Tetrahydro Fur An

A
PROJECT REPORT ON
TETRAHYDROFURAN
PREPARED BY:
AMEY
KALBHOR
(U15CH002)
PRASIL KAPADIYA
(U15CH003)
B.TECH IV
CHEMICAL ENGINEERING DEPARTMENT
GUIDED BY
Dr. SANJAY R. PATEL

ASSOCIATE PROFESSOR
DEPARTMENT OF CHEMICAL ENGINEERING
Sardar Vallabhbhai National Institute Of Technology

Surat-395 007, Gujarat, INDIA
i
CERTIFICATE
This is to certify that the B.Tech IV (8th Semester) PROJECT REPORT entitled
“TETRAHYDROFURAN” has been presented and submitted by candidates AMEY
KALBHOR bearing roll no. U15CH002, and PRASIL KAPADIYA, bearing roll no.
U15CH003, in the partial fulfilment of the requirement for the award of degree B.Tech in
Chemical Engineering.
They have successfully and satisfactorily completed their PROJECT EXAMS in all
respects. We certify that their work is comprehensive, compete and fit for evaluation.
Dr.Sanjay R. Patel
Project Guide
Associate Professor
Dept. Of Chemical Engineering
SVNIT, Surat
PROJECT EXAMINERS:
Examiner signature with date
Examiner 1
Examiner 2
Examiner 3 DEPARTMENT
SEAL
ii
AMEY KALBHOR (U15CH002) and PRASIL KAPADIYA(U15CH003), registered in

Chemical Engineering Department of S.V.N.I.T. have successfully completed the project
report entitled “Production Of TETRAHYDROFURAN” during year 2018-2019. The
preliminary report is presented before the following members of the Committee.
Sign Date
1) Examiner-1
2) Examiner-2
3) Examiner-3
The Project preliminary report entitled “Production of TETRAHYDROFURAN” is

submitted to the Head (ChED) along with this certificate.
Place: Surat
Date: 08/05/2019
Dr. Sanjay R. Patel

Associate Professor
Chemical Engineering Department
SVNIT, Surat
iii
ACKNOWLEDGEMENT
We would like to express deep sense of gratitude to our guide Dr. Sanjay R. Patel
(Associate Professor, Department of Chemical Engineering, SVNIT, Surat) for his
valuable guidance and motivation, and for her extreme cooperation to complete our project
work successfully. We would also like to thank all the teaching and non-teaching staff for
cooperating us in completing this project.
I express my sincere thanks to Dr. Mausumi Mukhopadhyay, Head of Department of

Chemical Engineering, Sardar Vallabhbhai National Institute of Technology, Surat, who
helped me to accomplish my dissertation work with preciseness and excellence.
In addition, we would also like to thank the department for including project in the
curriculum. Finally, we would like to express our heartfelt thanks to our beloved parents and
our friends for their constant help and wishes for the successful completion of the project.
iv
ABSTRACT
This project report is an attempt to understand the basic principles and technicalities of
manufacturing of a product at an industrial scale. Herein we have selected
TETRAHYDROFURAN as our product. This preliminary report describes about
introduction of Tetrahydrofuran, its various properties including physical, chemical as
well as thermodynamic properties. Also various methods of industrial production practiced
today are introduced and a comparison between them is made and the best and optimized
method of production is chosen according to the feasibility and context of the project. For the
method chosen we have presented an attempt to the material balance and energy balance for
the entire process as well as detailed balance at each stage of the process. We have shown
Kinetics and Thermodynamics, Equipment design and Cost Estimation. Thus this project
represents an idea of industrial production of Tetrahydrofuran.
v
TABLE OF CONTENT
ACKNOWLEDGEMENT....................................................................................................iv
ABSTRACT...........................................................................................................................v
CHAPTER 1: INTRODUCTION.......................................................................................1
1.1 PROPERTIES..................................................................................................................1
1.2 APPLICATIONS............................................................................................................2
CHAPTER 2 :DEMAND AND SUPPLY...........................................................................4
CHAPTER 3: PROCESS SELECTION AND DESCRIPTION......................................9
CHAPTER 4 : DETAILED MATERIAL BALANCE...................................................17
CHAPTER 5 : DETAILED ENERGY BALANCE........................................................24
CHAPTER 6 : THERMODYNAMICCS & KINETICS...............................................34
CHAPTER 7 : PROCESS EQUIPMENT DESIGN........................................................40
CHAPTER 8 : P & ID DIAGRAM...................................................................................69
CHAPTER 9 : PLANT LOCATION................................................................................74
CHAPTER 10 : PLANT LAYOUT..................................................................................81
CHAPTER 11 : COST ESTIMATION............................................................................85
CHAPTER 12 : SAFETY ISSUES ADAPTED...............................................................96
CHAPTER 13 : ENVIRONMENTAL ISSUES.............................................................98
APPENDIX I : MALEIC ACID
APENDIX II : HYDROGEN
APENDIX III : TETRAHYDROFURAN
REFERENCES
vi
CHAPTER 1 : INTRODUCTION
Tetrahydrofuran (THF) is composed of 4 carbon atoms, 8 hydrogen atoms and one oxygen
atom. THF is an organic compound with the formula (CH2) 4O. The compound is classified as
‘Heterocyclic Ether’. THF is a polar molecule. Since oxygen is more electronegative than
carbon and hydrogen, the oxygen pulls electron density towards itself in the form of the
covalent bonds within the ring structure. So, THF mixes readily with other polar species like
water, methanol, ethanol and acetonitrile. Tetrahydrofuran is a general-purpose, highly
volatile organic solvent. It is a colourless, water-miscible, and mobile liquid. THF offers very
good solvent power for numerous organic substances and is used as a starting material for
various synthesis.
[ Tetrahydrofuran ]
1.1 PROPERTIES [3]
Molecular Formula C4H8O
Molecular Weight 72.11 gm/mole
Appearance Colourless Liquid
Odour Odourless
Boiling Point 66 oC
Melting Point -108.4 oC
Vapor Pressure 190.7 kPa at 20 oC
Flash Point -14 oC
Density 0.889 gm/cm3 at 20 oC
1
Lower Explosive Limits 1.8 %
Upper Explosive Limits 11.8 %
Solubility Miscible with water
1.2 APPLICATIONS
Tetrahydrofuran (THF) has many industrial applications as a solvent, reaction medium, or

