supply lines situated
at the battery limit are closed and reposition the isolating blinds to open position.
11. Commission boiler feed water to the waste heat boiler and the sulphur condensers as follows:

Waste heat boiler


1. Ensure that all boiler feed water valves at the waste heat boiler are closed.
2. Commission the level control loop of the waste heat boiler. The control valve will open.
3. Open fully the battery limit valve of the boiler feed water supply line.
4. Open the vent on the waste heat boiler.
5. Open cautiously the block valve upstream the control valve and flush clean the boiler feed water
line up to the bleeders of the control valve until the water becomes clear.
6. Open fully the valves located downstream of the control valve, with the exception of the block
valve. Make sure that the bypass is closed.
7. Open slightly the block valve in the boiler feed water line at the waste heat boiler to prevent
hammering and start filling.
8. Open the drain valve of the waste heat boiler to drain initial dirty water, until the water becomes
clear.
9. Close the drain valve and establish a normal operating level.
10. Maintain a constant check on the level gauge during filling. The low level alarm lights will be
automatically extinguished. When the control valve is fully closed, fully open the block valve at the
waste heat boiler.

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Sulphur condensers

The following applies to all sulphur condensers except the SUPERCLAUS® condenser.

1. Ensure that all boiler feed water valves at the condensers are closed.
2. Commission the level control loops of the condensers. The control valves will open.
3. Open fully the battery limit valve of the boiler feed water supply line.
4. Open the vents on the condensers.
5. Open the block valve upstream the control valve and flush clean the boiler feed water line up to
the bleeders of the control valve until the water becomes clear.
6. Open fully the valves (located downstream of the control valve, with the exception of the block
valve. Make sure that the bypass is closed.
7. Open slightly the block valve in the boiler feed water line at the condensers to prevent hammering
and start filling.
8. Open the drain valve of the condensers to drain initial dirty water, until the water becomes clear.
9. Close the drain valve and establish a normal operating level.
10. Maintain a constant check on the level gauge during filling. The low level alarm lights will be
automatically extinguished. When the control valve is fully closed, fully open the block valve at the
condenser.

SUPERCLAUS® condenser
1. Ensure that the globe valve in the boiler feed water supply line at the condenser is closed. Open the
block valve near the condenser inlet.
2. Open the vent on the condenser.
3. Open slightly the globe valve in the boiler feed water line to prevent hammering and start filling.
4. Open the drain valve of the condenser to drain initial dirty water, until the water becomes clear.
5. Close the drain valve and establish a normal operating level.
6. Maintain a constant check on the level gauge during filling. The low level alarm lights will be
automatically extinguished. When the normal level has been established, the globe valve in the
boiler feed water line should be closed.

Steam condenser
Test the operation of the air cooled Steam condenser with reference to the manufacturer’s instructions.

Sulphur Lines & Locks

1. Ensure that sulphur lines, sulphur locks and sulphur pit are completely free of foreign materials.

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2. Fill all sulphur locks with solid or liquid sulphur by removing the top blind flange. Ensure that the
lock is completely filled before reinstalling the blind flange.
3. Ensure that the discharge valves of the sulphur pumps and valves in the sulphur rundown lines are
closed.

Control loops

Commision the following control loops:

1. Temperature control loops of the reactor inlets (TC-1145, TC-1167, TC-1184 and TC-1201).
2. Temperature and steam pressure controllers of the SUPERCLAUS® condenser E-1012: TC-1220
and PC-1217, acting on the steam condenser. The initial set point of PC-1217 should be 4 kg/cm2
(ga).
3. Pressure controllers in HP steam and LP steam.
4. Relevant loops in the utility systems.

Blowdown System

The boiler water blow down drum may now be filled and the system commissioned, using BFW drained
from the waste heat boiler.

1. Open the suction and discharge isolation valves on both blow down pumps.

2. Open the bleed of the blow down drum level control valve and fully open the upstream block valve and
the by-pass valve. Ensure that the downstream block valve is closed. Open the bleed op the battery
limit valve.

3. Put the waste heat boiler level controller in AUTO then open the waste heat boiler blow down valve to
start filling the blow down system. Ensure that the waste heat boiler level controller responds by
admitting BFW to maintain the set point level.

4. When the water bleed at the level control and the battery limit valve becomes clear, indicating that the
blow down pump system is filled and flushed, close the bleed valves.

5. Continue filling the blow down drum to normal operating level, then commission the level controller and
the pumps with the discharge block valve open to the battery limit.

6. Once the blow down system has been commissioned, close the blow down valve from the waste heat
boiler.

7. Stop the blowdown pumps, leaving the discharge block valve open to the battery limit.

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Leak Test

Leak testing of the unit has to be carried out with nitrogen or maximum available air blower pressure.
Special attention should be paid to the acid gas feed system.

When equipment, piping, and field instrumentation assembly is agreed by both operations and construction
personnel to be essentially complete, a detailed checkout will be made to verify that all systems are
complete and installed as shown on the P&ID's. In addition, manually operated items (primarily valves)
should be checked for proper operation, to the extent this can be determined by observation of full, unim-
peded travel over the full range of operation. An inspection should be made, and all items approved as
properly installed (proper orientation) and functionally correct before process or utility fluids are introduced
to the plant.

The piping and associated equipment should be checked on a "line-by-line" basis, generally following the
flow path of the sulphur, process air, and utilities into the unit and through the system. Piping system
components are checked as encountered in following the flow.

At this stage, it is usual for a number of deficiencies to be found. In order to explicitly identify these items,
each should be tagged and a detailed "Punchlist" should be developed and given to the construction
personnel for corrective action.

Once construction advises that a deficiency has been corrected, the item will be reinspected. If the item
passes inspection, note the correction on the punchlist original and remove the tag from the item.

When construction and equipment cleaning is complete, the unit area should be inspected to insure a safe,
orderly start-up. All construction equipment should be removed, particularly scaffolding and combustible
material such as canvas, ropes, and lumber. The area, particularly stairways, walks, and platforms, should
be free of debris and obstruction. All safety equipment should be checked to insure that it is in place and
operable.

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3.3.2 Start-up Procedure

3.3.2.1 Drying Out and Initial Heating Up

Prior to the initial start-up phase of the unit, it is necessary to accomplish a complete drying out of the
reaction furnace, thermal oxidiser and any equipment that contains refractory. This is performed by
increasing the temperatures at a controlled rate, following the steps below (see figure 2):

• Heating-up at a rate of 20ºC/h up to 100ºC


• Maintain temperature at 100ºC during approximately 8 hours
• Heating-up at a rate of 20ºC/h up to 220ºC
• Maintain temperature at 220ºC during approximately 10 hours
• Heating-up at a rate of 40ºC/h until operating temperature is reached

IF TAKEN TO USE DIRECTLY


HEATING UP WITH 40ºC / h COOLING DOWN AFTER OPERATION
WITH 50ºC / h

1400

1200

1000
Temperature ºC

800
HEATING UP
600 BY RESTART
WITH
50ºC / h
400

200

0
10 20 30 40 50 60 80 100 110 120 130 140

HEATING UP Time in hours


20ºC / h
IF COOLING DOWN AFTER DRYING OUT
COOLING DOWN WITH 20ºC / h

Figure 2. Drying-out & heating-up

Next, the unit is cooled-down to enable loading of the catalyst. NOTE: If cooling down directly after drying
out, it shall be carried out at a rate of 20ºC/h. However, if cooling down after operation, it shall be carried

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out at a rate of 50ºC/h.

In the initial start-up phase, the thermal oxidiser should only be started when the Claus section produces an
off-gas, as this gas acts as a cooling medium allowing for a gradual heating-up of the thermal oxidiser.
Once the thermal oxidiser is hot, it can be operated without Claus tail gas.

Remarks:
1. The drying-out and heating-up procedures as described below, indicated in Figure 2, are to be
considered as guidance only. The refractory lining manufacture should supply dedicated drying
out curves for all refractory.

2. At start-up of the reaction furnace burner the temperature will initially rise to approximately 400
°C and cannot be lowered without extinguishing the flame. This temperature should be
maintained for 24 hours to slowly heating up the refractory in the front-end of the reaction
furnace.

3. The Superclaus® stage is bypassed before ignition. Start-up without bypass operation is not
possible, as the safeguarding system does not allow initiating the ignition procedure when the
bypass valve is closed.

4. The procedure can be started as soon as commissioning has taken place and all
instruments/instrument loops have been tested.

Simplified Outline
1. Remove all isolating blinds, except for feed gases.

2. Reset the logic system.

3. Start the air blower and the air preheater.

4. Commission the remaining utility systems.

5. Dry-out the unit with hot air.

6. Purge the main burner with nitrogen.

7. Admit fuel gas to the main burner.

8. Start the reheaters of the catalytic reactors.

9. Start the thermal oxidiser burner.

10. Further dry-out and heat-up the unit.

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Detailed Outline
Preparations
1. All isolating blinds situated at the unit and battery limits are removed, except at acid feed gas
lines.

2. Check the permissives to start the main burner.

3. Check the liquid level in the waste heat boiler (LI-1125).

4. Ensure that fuel gas for the main burner is available (PI-1089).

5. Ensure that the emergency shutdown switches are in the correct position

6. (HS-1113A/B/C for the main burner and HS-1290A/B/C for the thermal oxidiser).

7. Ensure that the inlet valve EIV-1511 of the SUPERCLAUS® stage is closed and that EIV-1512
in the bypass is open.

8. Reset the logic system for the main burner by HS-1108.

9. Start one of the air blowers. Confirm that the blower vents properly to the atmosphere to
prevent surging.

10. Commission all utility systems.

11. Open the air supply to the main burner with HS-1115. Adjust an initial air flow rate of 30% on
FC-1081. Gradually increase the air flow to maximum. Both control valves FV-1081 and XV-
1077 can be used.

12. Commission HP steam to the air preheater and commission its condensate system. Put the air
preheater carefully into operation: admit slowly steam to the preheater via the bypass valve. Do
not open the main steam valve until the preheater is sufficiently heated.

13. The unit is dried out as far as possible with the air preheater according to figure 2. On
conclusion, the air supply is stopped with HS-1115. The steam supply to the air preheater is
also stopped.

Purging and ignition in the Main Burner


The ignition sequence is started with the nitrogen purge of the main burner and proceeds automatically until
ignition is obtained. Within 15 minutes after purging, a flame should be established.

1. Commission the nitrogen for purging to prevent sooting of the flame scanners and sight
glasses.

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2. Start the ignition procedure by actuating button HS-1109. Purging of the main burner is started
automatically. Ensure that the nitrogen flow is above the trip setting of FI-1087. The purge is
completed after 5 minutes.

3. When the purge is completed, the next step is automatically started. The ignitor is inserted, the
combustion air supply is started, the ignitor is energized and the fuel gas valves are opened.
Within 5 seconds ignition should be obtained, otherwise the unit is tripped. The air flow rate is
normally the minimum allowable air flow to the burner (4020 kg/h). In case ignition is hard to
obtain with this flow rate, it can be manually increased within a certain range by varying the
output of controller FC-1081. The fuel gas flow rate is such that the combustion is
stoichiometric (239 kg/h). In addition, the fuel gas flow (FC-1088) can be manually adjusted
within a certain range. The settings are determined empirically.

Remark
Normally the burner can be started quickly with the predefined positions on the air and fuel gas controllers.
These settings correspond with stoichiometric combustion at the minimum air flow with the corresponding
fuel gas flow. However, due to the actual burner dimensions and location of the tip of the ignitor, it is
sometimes easier to obtain ignition at other flow rates. This should be empirically found. Once these flow
rates have been adjusted in the DCS, they can be used for subsequent start-ups.

1. One minute after ignition following controllers are accessible for the operator.

• FC-1081, acting on the trim air valve.


• XC-1077, acting on the main air valve.
• FC-1080, fuel gas.

2. After establishing a stable flame, the size of the flame should be restricted. Decrease the fuel gas
flow to its minimum value of 72 kg/h and adjust the air flow to 4020 kg/h. This results in a “330%
of stoichiometric burn”, i.e. with 230% excess air.

Switch FC-1080 (fuel gas) and FC-1081 (total air) to AUTO mode. After switching FC-1081 to CASCADE,
the ratio between fuel gas and air can be adjusted with HC-1090. XC-1077 can be taken into operation to
allow the operator to increase the air flow during warming-up. Steam can be added to the flame for
quenching purposes by actuating HS-1111.

Heating of the First Claus Reactor

1. Commission HP steam to the first steam reheater E-1005 and commission its condensate system.
Ensure that control valve in the steam supply line is fully closed.

Put the heater carefully into operation by slowly admitting steam via the control valve bypass. Do not open

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the control valve until the heater is sufficiently heated!

2. Commission the automatic temperature control system (TC-1145). Keep the temperature at TC-
1145 between 150°C and 180°C during the first six hours in order to obtain a gradual heating-up of
the reactor.

Heating of the Second Claus Reactor


1. Commission HP steam to the second steam reheater E-1007 and commission its condensate
system. Ensure that control valve in the steam supply line is fully closed.

Put the heater carefully into operation by slowly admitting steam via the control valve bypass. Do not open
the control valve until the heater is sufficiently heated!

2. Commission the automatic temperature control system (TC-1167). Keep the temperature at TC-
1167 between 150°C and 180°C during the first six hours In order to obtain a gradual heating-up of
the reactor.

Heating of the EUROCLAUS® Reactor

1. Commission HP steam to the third steam reheater E-1009 and commission its condensate system.
Ensure that control valve in the steam supply line is fully closed.

Put the heater carefully into operation by slowly admitting steam via the control valve bypass. Do
not open the control valve until the heater is sufficiently heated!

2. Commission the automatic temperature control system (TC-1184). Keep the temperature at TC-
1184 between 150°C and 180°C during the first six hours In order to obtain a gradual heating-up of
the reactor.

Heating of the SUPERCLAUS® Stage


1. Supply heating air at maximum flow via the start-up line (FO-1212) and E-1011 to the
SUPERCLAUS® reactor.

2. Commission HP steam to the fourth steam reheater E-1011 and commission its condensate
system. Ensure that control valve in the steam supply line is fully closed.

Put the heater carefully into operation by slowly admitting steam via the control valve bypass. Do
not open the control valve until the heater is sufficiently heated!

3. Commission the automatic temperature control system (TC-1201). Keep the temperature at TC-
1201 between 150°C and 180°C in order to obtain a gradual heating-up of the reactor.

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Start of Thermal Oxidiser

When the main burner is in operation, sufficient off-gas is produced to start heating-up procedure of the
thermal oxidiser.

Reference is also made to the “Description of the Logic System for Start-up and Shutdown Operation”.