starting product for synthesis. It can be used alone or along with other solvents in the leather
industry as part of coating systems. It is a cyclic ether with two primary industrial uses. The
major use is as a monomer in the production of polytetramethylene ether glycol (PTMEG), a
component of cast and thermoplastic urethane elastomers, polyurethane stretch fibers
(spandex), and high-performance copolyester-polyether elastomers (COPE).
THF is the solvent used in the synthesis of PVC pipes, which are commonly found in
household plumbing systems
The magnetic tapes used in electronic devices such as computers can be made abrasion
resistant by applying a coat of THF.The chemical is also used for the production of PVC
adhesives as well as for the fabrication of PVC pipe systems that are used in industrial
processes in heating and cooling systems.THF can be used for the production of highly
concentrated solutions, due to its high solvent power. It is used on a wide scale in the
pharmaceutical industry as a reaction medium for the synthesis of organometallic
compounds.
THF is a popular solvent choice for small-scale laboratory experiments, because it can
dissolve a wide variety of organic compounds and has a relatively low boiling point. The
2
low boiling
3
point is convenient, because it makes the solvent easy to remove from the chemical reaction
by evaporation.
Due to strong solubility of Vinyl Chloride, even at a high degree of polymerization, THF is
used as a solvent for synthetic lather coating. Due to its excellent solubility and diffusion
properties, THF is used as a solvent for vinyl and epoxy adhesives. It is used for vinyl
chloride heat-shrinkable film. THF is suitable for printing inks, because slightly soluble
inorganic compounds can be dissolved and evaporation is quick.
THF is widely used as a solvent for special resins such as photosensitive resins, because even
at room temperature it can dissolve various resins, and it is miscible with water and most
organic solvents. It is also used for Grignard and Witting reactions. It is also used as solvent
for purification and reaction in Pharmaceutical and agricultural manufacturing.
4
CHAPTER 2 : DEMAND AND SUPPLY
A large majority of the proposed additions will be based in China. The two largest global
producers of THF are BASF and Dairen Chemical Corporation, together accounting for 47%
of world capacity by the end of 2015.
Figure 2.1 : World Consumption Of THF [15]
Chinese THF production capacity has expanded dramatically (more than 20% per year during
2005–15); even so, the country depends on imports to meet a portion of demand. In 2015,
China accounted for about 44% of global THF capacity and consumption. In 2015, Asia
(including China, Japan, and Other Asian countries) accounted for about 73% of world THF
consumption, including captive production for PTMEG. In Asia, the portion of THF
consumed for PTMEG is more than 88% of total THF demand, to supply the region's rapidly
growing market for spandex.
Asia-Pacific represents the largest regional market for THF, as stated by the new market
research report on Tetrahydrofuran. THF market was valued as USD 2.77 Billion in 2016 and
is projected to reach USD 4.12 Billion by 2022 at a CAGR of 6.9 % from 2017 to 2022. The
growing demand for spandex fibres and polyurethane across the globe is driving the growth
of THF market.The flourishing textile industry across the globe is driving the demand for
PTMEG, which is used as a raw material for producing spandex. This in turn leads to the
increased demand for THF across the globe.
5
In the United States, major producers are both back- and forward-integrated into 1,4-
butanediol and PTMEG. THF is used primarily for PTMEG production, which accounted for
about 80% of total THF consumption in 2015. Solvent production accounted for the
remaining 20%. As the market is already mature, THF consumption in the United States is
expected to grow annually by less than 1% on average through 2020. The growth rate will be
hampered by reduced demand for PTMEG—a market that is affected by a continued decline
in spandex production in the United States, despite modest growth in other markets.
Figure 2.2 : Import Data of THF[15]
Figure 2.3 : Import Volume and Value data for THF[16]
6
Figure 2.4 : Average Price of THF per unit [16]
Table 2.1 : Import Data for THF [16]
Date Origin Port of Unit Quantity Value Per Unit

Country Discharge
(INR) (INR)
Nov 22, Malaysia Nhava KGS 14,400 1,661,565 115

2016 Sheva Sea
Nov 22, Germany Vizac Sea KGS 28,800 3,374,209 117

2016
Nov 22, Malaysia Vizac Sea KGS 14,400 1,651,733 115

2016
Nov 21, Taiwan Chennai KGS 19,550 2,031,249 104

2016 Sea

2016 Sheva Sea
Nov 19, Malaysia Nhava KGS 2,492 287,525 115

2016 Sheva Sea

2016 Sheva Sea
7
2016 Sheva Sea

2016 Sheva Sea

2016 Sheva Sea

2016 Sheva Sea
Nov 19, Malaysia Chennai KGS 11,908 1,661,565 115

2016 Sea
Nov 18, Taiwan Nhava KGS 14,400 1,494,425 104

2016 Sheva Sea

2016 Sheva Sea
Nov 18, Malaysia Nhava KGS 10,899 406,358 116

2016 Sheva Sea
Nov 18, Malaysia Chennai KGS 3,501 1,622,238 113

2016 Sea
Nov 17, Malaysia Vizac Sea KGS 14,400 1,611,213 112

2016

2016 Sheva Sea
Nov 11, Taiwan Chennai KGS 19,580 2,034,157 104

2016 Sea
Nov 10, Germany Chennai KGS 14,400 1,523,920 106

2016 Sea
8
From the above data obtained in the form of graphs and pie charts, we find out that almost all
of the THF used in India is imported mainly from countries like Taiwan, Malaysia and
Germany. The demand exceeds the supply with a huge margin and thus, setting up a THF
plant would be highly profitable.
BASF (Germany), Dairen Chemical (Taiwan), Ashland (US), INVISTA (US), Mitsubishi
Chemical (Japan), LyondellBasell (The Netherlands), Sipchem ( Saudi Arabia), Nova
Molecular Technologies (US) are the key players operating in the THF market.
9
CHAPTER 3 : PROCESS SELECTION AND DESCRIPTION
3.1 Available Processes
3.1.1 By Acetoxylation of Butadiene
Butadiene, Acetic acid and air are mixed and fed to the reactor. Here, acetoxylation of
butadiene is carried out at 70oC and 70 atm.
Chemical Reaction:
3.1.2 From propylene oxide
In this process propylene oxide is isomerized to allyl alcohol at 250-300oC and 1MPa over
Tri- lithium orthophosphate (Li3PO4) catalyst. This allyl alcohol is then hydroformylated to
4- hydroxybutyraldehyde andby-product 3-hydroxy-2-metylpropionaldehyde.Now
hydrogenation of 4-hydroxybutyraldehyde yields 1,4-butanediol. Dehydration of this alcohol
gives THF.
10
Chemical Reaction:
3.1.3 From Acetylene and Formaldehyde
Here, in the reactor acetylene gas is introduced from the bottom and formaldehyde from the
top. From this reaction 2-butyne-1,4diol is obtained. After that hot vapors of 2-butyne-1,4diol
are cooled and later hydrogenated to give 1,4-butanediol. This diol is cyclized in cyclization
tower at 100oC to form THF. THF obtained from cyclization is then distilled for further
purification.
Chemical Reaction:
3.1.4 By Hydrogenation of Maleic Acid
Because of its structure Maleic Acid is an active precursor for preparation of THF.
Maleic acid is passed to a fixed bed hydrogenation reactor and over-head gases from scrubber
incinerated. The crude hydrogenation product is cooled in cooler and passed to a distillation
column to produce commercial grade 1,4-butanediol and water is removed from the top. 1,4-
butanediol is then sent to dehydrator where it is heated to remove water and obtain THF as
product.
11
Chemical Reaction:
3.2 Process Selection
Table 3:2 Tabulated analysis of each of the process used to manufacture THF
Process Acetoxylation From From Hydrogenation

of Butadiene Propylene Acetylene and of Maleic Acid
Oxide Formaldehyd
e
Raw 1. Butadiene 1. Propylene 1. Acetylene 1. Maleic
Materials 2. Acetic Oxide Gas Acid

Acid 2. Hydrogen 2. Formalde 2. Hydrogen
3. Air 3. CO hyde
Catalyst - Tri-Lithium - Palladium-rhenium

Orthophosphate on carbon support
Operating 70 oC 250-300 oC 100 oC 250 oC
Temperatu
re (oC)
Operating 70 atm 9.89 atm 5 atm 7 atm
Pressure
(atm)
12
Process 1. Mixer 1. Isomeriza 1. Reactor 1. Fixed Bed
Units 2. Reactor tion 2. Hydrogen Reactor