1. Ensure that the emergency shutdown switches are in the correct position
(HS-1113A/B/C for the main burner and HS-1290A/B/C for the thermal oxidiser).

2. Reset the logic system for the thermal oxidiser by HS-1286.

3. Start one of the thermal oxidiser air blowers. Confirm that the blower vents properly to the atmosphere
to prevent surging.

4. Commission the instrument air supply for purging to prevent sooting of the flame scanner and sight
glasses.

5. The ignition sequence is started with an air purge of the thermal oxidiser and proceeds automatically
until ignition is obtained. Open ZV-1515 by actuating HS-1285. Ensure that the air flow is above the trip
setting of FI-1286. The purge is completed after 3 minutes. The air flow rates are following:

• FC-1285, primary air (2000 kg/h).


• FC-1287, staged air (7150 kg/h).
• FC-1288, secondary air (14900 kg/h).

6. When the purge is completed, the next step is automatically started. The ignitor is inserted and
energized and the fuel gas valves are opened. Within 5 seconds ignition should be obtained, otherwise
the unit is tripped.

7. In case ignition is hard to obtain at the pre-defined air flow rate, it can be manually increased within a
certain range by varying the output of controller FC-1285. The fuel gas flow rate is such that the
combustion is stoichiometric. In addition, the fuel gas flow (FC-1281) can be manually adjusted within a
certain range. The settings are determined empirically.

Remark

Normally the burner can be started quickly with the predefined positions on the air and fuel gas controllers.
These settings correspond with stoichiometric combustion. However, due to the actual burner dimensions
and location of the tip of the ignitor, it is sometimes easier to obtain ignition at other flow rates. This should
be empirically found. Once these flow rates have been adjusted in the DCS, they can be used for
subsequent start-ups.

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8. One minute after ignition following controllers are accessible for the operator.

• FC-1285, primary air.


• FC-1287, staged air.
• FC-1288, secondary air.
• FC-1281, fuel gas.

9. After establishing a stable flame, the size of the flame should be restricted. Decrease the fuel gas flow
to its minimum value of 119 kg/h and adjust the primary air flow to 6600 kg/h. This results in a “330% of
stoichiometric burn”, i.e. with 230% excess air. Switch FC-1281 (fuel gas), FC-1285 (primary air), FC-
1287 (staged air) and FC-1288 (secondary air) to AUTO mode. After switching FC-1285 to CASCADE,
the ratio between fuel gas and air can be adjusted with HC-1283. The staged air flow on FC-1287 and
the secondary air flow on FC-1288 should initially be maximum to provide as much cooling as possible.

Remark

During the initial start-up the off-gas from the main burner provides sufficient cooling, so that a gradual
heating-up is obtained. Once the refractory in the thermal oxidiser is dried-out, a faster temperature rise is
allowed. Therefore, at the next start-up the thermal oxidiser is started before the main burner.

Drying out and Heating up of the Reaction Furnace


10. After about 52 hours the drying out phase is complete (see figure 2) and the heating up of the reaction
furnace can commence. The reaction furnace is heated up to about 1000°C at a rate of 20°C per hour
by adjusting the air and fuel gas flows to the main burner. To restrict the temperature rise, quenching
steam should be admitted to the burner. The steam supply is started with HS-1111, but not before all
temperatures in the unit exceed 100°C.

11. The generation of steam from the waste heat boiler starts with increasing heat input. When a large
amount of steam is exhausted, the vent is closed.

Check again that the condensate disposal system has been correctly commissioned.

Drying-out and Heating-up of the Reactor Stages


1. During the first 24 hours of operation, the outlet temperature of the reheaters should be limited to 150-
180°C. After this period the reactors are heated to the maximum temperature that can be obtained with
the reheaters at 15°C - 20°C per hour.

2. The generation of steam from the condensers starts gradually. When a large amount of steam is

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exhausted, the vent is closed. Operate the condensers at their normal operating pressure. The steam
pressure in the SUPERCLAUS® condenser is however 4 kg/cm2 (ga). It may be necessary to maintain
this pressure by additionally supplying LP steam into the bottom of the condenser. If LP steam is
supplied to the condenser, blow-down water has to be drained off as well.

Drying out and Heating up of the Thermal Oxidiser


After about 52 hours the drying out phase is complete (see figure 2) and the heating up of the thermal
oxidiser can commence.

The thermal oxidiser is heated up to about 750 °C at a rate of 10 °C per hour by adjusting the air and fuel
gas flows to the burner, as well as the staged air flow and secondary air flow.

Inspection of refractory
To be sure that refractory curing has been successful it is recommended to inspect the refractory of the
reaction furnace and the thermal oxidiser. A good opportunity to do this is during the time of catalyst loading
since the unit has to be cooled down to make this possible anyway.

3.3.2.2 Handling, storage and loading of Catalyst

After the initial drying-out and heating-up procedure, the unit is shut down to allow opening of the equipment
to start loading of catalyst into the reactors.

Stopping the unit


1. Decrease gradually the temperature in the reaction furnace by reducing the fuel gas supply. Adjust
an excess of air of approximately 200%.

2. Cool down the catalyst beds of the reactors by shutting-off the steam reheaters. Also shut-off the air
preheater.

3. Close the steam supply to the SUPERCLAUS® condenser and the blow-down valve.

4. The unit will gradually cool down.

5. Close the fuel gas supply to the main burner with HS-1110. The air is automatically tripped as well.

6. Shutdown the thermal oxidiser.

7. Reset the logic system for the main burner by HS-1108.

8. Open the air supply to the main burner with HS-1115. Adjust an initial air flow rate of 30% on FC-
1081. Gradually increase the air flow to maximum. Both control valves FV-1081 and XV-1077 can
be used.

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9. Install spectacle blinds in the fuel gas at the battery limit.

10. When the temperature is no longer decreasing, open the upper manhole on the reactor.

11. As soon as the reactor temperatures are sufficiently low, catalyst loading can take place.

Remark: During catalyst loading there is an opportunity to inspect the refractory of the reaction furnace and
thermal oxidiser after refractory curing.

Handling of Catalyst
Catalyst dust should not be inhaled. Dust masks should be worn by personnel who are outside the
converter during catalyst loading. Personnel inside the converter should wear a positive pressure air mask.
Eye contact and prolonged skin contact with the catalyst should be avoided by wearing relevant protective
clothing. Reference is made to the Catalyst Safety Datasheets in Section II.B.6.b).

The catalyst has to be protected against water.

Storage of Catalyst

The catalyst cannot withstand liquid water or air with a high water vapour content, after the catalyst has
been used to produce sulphur. It implies that the catalyst should be kept dry during a shutdown period, i.e.
the converter has to be purged with dry ambient air, and the manholes have to be closed to prevent ingress
of rainwater.

The catalyst is supplied in drums and can be stored outside, in vertical position, placed on pellets and
protected by a tarpaulin. Catalyst drums have to be closed carefully when the Superclaus® catalyst is
stored.

Catalyst Loading
1. Remove the pipe or bellow between the reactor outlet and the condenser inlet and place a
temporary blind at the condenser inlet. In this way, no catalyst dust will come into the condenser.

2. Check the interior of the reactor for cleanliness, with particular attention to the area beneath the
support grid.

3. Indicate on the wall the required heights for ceramic balls and catalyst. The height of the catalyst
bed is approximately 10% higher than indicated on the data sheet. After some time of operation, the

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bed height specified in the data sheet will be obtained as the catalyst density will increase to the
normal bulk packed density.

1. First Reactor

From the top of the grid support, the following heights are applicable:

a. Bottom layer (support balls): indication at 100 mm. The bottom layer (height: 100 mm) consists of
6 mm ceramic balls for support of the catalyst bed.

b. Bottom catalyst layer (CRS-31): indication at 460 mm. The bottom catalyst layer (normal height:
330 mm) consists of CRS-31 catalyst. Initially the catalyst bed is 10% higher than indicated on
the equipment drawing. The catalyst will shrink to its normal height after some time of operation.

c. Top catalyst layer (CR-3S): indication at 1480 mm. The top catalyst layer (normal height: 970
mm) consists of CR-3S catalyst. Initially the catalyst bed is 5% higher than indicated on the
equipment drawing. The catalyst will shrink to its normal height after some time of operation.

2. Second Reactor

From the top of the grid support, the following heights are applicable:
a. Bottom layer (support balls): indication at 100 mm. The bottom layer (height: 100 mm) consists of
6 mm ceramic balls for support of the catalyst bed.

b. Catalyst layer (CR-3S): indication at 1460 mm. The catalyst layer (normal height: 1300 mm)
consists of CR-3S catalyst. Initially the catalyst bed is 5% higher than indicated on the equipment
drawing. The catalyst will shrink to its normal height after some time of operation.

3. EUROCLAUS® Reactor

From the top of the grid support, the following heights are applicable:

a. Bottom layer (support balls): indication at 100 mm. The bottom layer (height: 100 mm) consists of
6 mm ceramic balls for support of the catalyst bed.

b. Catalyst layer (CRS-31): indication at 400 mm. The catalyst layer (normal height: 270 mm)
consists of CRS-31 catalyst. Initially the catalyst bed is 10% higher than indicated on the
equipment drawing. The catalyst will shrink to its normal height after some time of operation.

c. Catalyst layer (KF-756): indication at 550 mm. The catalyst layer (normal height: 130 mm)
consists of KF-756 catalyst.

d. Catalyst layer (CR-3S): indication at 1500 mm. The catalyst layer (normal height: 900 mm)
consists of CR-3S catalyst. Initially the catalyst bed is 5% higher than indicated on the equipment
drawing. The catalyst will shrink to its normal height after some time of operation.

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4. SUPERCLAUS® Reactor

From the top of the grid support, the following heights are applicable:

a. Bottom layer (support balls): indication at 50 mm above the support grid. The bottom layer (height:
50 mm) consists of 6 mm Denstone or Duranit balls for support of the catalyst bed.

b. Second layer (support balls): indication at 50 mm above the support grid. The second layer
(height: 50 mm) consists of 3 mm Denstone or Duranit balls for support of the catalyst bed.

c. Catalyst bed: indication at 870 mm above the support grid. The initial catalyst bed height is
approximately 770 mm; the normal bed height 700 mm. The catalyst will shrink to its normal
height after some time of operation.

d. Top layer: indication at 920 mm above the support grid. The top layer (height: 50 mm) consists of
6 mm Denstone or Duranit balls on top of the catalyst bed.

5. Special Loading Procedure for SUPERCLAUS® Reactor


The catalyst should be protected from contact with water (such as rain and condensate). It is advisable to
delay loading during rainfall. Ensure no rain water can enter the reactor via the manholes.

4. If a deviation of following reactor loading procedure is proposed, approval shall be obtained from
JNL.

a. Load the support balls to the specified and marked height.

b. Install the catalyst sample baskets beneath the manhole. The sample baskets are placed on
the catalyst support balls and are filled with catalyst equal in height to the catalyst bed.

c. Load the SUPERCLAUS® catalyst via the manhole of the reactor using a bucket or sock (figure
3). All supplied catalyst shall be loaded. The procedure is as follows:

d. Load the SUPERCLAUS® catalyst in small layers to the specified and marked height. Level
every layer. Use a ventilator to discharge the catalyst dust to outside of the reactor.

e. Levelling of the catalyst is done gently using a rake. Do not tread, sit or lie down directly on the
catalyst. Use a “temporary work floor” of planks to move in the reactor.

f. Special care shall be taken when reaching a thermowell to prevent damage.

g. Load ceramic balls on top of the catalyst bed. Use planks during loading to prevent damage of
the catalyst (figure 3 and 4).

h. After the reactor has been loaded, catalyst dust and fines have to be removed by an air flow
from the blower through the reactor. Then, close the reactor.

i. Reinstall the pipe or bellow between the reactor and condenser.

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j. Make a report of the catalyst loading with regard to the number of drums loaded (ceramic balls
as well as catalyst) and take samples of the ceramic balls and catalyst.

5. On completion of catalyst loading, check that the surface area has been levelled. Measure in
several places inside each reactor the height of the free space from the catalyst surface to the top
of the reactor.

6. After the first reactor has been loaded, dust and fines should be removed by an air flow from the
blower through the reactor. Next, the reactor is closed.

7. Reinstall the pipe or bellow between the reactor and condenser.

8. Removal of dust from the second reactor should take place when the first reactor has been closed.
This is repeated for all reactors.

9. Make a report of the catalyst loading, mention the number of drums and take samples of the
catalyst. Do the same for the ceramic balls.

10. After catalyst loading and leak testing of the reactors, the unit is heated up again.

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CATALYST BAG

RECEIVING HOPPER

Figure 3: Loading of SUPERCLAUS® reactor

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TEMPORARY WOODEN FLOOR

MANHOLE INLET LAYER OF SUPERCLAUS® CATALYST


TEMPORARY BAFFLE

2 m APPROX.
6 mm BALLS

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Figures 4 and 5: Loading of SUPERCLAUS® reactor

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General remarks
• Care must be taken to minimize the creation of catalyst fines during the loading of the reactors.
Catalyst dust and fines are to be removed with the help of an air flow through the reactor. For this
reason, the pipe between reactor outlet and condenser inlet should be removed and a temporary
blind at condenser inlet should be installed. This procedure has to be followed for each reactor
separately.

• During catalyst loading some dust is produced which should not be inhaled.
Personnel who are outside the reactor during loading should wear dust masks. Inside the reactor, a
positive pressure air mask should be worn. Eye contact and prolonged skin contact with the catalyst
should be avoided by wearing the relevant protective clothing.

• The catalyst bed heights indicated on the reactor walls are approximately 10% higher than
indicated on the equipment drawings. After some time of operation, the values of the equipment
drawings will be obtained when the catalysts have been settled.

• The catalyst should be protected against water.

3.3.2.3 Treatment of catalyst

c.1) Claus Catalyst Reactivation

Sulphate reduction (rejuvenation)

The main cause of ageing of alumina type catalyst is the formation of "superficial sulphate" by the reaction
of sulphur dioxide (present in the process gas) with the alumina of the catalyst whether in the presence of
oxygen or not.

When the SRU is operated in the SUPERCLAUS® mode, i.e. with an excess of H2S in the process gas, the
rate of ageing is considerably smaller.

This interaction between sulphur dioxide, oxygen and alumina is greater at higher temperature and partial
pressure of oxygen. Reversibly a reduction by hydrogen sulphide or by a mixture of H2S and SO2 starts at
elevated temperatures.

The velocity of this reduction reaction is fairly high in the range of 250 - 300°C compared to the velocity of
the sulphation reaction.

When contacted with H2S the superficial sulphate reacts to sulphur and water.