3. Distillatio Reactor ator 2. Flash Drum
Involved
n 2. Hydrofor 3. Cyclizatio 3. Distillation
4. Hydrogen mylation n Tower Columns
ator Tower
5. Hydrolyz 3. Scrubber
er 4. Extracting
6. Distillatio Column
n 5. Evaporato
Columns r
7. Cyclizatio 6. Hydrogen
n Tower ator
7. Cyclizatio
n Tower
End Main Product : Main Product : Main Product : Main Product :
Products THF THF THF THF
By Products : By Products : By Products : By Products :
1. Acetic 1. Water 1. Water 1. Water

Acid Vapors 2. GBL
2. Water 2. 1,4- 3. BDO
3. 1,4- butanedio
butanedio l
l
In process 1,2 and 3, cyclization of intermediate product is required to obtain final cyclized
product THF. In process 4, cyclized reactant Maleic Acid is converted into THF. It is better if
we are using the process which is directly converting a cyclized reactant into cyclized
product.
In process 1,2 we are using higher number of process units than process 4. If higher process
units are there, we have to maintain them and higher energy is required for these units.
13
14
From process chemistry, it can be seen that for process 1,2 and 3, higher number of
intermediates are formed. So, we need higher energy to convert them into final product THF.
Therefore, we have selected Hydrogenation of Maleic Acid process to produce THF.
15
3.3 Process Flow Diagram
16
3.3 Detailed Process Description
The process is divided into 6 sections.
A) Preparation of Reactants ( Section 100 )
A feed containing 60% Maleic Acid by weight is fed to a shell and tube heat exchanger which
increases its temperature from 40 oC to 94oC. Then it is fed to a reciprocating plunger pump to
increase its pressure up to 138.8 atm because the liquid head in the reactor is 136 atm.
The Hydrogen fed to the reactor is a combination of recycled hydrogen from the process and
make-up hydrogen. Make up hydrogen is compressed by using two stage compressor upto
138.8 atm and 199oC. This hydrogen stream is fed from the bottom of the reactor alongwith
maleic acid stream. In the reactor, Maleic acid is hydrogenated to produce THF and a number
of intermediates as well as by-products which are carried out with hydrogen in the vapor
phase from the top of the reactor. The vapor product stream leaves the reactor at 136 atm and
249oC. Here, palladium-rhenium catalyst on carbon support is used for hydrogenation.
B) Hydrogen Recycle Loop ( Section 200 )
The vapor product that leaves the reactor is cooled from 249oC to 40oC by passing it through
a shell and tube heat exchanger. The vapor stream is cooled to maximum extent possible
without using refrigeration in order to maximize the liquid fraction at 136 atm so that the
following flash vessel can effectively separate the low-boilers(hydrogen, methane, propane)
from the condensables. Around 99.5% of hydrogen in the product vapor stream from the
reactor is removed and heated from 40oC to 300oC with the help of a shell and tube exchanger
and fed to the reactor. The condensates from this flash drum are passed through another flash
separator at lower pressure in order to remove most of the hydrogen from the stream before it
is fed to the reactive distillation column. From the bottom of this flash drum, a mixture of
THF, GBL(gamma-butyrolactone), BDO(1,4-butanediol), and water is obtained.
C) Liquid Intermediate Recycle Loop ( Section 300 )
The liquid effluent from this flash drum is fed into the feed tray of the distillation tower
which separates heavy liquid intermediates, GBL and BDO in the bottom stream. The
distillate stream contains mostly THF and water which forms an azeotrope at the conditions
within the tower.
17
The column operates at 0.36 atm at a reflux ratio of 0.60. This enables us to obtain 98% of
GBL and BDO in the feed into the bottoms of the tower which is recycled back to the reactor.
The bottom stream leaving the tower is rich in GBL and BDO. The exiting stream is fed to
the bottom of the primary reactor and distillate stream is sent to pressure-swing distillation
process.
D) THF Recovery from Incineration Streams ( Section 400 )
The top product of the first is fed to a second flash drum to remove the THF from the other
components. This flash drum operates at 10.2 atm and 32.2 oC. This significant temperature
drop causes a large portion of the remaining THF to condense out of the incineration streams.
This THF stream is now sent to pressure-swing Distillation column.
E) Pressure-Swing Distillation( Section 500 )
A pressure swing distillation is selected to purify the THF product because of its known
effectiveness in breaking aqueous azeotropes. The first column operates at near atmospheric
pressure (1.02 atm), while the second column operates at an elevated pressure of 6.82 atm.
The pressure differential affects the THF-water azeotrope by moving it from 83 mol% THF at
atmospheric pressure to 71 mol% THF at 6.82 atm. The stream from the first distillation
column contains 95.8% water, 3% butanol and 1% propanol by mass which is sent to a
nearby wastewater treatment plant. The distillate stream contains the THF and water
azeotrope at the atmospheric conditions within the tower and is sent to the high-pressure
distillation column. The tower operates at a reflux ratio of 0.90 which gives the desired purity
of the azeotrope through the distillate without losing a significant amount of THF through the
bottoms.
The distillate from the first distillation column is sent to the second distillation column. The
bottom stream contains 99.97% pure THF by mass. The tower operates at a reflux ratio of
0.86 which gives the required purity of THF through the bottoms.
F) Production and Storage ( Section 600 )
The bottom stream from the distillation column is brought to near-atmospheric conditions for
storage. Due to the extremely flammable and toxic nature of THF, it is stored in a floating-
roof tank with a hold-up of 48 hours.
18
CHAPTER 4 : DETAILED MATERIAL BALANCE
Chemical Reaction :
Maleic Acid THF
Basis : 120 TPD of THF
( Plant works continuously for 24 hours a day )
Maleic acid required to produce 150 TPD of AA
1 kmol of Maleic Acid  1 kmol of THF
72.11 kg/h of Maleic Acid  116.07 kg/h of THF
Maleic Acid required to produce 120 TPD of THF = 120*(116.07/72.11)
= 193.15 TPD of Maleic Acid
At a yield of 86.73 %
Maleic Acid required = 193.15/0.8673 = 222.71 TPD = 9279.76 kg/h = 79.95kmol/h
1 kmol of Maleic Acid  5 kmol of H2
79.95kmol/h Maleic Acid  H2 required = 79.95 * 5= 399.76kmol/h = 799.53 kg/h
19
Section 100 : Reactor Train
At yield of 90.5%,
THF obtained = 72.11 × 9279.76 × 0.905 / 116.07 = 5217.5 kg/h
H2O obtained = 36 × 9279.76 × 0.905 / 116.07 = 2600.98 kg/h
H balance :
1532.4 + 2Y + 153.233 = 2X + 554.71 + 276.95
X-Y = 426.9865 (1)
Overall Balance :
9279.76 + 799.53 +Y = X + 527.5 + 2600.98 + Z
10079.29 = X-Y + 7818.48 + Z
Z = 1815.255 kg/h
20
Section 200 : Hydrogen Recycle Loop
Here, 99.5% of unreacted Hydrogen is recycled back to the Section 100 reactor. It is assumed
that 11.6% of THF is lost from the top.
Y = 0.995 × X (2)
By solving equation 1 &2,
Y= recycled Hydrogen = 88666.518 kg/h
X = Hydrogen obtained from top of the reactor Section 100 = 89112.08 kg/h
From top, THF = 0.115 × 5217.5 = 605.23 kg/h
Hydrogen = 89112.08 – 88666.518 = 445.562 kg/h
Water = 10.435 kg/h
From bottom, THF = 5214.5 – 605.23 = 4612.27 kg/h
Water = 2600.98 – 10.435 = 2590.545 kg/h
Waste = 1812.255 kg/h
21
Section 300 : Liquid Intermediate Recycle loop
From VLE data, ( 1 for THF, 2 for water )
y1 =0.728 x1 =0.143
y2 =0.272 x2 = 0.857
THF Balance :
4612.27 = V (0.728) + L(0.143)
Water Balance :
2590.545 = V (0.272) + L (0.857)
Solving this equations, we get,
V = 6123.748 kg/h
L = 1078.865 kg/h
THF from top = 6123.748 × 0.728 = 4457.832 kg/h
THF from bottom = 4612.27 – 4457.832 = 154.28 kg/h
Water from top = 6123.748 × 0.143 = 1665.916 kg/h
Water from bottom = 2590.545 – 1665.916 = 924.625
22
kg/h
23
Waste at bottom = 1815.255 kg/h
Section 400 : THF recovery
At 136 atm pressure, all Hydrogen will be obtained from the top only and all water from
bottom.
Assuming 10.34 % loss of THF,
THF obtained from top = 605.23 × 0.1034 = 62.61 kg/h
THF obtained from bottom = 605.23 – 62.61 = 542.62 kg/h
24
Section 500 : Pressure-Swing Distillation
Overall Balance :
542.62 + 4457.832 + 10.435 +1665.916 = L1 + L2
L1 + L2 = 6676.803
Overall H2O Balance :
10.435 + 1665.916 = (L1 × 1) + ( L2 × 0.000075)
1676.351 = 6676.803 L2 + 0.000075 L2
Solving Equations,
L1 = 1675.976 kg/h
L2 = 5000 kg/h
1st Column Operating at 1 atm
THF balance :
542.62 + 4457.832 + (A*0.907) = (B * 0.9514) + 0
5000.452 + 0.907A = 0.9514B
25
Overall Balance :
542.62 + 10.435 + 4457.832 + 1665.916 + A = B + 1675.976
B = A + 5000.827
Solving both equations,
A = 5465.36 kg/h
B = 10466.19 kg/h
In A stream,
THF = 0.907×5465.36 = 4957.08 kg/h
Water = 0.093×5465.36 = 508.28 kg/h
In B stream,
THF = 10466.19×0.9514 = 9957.53 kg/h
Water = 10466.19×0.093 = 508.656 kg/h
Here, THF obtained from 2nd distillation column = 5000 kg/h = 120 TPD
26
CHAPTER 5 : DETAILED ENERGY BALANCE
5.1 Data
5.1.1 Heat capacity constants
Compound Heat Capacity: Cp = A+BT+CT2+DT3+ET4