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As long as the surface area of the catalyst is above 150 m2/g and the activity decrease is the result of an
incidental sulphation, an improvement can be expected by operating the second reactor as follows:

• Increase the H2S content in the gas to the reactor to 2 - 3 vol.%

• Increase the reactor inlet temperature to the maximum possible.

• Maintain these conditions for at least 24 hours.

An increase of the H2S content in the gas to the second reactor is obtained by operating the main burner
with a deficiency of air. Therefore, an adjustment of the ratio air-to-feed gas or set point of the H2S analyser
controller has to be made.

In order to reach the maximum temperature in the reactor, the steam supply to the reheater is fully open
and the plant throughput is decreased to approximately 50% of the design feed. Catalyst reactivation is
advised after each shutdown operation.

The first reactor contains a titanium-based catalyst (CRS-31), which is insensitive for sulphation, with a top
layer of alumina type catalyst (CR-3S). The top layer protects the titanium catalyst against soot deposition.
Because of the elevated temperature in the first reactor and the high H2S content, sulphation of the top
layer will hardly occur.

Sulphur removal (heat soak)

During operation, sulphur is absorbed inside the pores of the catalyst. This has no adverse effect on the
performance of the plant. When, however, during operation the bed temperature is lower than the sulphur
dew point, sulphur condenses on the surface of the catalyst, which reduces the catalyst activity. This
applies only for the catalyst in the 2nd and 3rd reactor as the 1st reactor operates always far above the
sulphur dew point.

The dew points of the gas leaving the 1st, 2nd and 3rd reactors are 254°C, 213°C and 181°C, respectively.

As soon as a decline in temperature difference over a reactor becomes noticeable from the daily operating
figures, the most likely reason is that too much sulphur has accumulated on the catalyst.

To remove the sulphur from the concerned catalyst bed, the reactor inlet temperature should be increased
to maximum for a period of at least 24 hours.

c.2) EUROCLAUS® Catalyst


The active components of the EUROCLAUS® catalyst are the cobalt and molybdenum sulphides. The
catalyst is supplied by the manufacturer with the cobalt and molybdenum in the oxidic form and therefore
presulphiding is required. Contact of the catalyst with H2 at temperatures higher than 200°C prior to

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presulphiding should be avoided in order not to impair catalyst activity. The sulphur content of the
presulphided catalyst is approximately 6 wt% but the amount taken up during presulphiding may be less
than this.

The catalyst is presulphided with H2S containing process gas in the presence of hydrogen.

During the first two hours of presulphiding some sulphur is present in the reactor effluent.

1. When the Sulphur Recovery Unit is warmed up and acid gas is feeding the unit, presulphiding can
commence.

2. Raise the temperature in the catalyst bed to 240°C at the bottom and maintain for 24 hours.

3. The reaction is exothermic, therefore care must be taken not to overheat the catalyst.

4. After 24 hours reduce the reactor inlet temperature to the normal value of 195°C.

Remark
It is advised to presulphide the EUROCLAUS® catalyst after each shut down period.

c.3) SUPERCLAUS® Catalyst

Storage of SUPERCLAUS® catalyst

The SUPERCLAUS® catalyst cannot withstand liquid water or air with a high water vapour content, after
the catalyst has been used to produce sulphur. It implies that the SUPERCLAUS® catalyst should be kept
dry during a shutdown period, i.e. the reactor has to be purged with dry ambient air, and the manholes have
to be closed to prevent ingress of rainwater.

The catalyst is supplied in drums and can be stored outside, in vertical position, placed on pellets and
protected by a tarpaulin.

Catalyst drums have to be closed carefully when the SUPERCLAUS® catalyst is stored.

Heating up of SUPERCLAUS® bed

The SUPERCLAUS® catalyst bed should be heated before process gas is routed over it in order to prevent
sulphur and water condensation on the cold catalyst bed. Therefore, all start-ups should include the
following procedure.

When the SUPERCLAUS® catalyst bed is cold it should be heated-up by directing hot air via the air start-
up line to the SUPERCLAUS® stage. The maximum air flow is adjusted. The valve ZV-1511 (process gas
to SUPERCLAUS® reactor) is closed and the SUPERCLAUS® bypass valve ZV-1512 is open. The catalyst

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bed temperature should be at least 170°C, which is slightly above the sulphur dew point of the process gas
leaving the 4th sulphur condenser.

Initial start-up of SUPERCLAUS® stage.

Under normal operating conditions the SUPERCLAUS® catalyst is very selective for the conversion of H2S
to sulphur. However, when the catalyst is new it has not yet obtained its selectivity and will consequently
oxidize the H2S to SO2 instead of to sulphur. For this reason, the catalyst should be conditioned (sulphated)
first. This should be done carefully, since this operation mode is sensitive for runaways. Therefore, the
catalyst conditioning should be carried out as shown below in figure 1, increasing gradually the H2S and
inlet temperature at a feed gas load of at least 50-70% of the design throughput. Prior to switching from
SUPERCLAUS® bypass to SUPERCLAUS® in line mode the SUPERCLAUS® reactor should be heated
up 180°C. Simultaneously maximum oxidation air is supplied to the SUPERCLAUS® reactor.

To avoid the risk of plugging, the SUPERCLAUS condenser should initially be operated as hot as possible.
This can be realized by putting the steam pressure controller of the SUPERCLAUS condenser at a pressure
of 4 kg/cm2g .

At process gas intake, the temperature in the SUPERCLAUS® reactor will rise as a result of exothermic
reactions, which will largely disappear when the catalyst has obtained its selectivity. A reactor outlet
temperature of 260°C to 280°C can be expected in this period of operations.

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®
SUPERCLAUS STARTUP

0.8
0.7
0.6
H2S (vol%)

0.5
0.4
0.3
0.2
0.1
0
0 24 48 72 96 120 144 168 192
TIME (H)

Figures 5 & 6. Initial Start-up of SUPERCLAUS.

SUPERCLAUS® STARTUP
INLET TEMP (°C)

205
200
195
190
185
180
175
0 24 48 72 96 120 144 168 192
TIME(H)

When the catalyst is conditioned, the oxidation air will be slowly reduced to obtain an O2 content in the gas
leaving the sulphur coalescer at 0.5 vol.%. The steam pressure in the sulphur condenser can be reduced
from 4 kg/cm2g to 0.81 kg/cm2g after 2 weeks of stable operation. It is of major importance to verify the
readings of the analysers by Dräger tubes or laboratory analyses. In order to optimize the recovery, the inlet
temperature should be changed in steps of 5°C from 190°C up to 210°C determining at each step the H2S
concentration in the tail gas. The lowest value of (H2S+SO2) concentration will result in the highest
recovery. In the design case of this unit the H2S content to the SUPERCLAUS® stage is 0.58 vol.% (on a
wet basis), the inlet temperature is 210°C and the reactor outlet temperature is approximately 249°C.

For a quick check of the SUPERCLAUS® performance it is advised to take Dräger samples of the in- and
outlet of the SUPERCLAUS® stage every week. As a rule of thumb the temperature rise over the
SUPERCLAUS® bed in a good performing SUPERCLAUS® stage is about 70°C per percent of H2S in the
gas (on wet basis) to the SUPERCLAUS® stage. Less active catalyst requires a higher inlet temperature for
complete H2S conversion than fully active catalyst.

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The selective oxidation catalyst requires an oxidizing atmosphere to maintain a high sulphur yield.
Therefore the air required for the oxidation has to be supplied in excess. If this operation mode is
maintained properly there is no risk that the catalyst will be sulphided. If not, the sulphur yield may decrease
as a result of catalyst sulphidation. For protection of the catalyst, a low oxidation air flow trip will bypass the
SUPERCLAUS® stage.

The catalyst has been safeguarded against a temperature run-away of the catalyst bed by temperature trips
in the reactor. In such a case the SUPERCLAUS® stage is bypassed.

The trip value depends on the position of the thermocouples in the reactor catalyst bed. Moreover, the bed
is safeguarded against too high an H2S concentration in the process gas to the SUPERCLAUS® stage. If
this concentration is higher than 2.0 vol.% for more than 2 minutes, the stage is bypassed. This has been
done to limit the temperature rise in the bed. A too high a bed temperature would decrease the yield of the
stage anyway. In such a case it is better to bypass the stage and lower the bed temperature with the start-
up air, than running for a longer time with too high bed temperatures.

The inlet temperature of the 4th reactor is typically 210°C at design capacity, and slightly lower at
decreased plant load (190 - 195°C). For this reactor, try to maintain the outlet temperature below 280°C
whilst the temperature development across the reactor bed for the top part is 70% of the total temperature
rise and for the bottom part 30%. If the difference between the bottom and middle temperature is low, this is
the indication, that the inlet temperature is too high. Moreover, the H2S slip out of the SUPERCLAUS®
reactor is then lower than the 200 and 300 ppm vol., which is required for an optimum performance of the
SUPERCLAUS® stage. The SUPERCLAUS® temperature controller tries to control the inlet temperature at
the optimum ΔT over the first part of the bed, whilst a set point limiter makes sure that the outlet
temperature does not become higher than 280°C.

3.3.2.4 Heating Up after Shutdown

Preparations

1. Ensure that the unit is leak-tight, that all utility systems are commissioned and that equipment is
ready for start-up (e.g. sufficient levels in waste heat boiler and condensers).

2. Ensure that the sulphur seals are filled with sulphur.

3. All isolating blinds situated at the unit and battery limits are removed, except at the acid feed gas
lines.

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Start of Thermal Oxidiser


1. Ensure that the emergency shutdown switches are in the correct position (HS-1113/1114 for the
main burner and HS-1290/1291 for the thermal oxidiser).

2. Reset the logic system for the thermal oxidiser by HS-1286.

3. Start one of the thermal oxidiser air blowers. Confirm that the blower vents properly to the
atmosphere to prevent surging.

4. Ensure that fuel gas for the thermal oxidiser burner is available (PI-1305).

5. Commission the instrument air supply for purging to prevent sooting of the flame scanner and sight
glasses.

6. The ignition sequence is started with an air purge of the thermal oxidiser and proceeds
automatically until ignition is obtained. Open ZV-1515 by actuating HS-1285. Ensure that the air flow is
above the trip setting of FI-1286. The purge is completed after 3 minutes. The air flow rates are the
following:

• FC-1285, primary air (2000 kg/h).


• FC-1287, staged air (7150 kg/h).
• FC-1288, secondary air (14900 kg/h).

7. When the purge is completed, the next step is automatically started. The ignitor is inserted and
energized and the fuel gas valves are opened. Within 5 seconds ignition should be obtained, otherwise the
unit is tripped.

In case ignition is hard to obtain at the pre-defined air flow rate, it can be manually increased within a
certain range by varying the output of controller FC-1285. The fuel gas flow rate is such that the combustion
is stoichiometric. In addition, the fuel gas flow (FC-1281) can be manually adjusted within a certain range.
The settings are determined empirically.

8. One minute after ignition following controllers are accessible for the operator.

• FC-1285, primary air.


• FC-1287, staged air.
• FC-1288, secondary air.
• FC-1281, fuel gas.

9. After establishing a stable flame, the size of the flame should be restricted. Decrease the fuel gas
flow to its minimum value of 119 kg/h and adjust the air flow to 6600 kg/h. This results in a “330% of
stoichiometric burn”, i.e. with 230% excess air.

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Switch FC-1281 (fuel gas), FC-1285 (primary air), FC-1287 (staged air) and FC-1288 (secondary air) to
AUTO mode. After switching FC-1285 to CASCADE, the ratio between fuel gas and air can be adjusted
with HC-1283. The staged air flow on FC-1287 and secondary air flow on FC-1288 should initially be
maximum to provide as much cooling as possible.

10. When the temperature in the thermal oxidiser is sufficiently high (250°C) FC-1281 is switched to
CASCADE.

Start of Main Burner


1. Start one of the air blowers. Confirm that the blower vents properly to the atmosphere to prevent
surging.

2. Check the permissives to start the main burner.

• Check the liquid level in the waste heat boiler (LI-1225).


• Ensure that fuel gas for the main burner is available (PI-1089).
• Ensure that the inlet valve ZV-1511 of the SUPERCLAUS® stage is closed and that ZV-1512
in the bypass is open.

3. Reset the logic system for the main burner by HS-1108.

4. Commission the nitrogen for purging the flame scanners and sight glasses to prevent sooting.

5. The ignition sequence is started with the nitrogen purge of the main burner and proceeds
automatically until ignition is obtained. Within 15 minutes after purging, a flame should be established. Start
the ignition procedure by actuating button HS-1109. Ensure that the nitrogen flow is above the trip setting of
FI-1087. The purge is completed after 5 minutes.

6. When the purge is completed, the next step is automatically started. The ignitor is inserted, the
combustion air supply is started, the ignitor is energized and the fuel gas valves are opened. Within 5
seconds ignition should be obtained, otherwise the unit is tripped. The air flow rate is normally the minimum
allowable air flow to the burner. In case ignition is hard to obtain with this flow rate, it can be manually
increased within a certain range by varying the output of controller FC-1081. The fuel gas flow rate is such
that the combustion is stoichiometric. In addition, the fuel gas flow (FC-1088) can be manually adjusted
within a certain range. The settings are determined empirically.

Remark

Normally the burner can be started quickly with the predefined positions on the air and fuel gas controllers.
These settings correspond with stoichiometric combustion at the minimum air flow with the corresponding
fuel gas flow. However, due to the actual burner dimensions and location of the tip of the ignitor, it is
sometimes easier to obtain ignition at other flow rates. This should be empirically found. Once these flow

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rates have been adjusted in the DCS, they can be used for subsequent start-ups.

7. One minute after ignition following controllers are accessible for the operator.

• FC-1081, acting on the trim air valve.


• XC-1077, acting on the main air valve.
• FC-1088, fuel gas.

After establishing a stable flame, the size of the flame is restricted. Decrease the fuel gas flow to its
minimum value of 72 kg/h and adjust the air flow to 4019 kg/h. This results in a “330% of stoichiometric
burn”, i.e. with 230% excess air.

Switch FC-203 (fuel gas) and FC-155 (total air) to AUTO mode.

After switching FC-1081 to CASCADE, the ratio between fuel gas and air can be adjusted with HC-1090.
XC-1077 can be taken into operation to allow the operator to increase the air flow during warming-up.

(See also the remark on next page).

Heating of the Claus and EUROCLAUS® Reactors

1. Commission HP steam to the steam reheaters E-1005, E-1007 and E-1009. Commission their
condensate systems. Ensure that the control valves in the steam supply lines are fully closed. Put the
heaters carefully into operation by slowly admitting steam via the control valve bypass. Do not open the
control valve until the heater is sufficiently heated!

2. Commission the automatic temperature control systems (TC-1145, TC-1167 and TC-1184). The
reactors are heated at a rate of 15-20°C per hour until a top temperature of 240°C is reached.

Heating of the SUPERCLAUS® stage

1. Commission HP steam to the fourth steam reheater E-1011 and commission its condensate
system. Ensure that control valve in the steam supply line is fully closed.

Put the heater carefully into operation by slowly admitting steam via the control valve bypass. Do not open
the control valve until the heater is sufficiently heated!

2. Supply heating air at maximum flow via the start-up line (FT-1212) and E-1011 to the
SUPERCLAUS® reactor.

3. Commission the automatic temperature control system (TC-1201). Keep the temperature at TC-
1201 between 150°C and 180°C in order to obtain a gradual heating-up of the reactor. The temperature of
the SUPERCLAUS® reactor is maintained at 170 - 180°C.

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For the reaction furnace and the thermal oxidiser, the temperature increase should be limited to 15 - 20°C
per hour until a temperature of 300°C is reached.

Hereafter, they can be heated up more rapidly (approx. 50°C per hour) to temperatures of 1300°C and
750°C, respectively.

Remarks

Please note that the above procedure only applies when the unit does not contain sulphur, since excess air
is introduced. At temperatures above 200°C in combination with the presence of sulphur, excess air may
lead to sulphur fires.

Reference is made to Section III.C.4 "Actions in case of automatic shutdown (Trip)" for the start-up
procedures in case sulphur is present in the unit. The presence of sulphur in the unit after a shutdown
should be avoided. Reference is made to Section II.C.4 for the proper shutdown procedures.

After a trip, the unit is brought on-stream as soon as possible. Then the unit is still hot, so introduction of
excess air for cooling is not required and should be avoided. Fuel gas shall be burnt substoichiometrically,
see also remark a, steam can be used to quench the flame if this should be necessary.

3.3.2.5 Check List and Preparation before Feed Gas Intake

1. Confirm that following items have been completed before feed gas intake.

2. Open the sulphur outlets of the sulphur condensers and coalescer.

3. Commission HP steam to the air and acid gas preheaters and commission their condensate
systems. Put the heaters carefully into operation: admit slowly steam to the heaters.

4. Confirm steam supply to the steam tracing and jacketing by means of temperature indicating stick
for 125°C or lumps of sulphur.

5. Check all steam traps, especially at the jackets of sulphur run-down lines.

6. Remove the blinds in the acid feed gas feed lines. The battery limit valves remain closed.

7. Check the burner flanges and sight glasses for leaks.

Check the availability of the following Dräger tubes for tail gas analyses:

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Component(s) Range
H2S 0.2 - 7 vol.%
H2S 100 - 2000 ppm vol
(H2S + SO2) 0.2 - 7 vol.%
SO2 50 - 8000 ppm vol
1. Prepare safety measures before start-up:

• Make at least 4 air masks available.


• Make air bottle available for refilling of air mask bottles or make air supply lines with filter
available, depending on the type of the mask.
• Check wind direction.
• Provide operating personnel with portable H2S detectors (personnel protection).
• Close to sulphur plant area to personnel during start-up, except for operating personnel.

2. Ensure that the burners are in stable operation and on automatic control.

3. Check following temperatures and pressures:

Reaction furnace 1000 - 1300 °C


Claus reactors inlet 240 °C
EUROCLAUS® reactor inlet 230 °C
SUPERCLAUS® reactor inlet 150 - 180 °C
SUPERCLAUS® condenser 4 kg/cm2 (ga)
Thermal oxidiser 750 - 800 °C

4. Check the supply of air and nitrogen for purging the flame scanners and the sight glasses.

5. Make tools such as locks, keys, valve handles, wrenches, sealing tape and soap for leak testing
available.

6. Check if the H2S monitor for personnel protection has been commissioned and set at the correct
alarm setting.

7. Ensure that the sulphur seals are filled with liquid sulphur.

8. Commission the tail gas analyser.

a. Take care that a portable O2 analyser for stack gas is available.

b. Check the level in the amine acid gas knock-out drum D-1001.

c. Check the level in the SWS gas knock-out drum D-1002.

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d. Commission steam to the ejectors on the sulphur pit. It is advised to start now the steam
ejectors (see Section 3.3.2.8 “Start-up of sulphur degassing system”).

3.3.2.6 Feed Gas Intake

Simplified Outline
1. Adjust the air and fuel gas flows to the main burner.
2. Adjust the "air-to-amine acid feed gas" ratio as well as the "air-to-SWS acid feed gas" ratio.
3. Admit amine acid feed gas to the main burner.
4. Switch the flow control for the amine acid feed gas to AUTO and gradually increase its feed gas
flow.
5. Stop the fuel gas supply to the main burner when desired.
6. Regenerate the Claus catalyst if required.
7. Increase the feed gas flow to the maximum available quantity.
8. Adjust the inlet temperatures of the Claus and EUROCLAUS® reactors to design conditions.
9. Admit SWS acid feed gas when desired.
10. Bring the SUPERCLAUS® reactor on stream when desired.
Detailed Outline

Adjusting air and fuel gas

Adjust the fuel gas combustion in the main burner to 95% of stoichiometric combustion (HC-1090). Note
that FC-1081 is in CASCADE mode and that XC-1077 should be switched to CASCADE before feed gas
intake.

Taking in Amine acid feed gas

1. Pre-adjust the “air to acid gas” ratio for HC-1038 (Amine acid feed gas) to 3.0 kg air/kg feed gas
and for HC-1045 (SWS acid feed gas) to 2.30 kg air/kg feed gas.

2. Open the battery limit valves in the Amine acid feed gas and SWS acid feed gas feed lines.

3. Start the Amine acid feed gas supply to the main burner with HS-1116.

4. Within 30 seconds the feed gas flow must be established. The air flow follows automatically the
feed gas flow. The initial feed gas flow is 2300 kg/h (20% of the design flow).

5. 60 seconds after establishing the Amine acid feed gas flow, the flow controller FC-1038 becomes
accessible for the operator. Switch it to AUTO mode.

6. Increase the feed gas flow to 30% by adjustment of the set point of FC-1038. The air flow will

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follow automatically.

7. Increase the feed gas flow to 40%.

8. Check the H2S content in the process gas from the fourth condenser with Dräger tubes and
compare this with the H2S analyser.

9. Slowly decrease the “air to acid gas” ratio for HC-1038 (Amine acid feed gas) to 2.0 kg/kg.

10. Ensure that sulphur is running by opening the funnels. Use air masks and eye protection
equipment.

11. Check the O2 content of the thermal oxidiser flue gas with Dräger tubes or portable analyser. It
should be approx. 2.1% by volume.

13. As soon as the unit runs stable, the fuel gas supply to the main burner can be stopped. Decrease
the fuel gas flow with FC-1088. Stop the fuel gas supply with HS-1110 and close the quenching steam with
HS-1111 in case it was in operation.

Note that the temperature in the reaction furnace must be kept above 1250°C when firing amine acid gas in
order to destroy all ammonia.

14. Increase the amine acid gas flow to maximum. When desired switch FC-1038 to CASCADE with
the pressure controller that is located in the upstream amine unit.

15. Decrease the Claus and EUROCLAUS® reactor inlet temperatures to the normal value of 240°C
(first reactor), 210°C (second reactor) and 195°C (third reactor).

16. Switch AC-1083 to AUTO mode to maintain the H2S value at 0.58 vol.% at the outlet of the
EUROCLAUS® reactor.

Taking in SWS Acid Feed Gas

1. Start the SWS acid feed gas supply with HS-1117.

2. Within 30 seconds the SWS acid feed gas flow must be established. The air flow follows
automatically the increased amount of feed gas flow. The initial SWS acid gas flow is 310 kg/h (20% of the
design flow).

3. 60 seconds after establishing the SWS acid feed gas flow, the flow controller FC-1045 becomes
accessible for the operator. Switch it to AUTO mode.

4. Increase the SWS acid feed gas flow. When desired switch FC-1045 to CASCADE with the
pressure controller that is located in the SWS unit.

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3.3.2.7 Taking the SUPERCLAUS® Stage into operation

1. After stable operation of the two Claus reactor stages and EUROCLAUS® reactor stage has been
established and the bed temperature of the SUPERCLAUS® reactor is above 170°C, the SUPERCLAUS®
stage can be brought on-stream. Air is still supplied to the SUPERCLAUS® stage via the start-up line with
FT-1212.

2. To avoid risk of plugging, the SUPERCLAUS® condenser initially should be operated at an


elevated pressure. This is realized by controlling the steam pressure at 4 kg/cm2 (ga). After a period of
stable operation (e.g. 2 weeks), the steam pressure can be reduced to the normal value of 0.81 kg/cm2
(ga).

3. Reduce slowly the setpoint of AC-1083 to a H2S value of 0.20 vol.% in the outlet of the
EUROCLAUS® reactor. (If necessary increase the “air to acid gas” ratio to achieve this H2S value of 0.20
vol.%.)

4. Open the hand valves in the oxidation air line. Since the oxidation air control valve is fully open
(the output from controller FIC-1201 corresponds to the open position), part of the air flows now directly into
the process gas line upstream the 4th reheater. Switch FIC-1201 to AUTOMATIC mode with maximum air
flow.

5. Close the valve downstream FO-1212 in the start-up air line.

6. Watch the SUPERCLAUS® reactor temperatures carefully.

7. Open ZV-1511 by HS-1202, thereby admitting process gas to the SUPERCLAUS® reactor. As
soon as ZV-1511 is fully open, ZV-1512 in the bypass is automatically closed.

8. The temperatures of the SUPERCLAUS® reactor will rise as a result of exothermic oxidation
reactions. During the first few hours of operation the SUPERCLAUS® catalyst will produce mainly SO2.
However, the selectivity of the catalyst will gradually increase.

9. Check the oxygen concentration with Dräger tubes after the reactor temperatures have stabilized
and turned to their normal values and the sulphur production starts.

10. Condition the catalyst according to Figures x and y. After conditioning, adjust the set point of the
H2S controller AC-1083 to optimum conditions (H2S = 0.58 vol.%). The corresponding design “air to acid
gas” ratio for HC-1038 (Amine acid feed gas) is 1.38 kg/kg and for HC-1045 (SWS acid feed gas) 2.30
kg/kg.
Make a complete check of all temperatures throughout the unit.

11. Slowly reduce the supply of oxidation air to normal value and switch the flow controller for the
oxidation air to CASCADE mode.

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Slowly adjust the SUPERCLAUS® reactor inlet temperature to the normal value of 190-210°C.

12. When the SUPERCLAUS® reactor temperatures have been stabilized and the throughput is more
than 30% of the design value, the steam supply to the final condenser can be stopped. Adjust the water
level in the condenser and close the boiler water drain valve. Decrease the set point of PC-1217 in the
steam line to the steam condenser to its normal value. (See figures 5 and 6)

Important Criteria for SUPERCLAUS® Stage Operation

1. Check that the O2 content in the outlet of the SUPERCLAUS® reactor is 0.5 vol.%. It should be
measured by Dräger tubes or a portable O2 analyser.

2. Maintain the ABC system well functioning in accordance with the Process Control Narrative.

3. Maintain about 0.58 vol.% H2S in the feed gas to the SUPERCLAUS® stage.

4. Maintain the inlet temperature of the SUPERCLAUS® reactor at 200-210°C (depending on plant
load).

5. Ensure that the H2S slippage in the gas from the SUPERCLAUS® reactor is approx. 250 ppm vol.
Use Dräger tubes.

6. Check the temperature profile in the SUPERCLAUS® reactor bed. The temperature should
increase equally over the whole depth of the bed, resulting in a more or less straight line.

7. Maintain the outlet temperature of the SUPERCLAUS® sulphur condenser at 125°C and the
steam pressure at 0.81 kg/cm2 (ga).

Remark

At subsequent start-ups, the SUPERCLAUS® catalyst is already stabilized. Then it is not required to start
with low H2S concentrations. The normal H2S setting can be used before switching from
Claus/EUROCLAUS® to SUPERCLAUS® operation.

3.3.2.8 Start-up of Sulphur Degassing System

It is assumed that the degassing system is commissioned.

Initial Start-up or Start-up after a Long Shutdown

The ejectors EJ-1001 A & B can be started as soon as the main air and the thermal oxidiser air blowers are
in operation. Both ejectors should initially be in operation to obtain a high vent air flow rate, since a high
amount of H2S is released immediately after admitting the stripping air.

Reset the degassing logic system with HS-1246.

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1. Open the steam supply to the ejectors with HS-1244. The vent air flow should exceed the set
point of FI-1251A within 60 seconds, otherwise the steam is stopped.

2. As soon as the bubble columns are completely submerged, the stripping air supply is started with
HS-1245. The stripping air flow should exceed the set point of FI-1238 within 60 seconds. If not, the
stripping air is stopped.

Adjust locally a stripping air flow of 288 kg/h to each bubble column on FI-1235 and FI-1236.

3. 60 minutes after starting the stripping air, the logic system allows to shut-down one of the ejectors.
However, it is advised to continue with both ejectors for a few hours during initial start-up, as the degassing
process is not efficient as long as the sulphur level is below its normal value.

4. Check the sulphur temperature in the stripping compartment frequently. It should be between
130°C and 155°C near the 2nd bubble column Z-1001B.

Start-up after Short Interruption

There is no need to start the second ejector after an interruption of the degassing process of less than one
hour. Then the system is restarted according to the following procedure:

1. Reset the degassing logic system with HS-1246.

2. Open the steam supply to the ejectors with HS-1244. The vent air flow should exceed the set
point of FI-1251B within 60 seconds, otherwise the steam is stopped.

3. Start the stripping air supply with HS-1245. Within 60 seconds the stripping air flow should exceed
the set point of FI-1238. If not, the stripping air is stopped. Adjust locally a stripping air flow of 288 kg/h to
each bubble column on FI-1235 and FI-1236.