(J/mol*K)
A B C D E
MAC -15.115 0.58902 -0.00064675 3.681× 10-7 -8 × 10-11
Hydrogen 29.088 -0.00192 0.000004 -8.7 × 10-10 0
Water 32.218 0.00192 0.00001055 -3.593 × 10-09 3.6934 × 10-12
THF 32.887 0.024554 0.00060226 -0.000062385 1.8528 × 10-10
5.1.2 Heat of formation of compounds
Heat of formation
Compound (KJ/mol)
MAC -789
Hydrogen 0
Water -285.82
THF -184.9
5.1.3 Antoine equation constants
Compound Antoine constants

A B C
Water (base e, kPa) 16.3872 3885.7 -42.98
THF (base 10, bar) 4.12118 1202.942 -46.818
27
5.1.4 Temperature dependent enthalpy equation
𝐶p 𝑑𝑇
ΔHT = ΔH298.15
𝑇
+∫ 298
ΔHT = ΔH298.15 + (A+B (A+BT+CT2+DT3+ET4) dT

𝐴 𝐵 𝐶 𝐷 𝐸
ΔHT2 = ΔHT1 + [ (T1-T2) + (T12-T22) + (T13-T 3) + (T14-T 4) + (T15-T 5)]
5
1 2 3
2 2
2
Section 100: Reactor Train
Heat going inside the reactor:
1. Heat contained in Maleic Acid stream:

376.9
ΔH376.95 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
Heat in with Maleic Acid is, ΔH376.95= -6.203×107 kJ/h
2. Heat in with Fresh Hydrogen(198oC):

471.15
ΔH471.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
28
Heat in with Hydrogen at 198oC ΔH471.15= 1.995×106 kJ/h
29
3. Heat in with Recycled Hydrogen(300oC):
573.15
ΔH573.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
Heat in with Hydrogen at 300oC is, ΔH573.15= 3.53×108
kJ/h Thus, total heat going inside the reactor:
Heat in = -6.203×107 + 1.995×106 + 3.53×108
= 2.93×108 kJ/h
Heat generated by reaction:

522.15
ΔH522.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
Heat generated during reaction is, ΔH522.25 = -7.369×107 kJ/h
Heat leaving the reactor:
1. THF:
522.15
ΔH522.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
Heat going out with THF is, ΔH522.25 = -8.5928×108 kJ/h
2. Water:
522.15
ΔH522.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
Heat going out with water is, ΔH522.25 = -4.018×107 kJ/h
3. Hydrogen
522.15
ΔH522.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
ΔH522.25 = 6.105×108 kJ/h
Total heat out = -8.5928×108 + -4.018×107 + 2.89×108
= -6.105×108 kJ/h (exothermic)
30
Heat balance of reactor: Q = ΔHo – ΔHo
product
- ΔH
reactant 522.25
= -6.105×108 -2.93×108 + 7.369×107
= -2.30×105 kW
Heat Exchanger:
Heat duty of the Heat Exchanger Q = 2.30×105kW
Cooling water is used to cool this stream
2.30×108 = nw× [{32.218× (522.25-298.15) + 0.00192× (373.152-305.372)/2 +
0.00001055× (373.153-305.373)/3 – 3.593×10-9× (373.154-
305.374)/4 + 3.6934*10-12× (373.155 - 305.375)} +
{32.218× (420.75-373.15) + 0.00192× (420.752-373.152)/2 +
0.00001055× (420.753-373.153)/3 – 3.593×10-9× (420.754-
373.154)/4 + 3.6934×10-12× (420.755 – 373.155)} + 40626]
Moles of water required, nw= 13700000 mol/h
Mass of water required, mw = 68.5 kg/s
Section 200: Hydrogen Recycle Loop
31
In this section the streams are just getting split in two sections or are obtained as top
stream or bottom stream.
Thus, the energies will also be split in the order of their mass flow rates.
Heat in (25oC to 40oC)

313.15
ΔH313.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
ΔH313.15 = -2914.46 kJ/kg
Heat of water:
313.15
ΔH313.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
ΔH313.15 = -15850.8 kJ/kg
Heat of Hydrogen:
313.15
ΔH313.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
ΔH313.15 = 216.4 kJ/kg
Total heat in: (-2914.26) ×5217.5 + (-15850.8) ×2600.98 + (216.4) ×89112.08}
= -26926.3 kJ/kg
From top:
THF: -2914.26×605.23/3600 = -489.98 kW
Water: -158050.8×10.435/3600 = -45.94 kW
H2 (recycle): 216.4×88666.518/3600 = 5329.84 kW
H2: 216.4×445.526/3600 = 26.78 kW
From Bottom:
THF: -2914.26×4612.27/3600 = -3733.96 kW
Water: -15850.8×2590.545/3600 = -11406.17 kW
32
Section 300 : Liquid Intermediate Recycle loop
From VLE data, ( 1 for THF, 2 for water )
y1 =0.728 x1 =0.143
y2 =0.272 x2 = 0.857
Calculation of Hf
FHf+ Qw = DHD + WHw + Qc
Heat going inside the reactor
FHf = FHf1 + FHf2
FHf1 : THF FHf2 : H2O
298.79
ΔH298.79 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
FHf1 = [-184.9×1000+ {32.887× (298.79-298.15) –
0.024554× (298.792-298.152)/2 + 0.00060226× (298.793-298.153)/3 –
0.000062385× (298.794-298.154)/4 + 1.8528×10-10× (298.795-
298.155)}] ×4612.27/(3600×72.11)
FHf1 = -21.06 kW
33
298.79
ΔH298.79 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
FHf2 = [-285.82×1000+ {32.218× (298.79-298.15) +
0.00192× (298.792-298.152)/2 + 0.00001055× (298.793-298.153)/3 –
3.593×10-9× (298.794-298.154)/4 + 3.6934×10-12× (298.795-
298.155)}] ×2590.545/(18×3600)
FHf2 = -10.57 kW
FHf = -21.06-10.57 = -31.63 kW
Heat coming out from top of the reactor
DHD = DHD1 + DHD2
DHD1 : THF DHD2 : H2O