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3.3.3 Normal Operation

3.3.3.1 Operating Variables and Control

The following table lists the set points for the controllers in the unit (according to material balance included
in PFD’s):

Controller
Inst. Tag no. Service
setting
H2S content in the process gas at the outlet of the
AC-1183 0.58 %mol
EUROCLAUS® stage
FC-1038 Flow of amine gas to the Main Burner 11513 kg/h
FC-1045 Flow of SWS gas to the Main Burner 1531 kg/h
FC-1081 Total air to the Main Burner 23561 kg/h
Fuel gas to Main Burner during normal operation /start-up,
FC-1088 50-100 kg/h
shut down and hot stand-by operation
FC-1201 Oxidation air flow to SUPERCLAUS® stage 1399 kg/h
FC-1237 Oxidation air flow to Bubble Columns 512
FC-1253 Flow of Liquid Sulphur to B.L. 11529 kg/h
FC-1285 Primary air flow to Thermal Oxidiser Burner 7035 kg/h
FC-1287 Staged air flow to Thermal Oxidiser Burner 4397 kg/h
FC-1288 Secondary air flow to Thermal Oxidiser Burner 7593 kg/h
FC-1281 Fuel gas flow to Thermal Oxidiser Burner 617 kg/h
FC-1318 Flow of Condensate Flash recirculation 5252 kg/h
FC-1327 Flow of Blow down recirculation 15933 kg/h
LC-1001 Liquid level in Amine Gas KO Drum 1100 mm
LC-1013 Liquid level in SWS Gas KO Drum 775 mm
LC-1126 Water level in Waste Heat Boiler 850 mm
LC-1145 Water level in Sulphur Condensers E-1004/1006 1800 mm
LC-1167 Water level in Sulphur Condensers E-1008/1010 1800 mm
LC-1253 Level in Sulphur Pit 600 mm
LC-1316 Liquid level in Condensate Flash Drum 1650 mm
LC-1326 Liquid level in Blow Down Drum 1650 mm
PC-1304 Fuel gas pressure to Fuel Gas KO Drum 2.5 kg/cm2g
PC-1330 HP steam pressure 44.5 kg/cm2g
PC-1332 LP steam pressure 5.3 kg/cm2g
PC-1333 LP steam pressure 5.3 kg/cm2g
PC-1342 Nitrogen from refinery system 2.5 kg/cm2g
PC-1217 Steam pressure in 5th Sulphur Condenser 0.8 kg/cm2g
TC-1336 LP steam temperature 161 ºC

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Controller
Inst. Tag no. Service
setting
TC-1145 Process gas inlet temperature of 1st Reactor 240 ºC
nd
TC-1167 Process inlet temperature of 2 Reactor 210 ºC
rd ®
Process gas inlet temperature of 3 (EUROCLAUS )
TC-1184 195 ºC
Reactor
Process gas inlet temperature of 4th (SUPERCLAUS®)
TC-1201 210 ºC
Reactor
TC-1281 Temperature in the Thermal Oxidiser 750 ºC

Main Burner

For a detailed description and explanation of the combustion air control system (ABC system), reference is
made to the “Process Control Narrative”, document no. 1800-8120-PD-R310-2001.

For an optimum performance of the plant it is required that the correct amount of air is added in the burner
to the acid feed gas.

This amount of air is the air required for combustion of slightly less than 1/3 of the total H2S present in the
feed gas. The air is also required for the complete oxidation of other combustibles in the feed gas
(hydrocarbons, ammonia).

Under normal conditions the H2S concentration in the process gas to the SUPERCLAUS® reactor is
approximately 0.6 vol.% The SO2 content in the tail gas is then very low. Therefore the H2S concentration in
the tail gas from the fourth sulphur condenser is measured by an analyser (AT-1184) and subsequently
controlled by AC-1083.

This controller will adapt the air supply to the main burner to maintain the correct H2S concentration to the
SUPERCLAUS® stage. The SO2 produced in the main burner is converted in the Claus and EUROCLAUS®
reactors and consequently the SO2 content in the flue gas is very low.

In the hot standby mode only fuel gas is burned in the main burner. The combustion is slightly
substoichiometrical to avoid oxygen break-through to the reactor stages. Without cooling the flame
temperature would be too high. Therefore, steam as a cooling medium is injected into the flame. The steam
flow rate is approximately four times the fuel gas flow rate on weight basis.

Remark

When during normal operation (SUPERCLAUS® mode) feed gas is combusted with a deficiency of air, the
tail gas to the SUPERCLAUS® stage contains an excess of H2S. This may cause a temperature run-away in
the SUPERCLAUS® reactor and even catalyst damage. Therefore high temperature trips have been

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installed in the SUPERCLAUS® reactor.

Flame Temperature

It is imperative that the combustion temperature in the reaction furnace burner is at least 1250°C in order to
destroy the NH3 present in the Sour Water Stripper gas. When the feed gas contains not sufficient
combustibles to maintain the required flame temperature, additional heat is supplied. This is obtained by
preheating both the air and the amine gas feed. The feed gas preheater will also be maintained in operation
when no SWS feed gas is supplied to avoid water condensation in the acid gas feed line. If due to shortage
of combustibles in the feed gas the temperature tends to drop below 1250°C with the heaters on, fuel gas
should be co-fired in the main burner.

Claus Stage

When the reactor inlet temperatures are according to the design values the conversion to sulphur is
maximum.

At a lower inlet temperature of the first reactor, consequently the outlet temperature is also lower. It may be
less than 300°C, which leads to insufficient conversion of COS and CS2. This is not recovered in the
downstream part of the unit and results in an increased SO2 emission from the stack.

At a lower inlet temperature of the second and third reactors, sulphur vapour may condense on the catalyst
beds, resulting in reduced catalyst activity. At higher temperatures, less H2S is converted as the equilibrium
shifts to H2S and SO2.

At high throughput, the reactor inlet temperatures are 240°C, 210°C and 195°C, respectively. When the unit
operates at low throughput (below 40% of design), it is advised to increase the inlet temperature of the
second and third reactor by 10°C, to compensate for heat losses. This prevents sulphur condensation on
the catalyst beds. The reactor inlet temperatures are automatically controlled: the controllers adjust control
valves in the steam supply lines to the reheaters.

The difference between the inlet and bottom temperature of the reactor is a measure for the conversion rate
in the catalyst bed.

As soon as a decline in temperature difference across the second and third reactor becomes noticeable
from the daily operating figures, the inlet temperature should be temporarily increased. In this way
condensed sulphur is evaporated from the catalyst bed. It is pointed out that condensation of sulphur on the
catalyst is the most likely reason for deterioration of the catalyst.

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Euroclaus® Stage

A low inlet temperature in the 3rd reactor will lead to a lower reactor outlet temperature. A low reactor
temperature will give insufficient conversion of SO2 in the reactor. A high inlet temperature in the reactor will
lead to a higher reactor outlet temperature. The outlet temperature should not be allowed to exceed 250°C
as above this temperature the main reversible reaction shifts. This leads to a decrease in sulphur
production as less SO2 is converted and sulphur is converted to H2S.

Once in the EUROCLAUS® reactor off-gas, the sulphur associated with the SO2 cannot be recovered and
part of the sulphur transformed into H2S will also not be recovered. The difference in between the inlet and
bottom temperature of the EUROCLAUS® reactor is a measure for the conversion rate in the catalyst bed.

As soon as a decline in temperature difference across the reactor becomes noticeable from the daily
operating figures, the inlet temperature should be temporarily increased (at least 24 hours). In this way
condensed sulphur is evaporated from the catalyst bed. It is pointed out that condensation of sulphur on the
catalyst is the most likely reason for deterioration of the catalyst (see III.C.2.c).

At high throughput, the reactor inlet temperature is 195°C. When the unit operates at low throughput (below
40% of design), it is recommended that the reactor inlet temperature will be increased by 10°C to
compensate for increased heat losses to obtain a safe dew point margin. This prevents sulphur
condensation on the bed.

Superclaus® Stage

The SUPERCLAUS® reactor inlet temperature is controlled similarly to the other reactor stages.

At high throughput the SUPERCLAUS® reactor inlet temperature is 210°C, maximum 220°C. The reactor
outlet temperature should however not exceed 280°C. Above this temperature the sulphur yield decreases
due to an increase in SO2 formation. This is shown in figure 1.

It is imperative to maintain oxidizing conditions to prevent sulfiding of the catalyst, which would decrease
the sulphur yield. Therefore, the oxidation air control system has been designed to maintain an excess of
oxygen in the reactor. In this way the catalyst is protected against reduction of the iron oxide. The intent of
the control system for the oxidation air is to maintain an oxidizing environment on the SUPERCLAUS®
catalyst, to ensure the maximum conversion of H2S to sulphur and to prevent consecutive oxidation of
sulphur to SO2.

The two feed gas flows to the main burner are measured and used to calculate the relative load of the unit.

The H2S concentration in the EUROCLAUS® tail gas is measured by the tail gas analyser and this
measurement, together with the relative load are used to calculate the required oxidation air flow. Since the
tail gas flow has some time lag with respect to the incoming flow, the calculated oxidation air flow is delayed
by a lag block. The calculated oxidation air flow is used as the set point of the oxidation air flow controller.

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This flow controller is provided with minimum set point limit and minimum output limit to prevent a too low
concentration of oxygen downstream the SUPERCLAUS® reactor.

In this way the oxygen content in the process gas leaving the SUPERCLAUS® reactor stage is kept at
0.5 vol.%. Only at low throughput the oxygen content increases as the minimum stop in the controller output
overrules the actions of the control system.

See also control narrative, document no. 1800-8120-PD-R310-2001.

Remarks

In contrast with the Claus reactors, no sulphur is absorbed in the pores of the SUPERCLAUS® catalyst.
Therefore, no sulphur fires can occur in the SUPERCLAUS® reactor.

First, Second, Third and Fourth Sulphur Condensers

The condensers are operated at a convenient steam pressure to be able to enter the refinery low pressure
steam system. The set point of the pressure controller is kept above the refinery pressure in order to
overcome the pressure losses inside the sulphur plant and on the other hand, to stabilize the steam
pressure in order to maintain constant sulphur condenser outlet temperatures.

Superclaus® Condenser

The steam pressure in the condenser is low in order to condense as much sulphur vapour as possible, but
not so low that the water temperature causes solidification of sulphur (approx. 115°C).

During the first days after admitting EUROCLAUS® tail gas to the SUPERCLAUS® stage, the condenser is
operated at an increased steam pressure, similar to the other condensers. This because during start-up of
the SUPERCLAUS® section the catalyst is very active and low levels of SO3 are formed. The SO3 will form
H2SO4 and this can react with NH3, to form ammonia salts causing plugging of the condenser. Also plugging
by solidification of sulphur can take place. Operating at increased steam pressure may also be done at low
throughput operation.

Thermal Oxidiser

The function of the thermal oxidiser is to convert the residual H2S and other sulphur compounds, present in
the SUPERCLAUS® off-gas and the vent gas from the sulphur pit, into SO2. The maximum allowable H2S
content in the flue gas from the thermal oxidiser is 10 ppm vol.

The gas to be oxidized is heated by mixing with hot flue gas. The hot flue gas is produced in the thermal
oxidizer burner by combustion of fuel gas with air.

The combustion air for the fuel gas is supplied by the thermal oxidiser air blower. The air required for
oxidizing the sulphur compounds is partly supplied as vent air from the sulphur pit at a constant quantity.

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The remainder is supplied by the thermal oxidiser air blower. The fuel gas is burnt in two stages.

The first stage is the primary air, supplied to the burner. The primary air flow is ratio controlled by the fuel
gas flow. It is important to operate the primary air at substoichiometric conditions (between 80% and 90% of
stoichiometry) to prevent NOx formation.

The next stage is the "staged" air, supplied after the flame zone. The staged air flow is also ratio controlled
by the fuel gas flow, but moreover the output of the oxygen controller is added to the air flow rate,
calculated from the fuel gas flow. As the staged air flow corresponds with 50% of stoichiometric combustion
of the fuel gas, the fuel gas is actually burnt with approximately 130% of the stoichiometric air quantity.

Secondary air is supplied to the thermal oxidizer chamber to obtain an oxidizing environment. The
secondary air flow controller is adjusted by the output of the oxygen controller. Consequently, free oxygen is
available for the incineration of non-recovered sulphur components.

The flue gas leaving the thermal oxidiser is discharged via the stack to the atmosphere.

The operating temperature in the thermal oxidiser is 750°C and the oxygen concentration is 2.1 vol.%
during the SUPERCLAUS® mode. It is obtained from:

a. Combustion of fuel gas in the thermal oxidiser burner.


b. Combustion of the combustibles present in the tail gas, which is however small in the
SUPERCLAUS® mode.

At lower temperatures than 750°C the H2S content in the flue gas will increase. This might be partly
compensated by increasing the O2 concentration. A higher temperature will result in higher fuel gas
consumption. In the Claus mode, the tail gas contains considerably more H2S. In order to keep the H2S
content in the flue gas below 10 ppm vol, the operating temperature should be increased.

A low O2 concentration has the same effect as a low temperature: the H2S content increases. More O2
means that too much air is supplied, resulting in high fuel gas consumption.

In the Claus mode, more air is required for oxidation of the tail gas than in the SUPERCLAUS® mode as the
tail gas from the SRU contains more combustibles.

The flue gas leaving the thermal oxidiser is discharged via the stack to the atmosphere.

Apart from at initial start-up, the thermal oxidiser should be started before the main burner at subsequent
start-ups. Then poisonous gas with sulphur combustibles that might still be present in the unit, is converted
and released via the stack.

Sulphur Degassing

The air (with the released H2S) leaving the bubble columns is drawn off by the steam ejector. The capacity
of the ejector is higher than the stripping air flow, so that an additional amount of sweep air is drawn in via

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an air intake on the pit cover.

Initially the pit contains undegassed sulphur. At start-up, i.e. after opening the air supply to the bubble
columns, the released H2S is more than at normal operation. To prevent the creation of an explosive gas
mixture (H2S with air), an additional amount of sweep air flows into the pit by having the second ejector in
operation during at least one hour after start-up.

The sulphur temperature in the stripping section of the pit should be maintained between 125°C and 155°C.
Below 125°C the margin between operating and solidification temperature of 115°C would become too
small. Please note that the melting temperature is 119°C. Above 155°C degasification is less effective due
to the increased sulphur viscosity.

In order to operate the stripping section below 150°C, the incoming sulphur is cooled. The sulphur passes
through the sulphur cooler, located inside the pit. The cooling medium is boiler water from the
SUPERCLAUS® condenser with a temperature of 117°C.

The sulphur is cooled to 159°C in the cooler. Further cooling takes place by heat losses from the sulphur
pit.

When the temperature in the storage compartment exceeds 155°C, problems in the sulphur pumps
bearings may occur as the viscosity of the degassed sulphur rises excessively.

It is expected that during normal operation the steam coils in the stripping section will be switched off.

3.3.3.2 Ammonium Salt Plugging

During considerable upsets in the SWS gas (excess NH3) or hydrocarbon carry over from the Amine
Regeneration Units, there may temporary be a deficiency of air. Under these circumstances the possibility
exists that the ammonia is not converted completely. If so, ammonium salts are formed. Also when burning
ammonia in a Claus plant below the temperature limit of 1250°C, ammonium salts are formed.

These salts are experienced at the locations of the lowest temperature in the plant like outlet channels of
the condenser, wire demisters, sulphur lines and seals, resulting in pressure drop problems.

In particular ammonium salts are formed at the outlet of the final condenser and coalescer where the salts
tend to plug the mist mats. Fortunately the formation is reversible and at a temperature of 150°C or above
the salts sublimate into the process gas. In order to achieve this temperature, increase the steam pressure
in the final condenser to 3.2 kg/cm2 (ga) (steam temperature 145°C) or higher. If required, also increase the
steam pressure of the other condensers. In addition, it is advised to raise the flame temperature above
1250°C by using preheaters and/or co-firing fuel gas, if necessary.

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3.3.3.3 Plugging of Sulphur Locks

Sulphur plugging problems are usually experienced in sulphur lines and sulphur seals. When plugging is
caused by pure solid sulphur, for example due to a malfunctioning steam trap, it can easily be removed by
heating. Sulphur, however, in combination with corrosion products, refractory and/or catalyst fines may give
grey sulphur (concrete sulphur) which is difficult to remove. At initial start-up the catalyst beds should be air
blown to remove fines (see Section .3.2.2). Careful cleaning of the tubes of waste heat boiler, sulphur
condensers, sulphur lines and sulphur seals will eliminate plugging problems at start-up.

Plugging of sulphur seals or sulphur rundown lines can be detected by checking the funnels. Please note
that personnel protection should be used, see also Section II.B.6.e). The system is plugged when no liquid
sulphur flows. When a sulphur seal is plugged, an LP steam or nitrogen hose can be connected to the top
of the seal. The block valve in the sulphur rundown line is closed and the seal is blown with the steam or
nitrogen. If plugging occurs in the sulphur rundown line, the sulphur seal outlet is to be blinded-off. Then
seal and sulphur lines are blown in the direction reverse to normal flow. At other locations, remove the
jacketed elbows in order to blow through.
®
Especially the sulphur seals downstream the SUPERCLAUS condenser and the coalescer shall be
checked regularly at least on a daily basis. Because of the relatively low temperature, the danger of
plugging is here higher.

3.3.3.4 Temperature Runaways

Fire inside the Claus reactors

During the shutdown phase and hot standby operation a rapid temperature rise in one of the catalyst beds
(temperature runaway) may occur. Such a temperature runaway or fire is caused by excess air into the
plant. Then the sulphur, absorbed in the catalyst, reacts violently with the oxygen in the air, resulting in a
fire. A fire inside the reactor bed deactivates the catalyst by severe sulphation and sintering. Shut-down
procedures, as described in Section 3.3.4 will prevent these temperature runaways.

When a temperature runaway happens, the air supply to the main burner should be decreased and/or the
fuel gas supply should be increased to stop the air break-through from the burner. The corresponding
steam reheater should be stopped by adjusting the set point of the temperature controller. LP steam should
be introduced directly into the reactor. When the temperature is dropped, the steam reheater can be
restarted.

Also, sulphur elsewhere in the plant can be set on fire by uncontrolled amounts of oxygen. In a sulphur
plant design, dead spots where sulphur may accumulate should be prevented. All equipment in which
sulphur condenses, should have a proper slope.

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Temperature runaway in the SUPERCLAUS® reactor

In the SUPERCLAUS® reactor, a temperature runaway can occur if the reactor is exposed to a high H2S
concentration (> 2.0 vol.%) continuously for several minutes or longer. This may happen if e.g. excessive
quantities of hydrocarbons are entrained in the acid gas feed.

In case of a temperature runaway the air flow to the main burner should be increased to reduce the H2S
content. When the H2S content exceeds 2.0%, the bypass across the SUPERCLAUS® stage is
automatically opened to prevent damage of the catalyst. The bypass is also opened when the catalyst bed
temperature exceeds 350°C.

This status should be kept until the H2S concentration is back in its proper range and the SUPERCLAUS®
reactor bed temperatures are below 300°C. In the SUPERCLAUS® reactor, steam should never be
introduced as condensate on the catalyst surface may decrease the catalyst activity. The SUPERCLAUS®
catalyst should always be operated with an excess of oxygen and kept in a dry atmosphere.

Fire in the sulphur pit

Fire inside a sulphur pit is often caused by static electricity. A fire in the sulphur pit is detected by the
temperature alarms in the air space of the sulphur pit. The fire should be extinguished by injection of
smothering steam.

3.3.3.5 Poor Sulphur Recovery

1. A decrease of sulphur recovery is often caused by deactivation of the catalyst due to sulphation.
Sulphates are mainly formed by excess oxygen during shut-down operation. Therefore, immediately after
restart, the catalyst should be reactivated. Also, if required, the catalyst can be reactivated during operation.
Reactivation (also called regeneration or rejuvenation) is the reduction of sulphates at elevated temperature
(as high as possible) with slight excess of H2S (2 - 3 vol.%). Titanium catalyst (CRS-31) which is installed in
the 1st Claus reactor is insensitive to sulphation.

2. Catalyst deactivation can also occur when the reactor bed temperature drops below the sulphur dew
point of the process gas. This can be solved by raising the reactor inlet temperature to 15-30°C above the
normal value for some time to vaporise the sulphur (heat soak).

3. Another cause of low sulphur recovery can be a poor acid gas/air ratio control. In refineries, often the
acid gas composition is not known and usually it fluctuates during operation. The H2S/SO2 analyser corrects
for this, but it is advised to adapt the air/ acid gas ratio if there is a continuous correction by the analyser.

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4. Good sulphur separation after each condenser is also important. For this purpose, all sulphur condenser
outlet channels have been provided with demister pads. Furthermore, a coalescer with demister
downstream the last condenser has been provided.

5. In the main burner, COS and CS2 are formed as by-products. They are present especially when large
amounts of CO2 and/or hydrocarbons are present in the feed gas. If they pass through the unit untouched,
they account for some loss of sulphur recovery. However, at a sufficiently high temperature (higher than
300°C), COS and CS2 are largely hydrolysed to H2S in the first Claus reactor. Therefore it is important to
maintain the 1st reactor inlet temperature at 240°C.

3.3.3.6 Pressure Drop

Soot, corrosion products such as FeS, refractory fines or ammonium salts can be the cause of an
increasing pressure drop over the unit.

Soot is formed when hydrocarbon carry-over from the amine regeneration units occur. The flow ratio
controller cannot follow such upsets, and hydrocarbons are carried through the whole unit and too little H2S
is burnt in the main burner. Sometimes a fire starts in the thermal oxidiser and/or stack due to combustion
of large quantities of H2S.

Soot is deposited on the catalyst and the sulphur produced is brown or black under such conditions.
Hydrocarbon carry-over can be prevented by better operation and/or modifications to the amine
regeneration units.

Another possibility of soot formation occurs when the burners are fired at very low air/fuel gas ratios. It is
recommended to keep the ratio at 90 - 95% stoichiometry. This can be checked visually by observing the
colour of the flame, which should be salmon pink when fuel gas is fired.

A common refinery regeneration procedure to remove soot is to burn off the soot at 500°C flame front
temperature. This procedure, however, is not recommended as this high temperature will promote sulphur
fires and sintering of the catalyst. A better way is to replace 10 cm top layer of the catalyst as standard
procedure at each turn-around or at shut-down caused by too high pressure drop.

When burning ammonia in a Claus plant under the temperature limit of 1250°C, ammonium salts may
accumulate on lower temperature spots like outlet channels of the condensers, wire demisters, sulphur lines
and seals, resulting in pressure drop problems. A way to remove these salts is to increase the process gas
temperature. In addition, it is advised to increase the flame temperature of the main burner above 1250°C
by using the preheaters and/or co-firing fuel gas, if necessary. This will enhance the combustion of
ammonia and therefore plugging problems by salts will be avoided.

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Sulphur demisters may be plugged by sulphur. Therefore, all demisters have been located in an outlet
channel provided with a steam tracing to keep the outlet channel hot.

The pressure drop in a sulphur recovery unit is proportional to the square of the throughput. Operators
should daily check the plant pressure drop to make sure they notice early warnings in case the pressure
drop starts to deviate. To simplify their work the pressure drop can be said to be proportional to the square
of the air flow. As the pressure drop, divided by the square of the air flow, should be a constant figure, early
warning of pressure drop problems can be found by daily plotting this ratio.

3.3.3.7 Operational Hazards

The aim of this section is to highlight some important aspects.

General

• Sudden temperature changes should be avoided whenever possible, since they might cause
leaks at flanges or loosening of iron sulphide scale from the equipment walls.
• H2S and SO2 are extremely poisonous gases. Utmost care must be taken to avoid exposure of
personnel and environment to these gases, e.g. when draining H2S containing liquid or when taking gas
samples. In special circumstances, protective masks must be worn (see III.B.6.e). The lower and upper
explosion limits of H2S in a gas-air mixture are 4.3 and 45.5 vol.%, respectively. In the stoichiometric ratio
with air, it explodes violently when ignited.
• At a temperature of approximately 230°C, auto-ignition of liquid sulphur will occur when in contact
with air. This situation can occur, when the SUPERCLAUS® condenser is blocked, liquid sulphur is present
in the inlet and outlet channels of the SUPERCLAUS® condenser, and the SUPERCLAUS® bed is
simultaneously cooled with oxidation air. In such an event the temperature of the gas from the
SUPERCLAUS® reactor is above the auto-ignition point of sulphur and contains mainly air. It is brought in
contact with liquid sulphur at the inlet of the SUPERCLAUS® condenser. A fire could damage the condenser
Sulphur dust will ignite at approximately 190°C.
• The boiler water in the waste heat boiler and sulphur condensers should be sampled periodically
to check the concentration of solids. The maximum allowable total concentration of solids in the waste heat
boiler is 3000 ppm, of which a maximum 250 ppm of suspended solids is permitted. The maximum
allowable total concentration of solids in the sulphur condensers is 3500 ppm with maximum 300 ppm of
suspended solids. Higher figures might lead to dirt and scale deposition and finally to damage of the boiler
and condensers. The concentration of solids can be adjusted by varying the blow down rate.
• All steam traps should be checked frequently to ensure a proper heating performance. In this way
plugging of the process lines, equipment and valves by solid sulphur can be avoided.
• A frequent inspection of the sulphur flow from the sulphur seals and the flame colour as well as

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reading of the main burner inlet pressure may give an early warning before plugging by sulphur and/or
ammonia salts might occur.

Main Burner/Reaction Furnace

• Care should be taken that the air-to-fuel gas ratio at the main burner is correct. A major deficiency
of air at fuel gas firing might result in deposition of soot on the first catalyst bed (higher pressure drop and
less sulphur conversion). Soot can only be removed during a shut-down period by replacing the sooted
(top) layer of the catalyst bed. When the unit is still hot, an air excess might result in equipment damage
due to fire inside the equipment. It might also cause sulphation of the Claus catalyst in the second reactor,
resulting in less sulphur conversion.
Soot can only be removed during a shutdown period by replacing the top layer of the catalyst bed.
• To prevent damage of the burner, it is strongly advised to operate the air side of the burner at a
pressure drop of at least 1.0 mbar. For this purpose also a low air flow trip has been provided.
• During the (fuel gas) ignition stage in the burner, the maximum amount of fuel gas allowed to be
present inside the burner/reaction furnace is restricted to avoid an excessive pressure rise when the actual
ignition takes place. For this reason the burner/reaction furnace are purged before admitting fuel gas to
remove any combustibles that might be left from a previous ignition trial. The equipment is capable to stay
leak tight after a pressure rise during ignition or explosion, but the internals may be damaged.
• No carry-over of liquid hydrocarbons or high amounts of gaseous hydrocarbons from preceding
units should take place as it might damage the main burner/reaction furnace. It might also cause soot
deposition inside the unit, e.g. on the catalyst beds.
• The temperature in the reaction furnace should be at least 1250°C in order to maintain a stable
flame. Therefore, the air and acid gas preheaters should always be in operation.
• The windows of the flame scanners and the pyrometer should be cleaned on a regular basis.

Reactor Stages
• Runaway temperatures in the Claus reactors should be avoided during hot standby and
shutdown. When the temperature tends to rise to 400°C the air-to-fuel gas ratio at the main burner should
be reduced in order to obtain substoichiometric conditions. Introduce nitrogen to the reactor for additional
cooling.
• The oxidation air flow control system should always be in operation to obtain an oxygen
®
concentration of typically 0.5 vol.% in the process gas leaving the SUPERCLAUS stage. If no excess
oxygen is present, the catalyst in the SUPERCLAUS® reactor may be damaged.
• At start-up and upset conditions, the SUPERCLAUS® stage shall be bypassed to protect the
catalyst.

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• The performance of the tail gas analyser should be checked regularly.

Thermal Oxidiser

• The thermal oxidiser is started-up before the main burner to convert any hazardous gas, which
might leave the unit during the purging and ignition phases of the main burner. This does not apply to the
initial heating-up and drying-out phases. Then the temperature rise of the thermal oxidiser should occur
gradually and Claus off-gas from the main burner is required as a cooling medium.

Sulphur Pit

• Too high a liquid sulphur temperature should be avoided. Above 155°C the viscosity of the
sulphur rises rapidly and may harm the sulphur pumps. Therefore, the steam coils should only be in
operation when no sulphur is produced in the unit, unless the sulphur temperature drops below 125°C.

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3.3.4 Shut-down Procedure

A proper shutdown procedure is most important. Sulphation of the catalyst, plugging after restart and
corrosion are mostly the result of misoperation or wrong procedures during shutdown. Therefore, a
scheduled shutdown should be carefully carried out.

During normal operation sulphur vapour is absorbed in the pores of the Claus catalyst. Prior to a scheduled
shutdown it is necessary to remove the sulphur from the catalyst to prevent that the sulphur inside the
catalyst is exposed to air at elevated temperatures, which results in runaway temperatures. The procedure
also prevents sulphur solidification inside the catalyst.

For this purpose, the inlet temperatures of the Claus reactors are raised 15°C to 30°C above the normal
operating temperature and operated at this temperature for 48 hours prior to shutdown.

In this way the absorbed sulphur is removed from the catalyst pores and is subsequently condensed in the
sulphur condensers and drained to the sulphur pit. The inlet temperature of the SUPERCLAUS® reactor is
kept at its normal value. This operation is called “heat soak”.

After 48 hours of operation at elevated temperature, the feed gas supply is stopped and the unit is purged
with inert gas.

The inert gas is obtained by substoichiometric combustion (95% stoichiometry; substoichiometric means
shortage of air) of fuel gas and air in the main burner. The substoichiometry can visually be checked by
means of the flame colour. Blue means excess air, pink blue means stoichiometric combustion, pink means
slightly substoichiometric combustion and yellow means deep substoichiometric combustion.