349.15
ΔH349.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
DHD1 = -1774 kW
349.15
ΔH349.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
DHD2 = 37.05 kW
DHD1 + DHD2 = -1774 + 37.05 = -1736.95 kW
Heat coming out from bottom of the reactor
WHw = WHw1 + WHw2
WHw1 : THF WHw2 : H2O
WHw1 = ΔHo + CpdT
379.15
ΔH379.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
WHw1 = -150.55 kW
379.15
ΔH379.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
WHw2 = 44.05 kW
34
WHw1 + WHw2 = -150.55 + 44.05 = -106.5 kW
The condenser heat load may be calculated as

QC = mλ where λ is the latent heat of vaporization the values for THF and Water are 2256 kJ/kg
and 2307.52 kJ/kg respectively.
Hence total QC is obtained as 1.404 x 107 kJ/h.
Substituting the values obtained in the heat balance equation we get
QW = 2088.18 kW
Section 400 : THF recovery
Heat in:
THF: -2914.26×605.23/3600 = -489.98 kW
Water: -158050.8×10.435/3600 = -45.94 kW
H2: 216.4×445.526/3600 = 26.78 kW
Heat out from top:
THF: -2914.26×62.61/3600 = -50.96 kW
H2: 216.4×445.526/3600 = 26.78 kW
35
Heat out from bottom:
THF: -2914.26×542.62/3600 = -439.29 kW
Water: -158050.8×10.435/3600 = -45.94 kW
Section 500 : Pressure-Swing Distillation
Heat coming in from 3 streams
FHf = FHf1 + FHf2 + FHf3
FHf1 = -1774+ 37.05 = -1736.95 kW (coming from 400)
FHf2 = -165.18 + 0.178 = -165.95 kW (coming from 200)
FHf3 = -5635 + 27.2 = -56.35 kW (coming from recycle of 2nd
column) FHf = = -1736.95 + -165.95 + -5635 kW
Heat going out from bottom of 1st column (water)

376.15
ΔH376.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
WHw1 = [-285.82*1000+ {32.218*(367.15-298.15) +
0.00192*(367.152-298.152)/2 + 0.00001055*(367.153-298.153)/3 –
36
3.593*10-9*(367.154-298.154)/4 + 3.6934*10-12*(367.155-
298.155)}]*1675.976/(18*3600)
WHw1 = 53.18 kW
Heat going out from bottom of 2nd column
WHw2 = WHw(THF) + WHw(water)
WHw(THF) : THF WHw(water) : H2O
WHw(THF) = ΔHo + CpdT

421.15
ΔH421.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
WHw(THF) = -6787.017 kW
421.15
ΔH421.15 = ΔH298.15 +∫ 298 𝐶p
𝑑𝑇
WHw(water) = 0.023 kW
WHw(THF) + WHw(water) = -6787.017 + 0.023 = -6733.837 kW
1 atm column
FHf = -7536.95 kW
WHw1 = 53.18 kW
For DHD:
337.15
ΔH337.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
DHD1 = - 2854.83 kW
337.15
ΔH337.15 = ΔH298.15 +∫ 𝐶p 𝑑𝑇
298
DHD2 = 8.109 kW
DHD1 + DHD2 = -2854.83 + 8.109 = -2846.72 kW
37
For 7 atm column
FHf = -2846.72 kW
38
WHw = -6787.017 kW
DHD = -5635 kW
All three values have been calculated in earlier sections.
39
CHAPER 6 : THEMODYNAMICS & KINETICS
6.1 Thermodynamics
For any reaction to take place, we must check its thermodynamic and kinetic feasibility. If
the reaction is feasible, then, one may proceed towards production.
A well-known thermodynamic property, Gibbs free energy (ΔG), gives the feasibility and the
spontaneity of the reaction. Thus, we can evaluate whether or not our reaction is spontaneous
or not by the value of ΔG as follows:
If ΔG < 0 reaction will occur
If ΔG > 0 reaction will not occur
Thus, we will check this thermodynamics feasibility for the guiding chemical reaction:
Maleic Acid THF
Thus, we calculate ΔG for this reaction. Below we have tabulated the thermodynamic
properties from the literature.
ΔGo
Component (kJ/mole) ΔHo (kJ/mole)
Maleic Acid -468.46 -789
Hydrogen 0 0
THF -59.06 -184.9
Water -237.14 -285.82
Table 5: Enthalpy, Gibbs free energy, and Entropy values of formation of all the reactants
and products (Note that all data is at 298.15 K).
40
Reaction occurs at 522.15 K.
Moles of components in the rector.
Mole
Component Moles Fraction
Maleic Acid 79950 0.2694
THF 72354.74 0.2438
Water 144498.9 0.487
Hydrogen (inert) 44556040 0.993
𝑃
( 𝑖)
P
We use the formula, G = Go + RT ln
Here, the ratio 𝑃𝑖 mole fraction of the respective compound.