Steam is supplied to the burner to prevent overheating of the reaction furnace. Moreover, it increases the
inert gas flow through the unit. The “steam to fuel gas” ratio is approximately 4 on weight basis.

During this operation the air flow to the main burner is 4020 kg/h at a fuel gas flow of 250 kg/h. Steam for
cooling is approximately 1000 kg/h.

The SUPERCLAUS® stage is manually switched to bypass operation before fuel gas intake. The air to the
SUPERCLAUS® reactor is supplied via the start-up air line at maximum flow rate to obtain an inlet
temperature of the SUPERCLAUS® reactor of 190-210°C.

When it is planned to shutdown the unit completely, the inlet temperatures of the Claus reactors are raised
as high as possible during the substoichiometric fuel gas combustion in the main burner. This operation is
called “sulphur stripping”. No excess air should be introduced via the main burner during this operation as
the air will react with the sulphur on the catalyst which may result in too high a catalyst temperature and
sulphation of the catalyst.

On the other hand, the thermal oxidiser should be operated with excess air to convert any sulphur vapour

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into sulphur dioxide.

There are two shutdown procedures to be considered:

1. Shutdown for a short period (hot standby).

The feed gas supply is stopped, but the unit is kept on standby, so that the unit can be restarted
immediately on feed gas. The whole unit is kept hot during this period; the burners remain in operation on
fuel gas. The SUPERCLAUS® stage is bypassed.

The fuel gas at the main burner is burnt substoichiometrically. In this way, an inert flue gas is obtained for
purging the unit. Steam is supplied to the burner for cooling of the flame.

This shutdown procedure is preferred because formation of corrosion products is prevented and there is
less chance on plugging and on sulphate formation in the Claus catalyst, which causes deactivation. In this
way the unit can be operated for a few days or even for a few weeks.

It is essential that during hot standby operation, no excess air is introduced into the plant, as it will
result in sulphate formation in the catalyst and consequently in deactivation of the catalyst.

a) Simplified Outline

1. Stop the SWS acid gas feed supply and reduce the Amine acid gas feed flow to 30%.
2. Increase the Claus reactor inlet temperatures at 48 hours prior to feed gas shut-off.
3. Bypass the SUPERCLAUS® stage.
4. Commission fuel gas and steam to the main burner and shut-off the feed gas.
5. Keep an eye on the reactor temperatures.

Detailed Outline

Reducing Feed Gas flows and increasing Reactor Inlet Temperatures

1. Switch FC-1045 to AUTO mode and reduce the SWS acid feed gas flow, followed by a complete
stop with HS-1117.
2. Switch FC-1038 to AUTO mode and reduce the Amine acid feed gas flow to 30%.
3. Increase the inlet temperatures of the first, second and third reactor as high as possible. Watch the
temperatures in the SUPERCLAUS® reactor and thermal oxidiser. Maintain this situation for 48 hours.
4. Bypass the SUPERCLAUS® stage with HS-1202. Route the air via the start-up line to the fourth
reheater E-1011. Adjust the air flow to maximum.
5. Increase the set point of PC-1217 in the steam line from the SUPERCLAUS® condenser to the
steam condenser to 4 kg/cm2 (ga). Open the steam supply to the bottom of the SUPERCLAUS® condenser.

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Open the boiler water drain valve and maintain the water level in the condenser.
6. Open the fuel gas supply to the main burner with HS-1110. Adjust a flow rate of 250 kg/h,
corresponding with the hot standby flow.

Shut off the Feed Gas

1. Start the steam supply to the main burner (HS-1111) in order to avoid too high a temperature in the
reaction furnace.
2. Stop the feed gas flow with HS-1116. By doing so, also AC-1083 is switched to MANUAL mode.
The steam supply to the main burner should now be 1000 kg/h. Note that it is essential that the “steam to
fuel gas” ratio is approximately 4 (on weight basis).
Maintain the acid gas preheater in operation.
3. Ensure that the combustion in the main burner is substoichiometric.
4. Open the steam supply to the steam coils in the sulphur pit.
5. Close the hand valves in the boiler water supply and return lines of the sulphur cooler.

2. Shutdown for a Long Period (Complete Shutdown)

This procedure should be followed in the event the unit has to be shutdown completely and opened for
maintenance or catalyst exchange.

The difference between this procedure and the procedure discussed above is that now all absorbed sulphur
is removed from the catalyst bed and pyrophoric FeS on the equipment walls is oxidized before the actual
shutdown.

This shutdown procedure normally takes four days. It is pointed out that before excess air is introduced, the
unit should be purged by inert flue gas for at least 24 hours and the catalyst beds should be cooled during
this period to 200°C.

The inert gas flow is produced by substoichiometric combustion of fuel gas in the main burner. During this
operation the air flow to the main burner is 4020 kg/h at a fuel gas flow of 250 kg/h; steam for cooling is
approximately 1000 kg/h. The SUPERCLAUS® reactor is kept hot with air via the start-up line.

It is advised to make a temperature plot of top and bottom temperatures of the Claus and EUROCLAUS®
catalyst beds, the outlet temperatures of the reactors, as well as a plot of the SO2 content in the tail gas
from the EUROCLAUS® reactor.

After 24 hours, excess air is gradually introduced to remove the last traces of sulphur and to oxidize the
pyrophoric FeS, created during normal operation in the equipment. In case at any point the temperature
raises too high, reduce the air flow to obtain (sub)stoichiometric conditions.

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Simplified Outline

1. Stop the SWS acid gas feed supply and reduce the Amine acid gas feed flow to 30%.
2. Make the Claus/EUROCLAUS® reactor inlet temperatures as high as possible at 48 hours prior to
feed gas shut-off.
3. Bypass the SUPERCLAUS® stage.
4. Commission fuel gas and steam to the main burner and shut-off the feed gas.
5. Raise the Claus/EUROCLAUS® reactors inlet temperatures as high as possible and maintain
these conditions for at least 24 hours.
6. Make a plot of the Claus/EUROCLAUS® reactor temperatures and the SO2 content in the tail gas.
7. Reduce the Claus/EUROCLAUS® reactor bed temperatures to 200°C.
8. Slowly introduce excess air to remove the remaining sulphur and FeS from the unit.
9. Keep all plant heating systems in operation.
10. Gradually cool down the unit.
11. Shutdown the thermal oxidiser.

Detailed Outline

Initially follow the shutdown procedure for short period (Section 3.3.4.1).

Strip Sulphur from the Catalyst

1. Check the fuel gas and air supplies to the main burner. The “air to fuel gas” ratio should be slightly
substoichiometric. Check the O2 content in the flue gas from the main burner.
2. Make the inlet temperatures of the Claus/EUROCLAUS® reactors as high as possible and
maintain these temperatures for at least 24 hours. Maintain the inlet temperature of the SUPERCLAUS®
reactor at 180 - 210°C.
3. Keep all plant heating systems in operation.
4. Make a plot of the top, bottom and outlet temperatures of the Claus/EUROCLAUS® reactors.
Take readings every 5 minutes for the first hour and every 15 minutes thereafter. Make also a plot of SO2
content in the tail gas. Take readings every 10 minutes during the first hour and every 30 minutes
thereafter.
5. If the temperature in a reactor tends to rise above 350°C, the corresponding steam reheater
should be shutdown. Restart the steam reheater when the reactor temperature has dropped below 150°C. If
the temperature still tends to rise to 380°C, it might be considered to inject nitrogen into the reactor inlet.
A temperature of 400°C is the absolute maximum for the catalyst bed.

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6. Maintain the following temperatures:

Reaction furnace 1250 - 1400 °C


Claus reactors 250 °C
EUROCLAUS® reactor 240 °C
SUPERCLAUS® reactor 180 - 210 °C
Thermal oxidiser 750 °C

Cool down the Unit

1. Shut-off the steam reheaters to cool down the Claus, EUROCLAUS® and SUPERCLAUS®
reactors.
2. Slowly introduce a small amount of excess air to the main burner as soon as the catalyst bed
temperatures are 200°C. The initial O2 content in the flue gas from the main burner should be approximately
1%, to be checked by oxygen analyses.
The bed temperatures should be watched for any sign of temperature increase. Reduce immediately the
excess air in the event the temperature shows indications of rising above 230°C. If the temperature tends to
increase towards 350°C, it might be considered to inject nitrogen into the corresponding reactor inlet. The
temperature should never exceed 400°C.
3. Start a plot of the Claus/EUROCLAUS® reactor temperatures. Read the temperatures every 5
minutes during the first hour of the excess air operation, hereafter every 15 minutes. Also, make a plot of
the SO2 content in the tail gas, reading every 10 minutes during the first hour of the excess air operation,
hereafter every 30 minutes.
4. Gradually cool down the unit by introducing more excess air. Continue to watch the reactor bed
temperatures.
5. Close the sulphur outlets of the sulphur condensers and coalescer (order of closure: Sulphur seal
A, B, C, D, E and F).
6. Close the fuel gas and steam supplies to the main burner by actuating HS-1110 (fuel gas) and
HS-1111 (steam). Purge the unit with air so that no wet process gas has been left in the equipment, which
might cause corrosion. Stop the air supply to the Claus section after purging and stop the air flow to the
®
SUPERCLAUS stage.
7. Shut-off the main air blower after finishing the sulphur stripping process in the degassing pit (refer
to next section).
8. Shutdown the thermal oxidiser.
9. Open the valve in the separation wall between the stripping and the storage compartments of the
sulphur pit. Empty the sulphur pit and close the valves in the sulphur transfer line to the battery limit. When
it is necessary to open the sulphur lines and seals, the seals can be emptied by blowing with steam or

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nitrogen. Otherwise, sulphur may be kept as liquid in the sulphur seals by maintaining the supply of heating
steam.
10. Block-off the boiler feed water supply and close the blow down valves at the waste heat boiler and
sulphur condensers.
11. Vent and drain the waste heat boiler and sulphur condensers if necessary.
12. Check if all shutdown valves are closed.
13. Install spectacle blinds at the battery limits, except for the LP steam for internal heating.

Remark
During the shutdown phase it must be constantly born in mind that a rapid temperature drop is undesirable
because:

• Lining materials may be damaged.


• High thermal stresses or contraction may deform piping and equipment, causing leaks after a
restart.
• Solidification of sulphur may occur.

SHUTDOWN OF SULPHUR DEGASSING PIT

1. Continue the stripping process for approximately 6 hours after the sulphur supply stops.
2. Close the steam jacketed plug valves in the air supply to the spargers.
3. Keep the steam ejector, the sweep air flow and the heating system in operation as long as the pit
contains sulphur.
4. If the sulphur supply is stopped for a long period, the drain valve at the bottom of the separation
wall can be opened. The pit is emptied by starting the sulphur transfer pump.
5. Stop the steam supply to the steam coil and the steam ejector when the pit is empty.
6. Before the steam supply to the steam jacketed sulphur lines is shut off, make sure the sulphur is
drained from these lines.
7. Close the battery limit valves.

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3.3.5 Emergency Shutdown and Restart Procedures

3.3.5.1 Automatic Shutdown (Trip)

The unit is shutdown either automatically by the safeguarding system or manually when the shutdown
switches in the control room or in the plant are actuated.

As the unit is hot, there will be enough time to take measures before sulphur will solidify.

After a trip, the unit shall be brought on stream as soon as possible to avoid the heating-up procedure of the
reaction furnace. This would require excess air combustion in the main burner, which might harm the
catalyst and equipment when FeS and sulphur are present.

3.3.5.2 Restart after an Automatic Shutdown (Trip)

Restart when the Unit is hot and the Sulphur is inside de Equipment

1. Open the bypass of the Superclaus® stage and close the Superclaus® inlet valve.

2. Start the thermal oxidiser (see Section 3.3.2.1).

3. Start the purge/ignition procedures for the reaction furnace burner (see Section 3.3.2.1)).

4. After establishing a stable fuel gas flame, adjust substoichiometric combustion at the reaction furnace
burner at a fuel gas flow of 250 kg/h and air flow of 4020 kg/h through the trim air line. Admit steam to the
burner for cooling. The reaction furnace burner is now in the hot standby mode. Excess air should be
avoided as it may lead to sulphur fires.

5. It is assumed that the preheaters and reheaters are still in operation. Adjust following temperatures:

Reaction furnace 1000 - 1300 °C


Claus reactors inlet 240 °C
EUROCLAUS® reactor inlet 230 °C
SUPERCLAUS® reactor inlet 150 - 180 °C
Thermal oxidiser 750 - 800 °C
6. Admit feed gas (see Section 3.3.2.6)).

7. Take the Superclaus® stage in operation (see Section 3.3.2.8).

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Restart when the Unit is cold and Sulphur is inside the Equipment

1. Open the bypass of the Superclaus® stage and close the Superclaus® inlet valve.

2. Start the thermal oxidiser (see Section 3.3.2.1).

3. Start the purge/ignition procedures for the reaction furnace burner (see Section 3.3.2.1)).

4. After establishing a stable fuel gas flame, adjust the minimum design air flow of 4020 kg/h through the
trim air line and a fuel gas flow of 200 kg/h, corresponding with 15% to 20% overstoichiometric combustion.
Steam cooling is not allowed, as it will condense on the cold walls of the downstream equipment. Only
admit steam to the burner when all equipment has reached a temperature of at least 80 °C.

5. When available, nitrogen can be supplied to the burner for cooling. Carefully watch the temperature in
the reaction furnace. In case the temperature rises too rapidly, the burner should be stopped temporarily.

6. Watch the unit temperatures carefully. Be aware that sulphur fires may start, as excess air is present.
Ignition of FeS on the equipment walls might also occur.

7. Start the reheaters and slowly increase the temperature of the converter beds. The Claus converter
temperatures should be restricted to 120 °C to avoid a sulphur fire in the catalyst.

8. As soon as the equipment temperatures are above 80 °C steam can be supplied to the reaction
furnace burner. Increase the fuel gas flow to 250 kg/h to obtain substoichiometric combustion. From now
on, it is easier to have the temperatures under control.

9. Continue with the heating-up procedure for the reaction furnace, thermal oxidiser and converter
stages (see Section II.C.2.a)). The temperature rise in the reaction furnace and thermal oxidiser is
maximum 50°C/hour.

10. Adjust following temperatures:

Reaction furnace 1000 - 1300 °C


Claus reactors inlet 240 °C
EUROCLAUS® reactor inlet 230 °C
SUPERCLAUS® reactor inlet 150 - 180 °C
Thermal oxidiser 750 - 800 °C
11. Admit feed gas (see Section II.C.2.e)).

12. Supply LP steam to the Superclaus® condenser. Increase the pressure inside the condenser to 4
kg/cm2g.

13. Take the Superclaus® stage in operation (see Paragraph Section 2.3.2.8)).

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Restart when no Sulphur is Inside the Equipment

When no sulphur is present in the unit, the normal start-up procedure as described in Section 2.3.2 can be
followed.

3.3.5.3 Critical Areas In Sulphur Recovery Plant Operation

MAIN CAUSES PHENOMENON COUNTERMEASURES IN


OBSERVED DESIGN/OPERATION

1. MAIN COMBUSTION
CHAMBER

Poor combustion of acid Selection of Main Burner


a. Damage of the burner gun of gas with combustion air with adequate pressure drop
Main Burner due to heat attack in all operational ranges
(especially during start-up, low
load and shut-down operation). Increase in residual NH3
content increase in SO3 Management on pressure
formation increase in drop indicator installed on
residual O2 content combustion air side
(Operation above limitation:
> 1.5 mbar)
(Above phenomena
resulting in plugging
and/or corrosion in
downstream
equipment/lines).

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MAIN CAUSES PHENOMENON COUNTERMEASURES IN


OBSERVED DESIGN/OPERATION

b. Damage of refractory lining Hot shell/hot spot (shut- Management on temperature


due to exceeding maximum down) indicators installed on
service temperature (flame Reaction Furnace
direct contact) or anchor failure
initiated by hot gas soaking.
Steam injection S atomizing
flame

Adjustment in upstream gas


treating unit (S)

Application of homogeneous
mixing especially for nozzles
of sight gas pilot burner and
instrument connections

c. Internal explosion (especially Leakage is of highly toxic Application of explosion


during start-up and shut-down). nature (H2S) (shut-down) proof equipment (explosion
pres-sure)

2. WASTE HEAT BOILER

a. Failure of tube-tube sheet Leakage of boiler feed Adequate maintenance for


joint due to high temperature water (shut-down) ferrules in tube and lining of
sulphide corrosion in process tube sheet
gas side.

Application of adequate tube


sheet thickness

Application of strength
welding or J-bevel welding
with adequate expansion for
tube-tube sheet
joint.

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MAIN CAUSES PHENOMENON COUNTERMEASURES IN


OBSERVED DESIGN/OPERATION

b. Rupture of tube due to ero- Leakage of boiler feed Management on quality of


sion and corrosion water (shut-down) boiler feed water
Adequate tube arrangement

c. Internal explosion Leakage is of highly toxic Application of explosion


nature (H2S) (shut-down) proof equipment (explosion
especially during start-up
pressure for inlet tube sheet
and shut-down)
and outlet channel)

d. Plugging of sulphur and/or High pressure drop (shut- Selection of moderate


ammonium salt (in case of LP down) operating temperatures
steam production)
Increase in gas outlet
temperature by increasing
product steam level
Adjust Main Burner operation
(minimising residual NH3 and
preventing SO3 formation)

3. REACTORS

a. Accumulation of soot High pressure drop and Correction of fuel gas/air


black sulphur production ratio in case of heavy
(regeneration or fluctuation in the fuel gas
skimming during shut- composition
down)

b. Sulphation Poor sulphur recovery Application of special


catalyst to prevent sulphation
(catalyst regeneration
during low load or before Adjust Main Burner operation
shut-down) (minimizing residual NH3 and
preventing SO3 formation)
Correction of fuel gas/air
ratio for preventing free O2

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MAIN CAUSES PHENOMENON COUNTERMEASURES IN


OBSERVED DESIGN/OPERATION

c. Temperature runaway Poor sulphur recovery Control for preventing O2


injection through main burner
(Claus reactors) (Sieving damaged
catalyst or replace with Application of Nitrogen in
new one) each Claus reactor inlet line

d. High H2S content in process High temperature in By-pass SUPERCLAUS®


®
gas to SUPERCLAUS reactor SUPERCLAUS reactor reactor
Air sweep of reactor

e. Plugging of sulphur with High pressure drop Increase in reactor inlet


other contaminants temperature
(Adjustment of operation
condition) Application of 50 mm
insulation on reactors to
minimise heat loss

f. Liquid sulphur formation on Poor sulphur recovery Increase in reactor inlet


catalyst (catalyst heat soak) temperature with
approximately 30 °C

4. (P)REHEATERS

a. Rupture of tube due to High pressure at process Adequate tube material


erosion and corrosion. side due to steam (stainless steel)
leakage (shut-down)

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MAIN CAUSES PHENOMENON COUNTERMEASURES IN


OBSERVED DESIGN/OPERATION

5. SULPHUR CONDENSERS

a. Plugging of sulphur and/or High pressure drop (shut- Selection of moderate


ammonium salt in tube and down) operating temperature
demister (above melting point of
ammonia salt)
Increase in gas outlet
temperature by increasing
product steam pressure
Adjust Main Burner operation

b. Corrosion in outlet channel Leakage of boiler water Selection of moderate


due to SO3 condensation (shut-down) operation temperature
(above dew point of SO3)
Increase in gas outlet
temperature by increasing
product steam pressure
Adjust Main Burner operation

6. SULPHUR DEGASSING
PIT

Damage of equipment Adequate H2S sweeping


a. Internal explosion due to installed in vessel and fire
Installation of flow meter in
H2S content in vapour space of product sulphur
vent gas line(s) with
above liquid sulphur in vessel
emergency system -
(low explosion limit:
provision of snuffing steam
approximately 4 vol.%)
system

b. Corrosion of steam coil due Steam leakage Application of stainless steel


to H2S and wet atmosphere pipe or carbon steel pipe
with enough thickness
Keep dry condition during
shut-down period

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MAIN CAUSES PHENOMENON COUNTERMEASURES IN


OBSERVED DESIGN/OPERATION

c. For degassing pit: corrosion Damage of degassing pit Enough investigation on


of steel between concrete walls concrete wall and degassing pit type selection
as water shield, due to destruction of degassing in case that ground water
difference in thermal expansion pit level is higher than
degassing vessel pit depth
Application of plastic material
as water shield (4 layer
construction)
Application of submerged
carbon steel tank with
alumina coating

7. LIQUID SULPHUR LINE(S)


AND SULPHUR SEAL(S)

a. Solid sulphur plugging due


Pressure drop increase Management on steam
to malfunctioning steam trap
supply conditions and check
on operation of steam trap(s)
by solid sulphur lump

b. Plugging of sulphur with Pressure drop increase Enough and careful cleaning
corrosion products, refractory (replace with new one) before start-up (wirebrush)
and/or catalyst fines (concrete
Provision of blowing facilities
sulphur)
in line(s) and seal(s) with air
and steam

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3.3.6 Special Operations

3.3.6.1 Operational procedure for draining sour water pumps

(See figure 7)
1. Isolate the spare pump from the process closing valves A and B.
2. Open valve E and depressurize the pump.
3. Rotate to open the spade on Utility Water injection line.
4. Open valve C.
5. Start to inject UW using the throttling valve D. Monitor the pressure with the local pressure
gages. Flush the pump for 5 minutes.
6. Once the Sour Water is replaced by clean water, close valve D and E.
7. Close valve C and rotate the spade.
8. The pump can be drained to OWS.

Figure 7. Sketch of operational procedure for draining sour water pumps.

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3.3.6.2 Maintenance

Maintenance operations for several types of equipments of this unit are described here below.

Knock-out drums
1. Clean the inside of the knock-out drum from loose scale and dirt.
2. Clean the demister mat with steam.
3. Pressure test the steam coil, which is at the outside of the drum.
4. Check the condition of the demister support.
5. Outlet nozzle at the bottom should be freed from dirt.
6. Check the condition and mounting of the gas inlet device.

Pre- and reheaters


1. Clean the shell side and tubes at the outside, in such a way that they are freed from any loose
scale and dirt.
2. Pressure test the steam side of the pre- or reheater for approximately 2 hours after cleaning
activities.
3. Check the steam traps.

Burners
1. Remove the main burner and thermal oxidiser burner from the equipment.

2. Check if the metal parts of the burners have not been damaged by overheating. Measure the
dimensions of the burner gun and air nose. If significant deviations are observed LD Duiker, the burner
manufacturer, should be contacted. Attention should be given to the vanes of the air register, the burner
gun and tip and the air nose. Replace damaged parts.

3. Check the electric ignitor. The tip may have to be replaced.

4. Check the refractory lining on cracks.

5. Clean the burners, including sight glasses and flame detectors.

6. Clean the air chamber of the burners and check if the drains are clean.

Reaction Furnace
1. Check the refractory lining of the reaction furnace. Bricks which are not in correct position have
to be replaced. Castable refractory, which is damaged, should be repaired.

2. Inspect if the matrix blocks of the protection wall are still in place. Replace those matrix blocks
which are cracked.

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3. Replace the ceramic well of the temperature indicator (instrument department).

4. Clean the reaction furnace from dust.

Waste heat boiler

1. Check the lining of the connection to the reaction furnace. Bricks which are not in correct
position have to be replaced

2. Remove the lining and ferrules from the tube plate, in case of severe cracking. Clean the tube
plate and check for leaking tubes and tube welds. Leaking tubes can be plugged off to maximum 5% of the
total number of tubes. Leaking tube welds should be repaired. Install new ferrules, with a 2 mm smaller
diameter than original ones and install new tube plate lining.

3. Tubes to be wire brushed inside and to be air blown, in such a way that they are freed from any
loose scale and dirt before new lining is applied.

4. Remove rust and scale from outlet channel.

5. Clean the waterside of the boiler. Special attention should be paid to the bottom of the boiler
and the blow-down drain.

6. Pressure test of the waterside of the boiler for approximately 2 hours after cleaning activities.

7. Check the main steam valve.

8. Bank testing of the safety relief valves.

Sulphur condensers

1. Remove rust and scale from the inlet channel. Check the condition of the lining in the inlet
channel. If the concrete surface is not flat, fill the holes with concrete and smoothen surface. Clean the tube
plate and check for leaking tubes and tube welds. Leaking tubes can be plugged off to maximum 5% of the
total number of tubes per condenser. If the lowest row of tubes has to be plugged off, install additional
concrete layer in the inlet channel to prevent collection of sulphur. Leaking tube welds should be repaired.

2. Tubes to be wire brushed and to be air blown inside, in such a way that they are freed from any
loose scale and dirt.

3. Remove rust and scale from the outlet channel. Sulphur outlet nozzle to be wire brushed.
Check the condition of the lining in the outlet channel. If the concrete surface is not flat, fill the holes with
concrete.

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4. Clean the waterside of the condensers. Special attention should be paid to the blow-down drain
nozzle.

5. Check the condition of the wire mat. If the mat is fouled and cleaning is impossible, the wire mat
has to be replaced.

6. Pressure test the steam coil, which is installed below the demister.

7. Pressure test the water side of the condensers for approximately 2 hours after cleaning
activities.

8. Check the main steam valve.

9. Bank testing of the safety relief valves.

Reactors

1. Open the top manholes of the reactors (catalyst should be protected during rainfall).

2. Check the condition of the top layer of the catalyst. In case only the top layer is soothed (black),
the top 100 mm is replaced. If the catalyst is heavily soothed, the recommended procedure for removing the
soot is by screening. The catalyst has to be taken out of the reactor. Never burn off carbon deposits.

3. Take catalyst samples from each reactor, halfway each catalyst layer. The samples are sent to
the catalyst manufacturer for analysis. Sampling of the catalyst is advised some time prior to the
maintenance shut-down.

4. Check the condition of the concrete lining as far as possible. If the refractory material is
dropped or loose from the cracks, which are usually present, the refractory should be repaired.

5. Remove the expansion bellows from the gas outlet piping for cleaning and examination of the
bottom part of the reactor.

6. Check the condition of the support grid and gauze.

7. Check the expansion bellows.

8. Lock the expansion bellows before removing them.

9. Leak test the expansion bellows.

10. Check the smothering steam nozzle and valve.

Sulphur coalescer

1. Clean the inside of the coalescer from loose scale and dirt.

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2. Check the condition of wire mat. If the mat is fouled and cleaning is impossible, the wire mat
has to be replaced.

3. Pressure test the steam coil, which is installed below the demister and at the outside of the
drum.

4. Check the condition of the demister support.

5. Sulphur outlet nozzle to be wire brushed.

6. Check the condition and the mounting of the gas inlet device.

Thermal oxidiser

1. Check the condition of the concrete lining. If refractory material is dropped or loose from the
cracks, which are usually present, the refractory should be repaired.

2. Clean the chamber from dust.

3. Check the air distributors for corrosion.

Sulphur seals

1. Remove as much as possible the sulphur from the seals as follows:

¾ Close the valve in the sulphur rundown line.

¾ Connect steam or nitrogen hose on the utility connection of the sulphur seal.

¾ Admit steam or nitrogen to the sulphur seal, thereby removing sulphur from the seal.

2. Disconnect steam hose.

3. Remove the sulphur seals from their shafts.

4. Remove the bottom flange of the sulphur seal and clean the inside of the seal.

5. Pressure test the steam jacketing of the seals.

6. Check the valves.

7. Check the condition of the funnels.

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Sulphur pit

1. Sulphur pit should be pumped out and cleaned completely.

2. Sulphur pumps should be removed and overhauled.

3. Bottom pumps to be cleaned.

4. Inlet and outlet vent pipes to be wire brushed.

5. Check supports of the sulphur pit covers.

6. Check condition bubble columns, including baffles and air spargers.

7. Check spindle-operated plug valve in sulphur pit partition wall.

Steam coil in sulphur pit

1. Wire brush the outside surface of the steam coils, including inlet and outlet piping inside the
sulphur pit.

2. Pressure test the steam coils in order to detect leaks. Leaking welds to be repaired.

3. For maximum security, the condition of the welds can be checked by X-raying.

Running equipment

1. For inspection and maintenance of all running equipment, reference is made to the
maintenance instruction manual of the manufacturers.

2. Suction screens of pumps and blowers to be cleaned and checked.

Piping and valves

1. Wire brush all sulphur lines.

2. Wire brush the main process gas lines.

3. Steam out the fuel gas lines. Remove and clean filters in these lines. Replacement of filters
may be required.

4. Lubricate and ease all valves.

5. Clean all steam traps and lines.

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6. Clean all restriction orifices in purge lines.

Analysers

1. Clean sample valves and sample lines (with steam).

2. Clean internal of analysers according to the manufacturer’s instructions.

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3.3.7 Analytical Requirements

See ANNEX VI

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3.4 EQUIPMENT AND INSTRUMENT LISTS

3.4.1 Equipment List

See ANNEX VII

3.4.2 Instrument List

See ANNEX VIII

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4 OUTLINE FOR INDIVIDUAL MAJOR EQUIPMENT


See ANNEX IX

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5 SUPPORT SYSTEMS
See ANNEX XI and ANNEX XII

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