P
ΔGMAC = ΔGo M + RT ln(0.2694)
= -468.46 + 8.314×522.15×ln(0.2694)
= -6162.62 kJ/mole
ΔGTHF = ΔGo T + RT ln(0.2438)
= -59.06 + 8.314×522.15×ln(0.2438)
= -6186.553 kJ/mole
ΔGWater = ΔGoWater + RT
ln(0.487)
= -237.14 + 8.314×522.15×ln(0.487)
= -3360.563 kJ/mole
ΔGHydrogen = ΔGoHydrogen + RT ln(0.993)
= 0 + 8.314×522.15×ln(0.993)
= -28.22 kJ/mole
41
ΔGreaction = ΣΔGProduct – ΣΔGReactant
= -3240.386 kJ/mole
Enthalpy change for each component is given by the formula as listed below.
522.15
ΔH522.15 = ΔH298.15 +∫ 298 𝐶p 𝑑𝑇
Cp=A+BT+CT2+DT3+ET4 J/(mole K)
Component A B C D E
Maleic Acid -15.115 0.58902 -0.00065 3.68E-07 -8E-11
Hydrogen 25.399 0.020178 -3.9E-05 3.19E-08 -8.8E-12
THF 32.887 0.024554 0.000602 -6.2E-05 1.85E-10
Water 33.933 -0.0084186 2.99E-05 -1.8E-08 3.6934×10^-12
= ΔHo + 522.15 𝐶p 𝑑𝑇
∫MAC 298.15
ΔH
= -789 + 31.283
= -757.717 kJ/ mole
522.15
ΔHHydrogen = ΔHo +∫298 𝐶p
𝑑𝑇
= 0 + 6.479
= 6.479 kJ/ mole
ΔH ∫Water
= ΔHo + 522.15
𝐶p
𝑑𝑇
298.15
= -285.82 + 7.767
= -278.052 kJ/ mole
ΔH ∫THF
= ΔHo + 522.15
𝐶p
𝑑𝑇
298.15
42
= -184.9 - 1001.84
= -1186.74 kJ/ mole
43
ΔHreaction = ΣΔHProduct – ΣΔHReactant
= -2216.03 kJ/mole
Applying the Gibbs free energy equation at T= 473 K
ΔGreaction = ΔHreaction – T × ΔSreaction
-3240.386 = -2216.03 – 522.15 × ΔSreaction
ΔSreaction = 1.962 kJ/mole
Since this energy is positive so our reaction is feasible according to thermodynamics.
6.2 KINETICS
Our chemical reaction is as follows:
Maleic Acid THF
Let A=Maleic Acid
B=Hydrogen
Molar flow rates of the reactants are,
A = 9279.76 kg/h
= 79950 mol/h
B = 89466.05 kg/h
= 44733024 mol/h
The operating conditions in the reactor are 522.15 K and 136.09 atm. Thus, we need to
calculate the densities of our compounds at these conditions.
44
Density (A) = 560.078 kg/m3
Density (B) = 6.0863 kg/m3
For Maleic Acid (A),
QA (m3/h) = 9279.76/560.078 = 16.5687 m3/h
CAo = (feed rate/flow rate) = 79950/16.5687 = 5.432 mol/m3
For Hydrogen, (B)
QB = (m3/h) = 89466.05/6.0863 = 14699.58 m3/h
CBo = (feed rate/flow rate) = 44733024/6.0863 = 3039.7237 mol/m3
From the general equation for a second order reaction in a CSTR ;
-rA = kCACB
-rA = kCAo2× (1-XA) × (M-XA)
M = CB0/CA0 = 3039.7237/5.432 = 559.475
From literature of a reference paper, the residence time of the reactants in the reactor is 40 s.
Thus, τ = 40 s
𝐶𝐴𝑂× 𝑋𝐴
τ= −𝑟𝐴
5.433 ×0.905
𝑘 ×5.433× 5.433
40 =
×(559.475−5×0.905)
k= 7.9×10-5 m3/mol×s
Now that we have the values of “k” and τ we will plot the graph of -1/ r A Vs XA, for different
XA values. The area under this curve will be V/Fo. From there, we can easily find the volume
of the reactor.
45
XA CA CB 1/(-r)
0 0.00543 3.039723763 1.022169301
0.2 0.00435 2.43177901 1.597139532
0.4 0.00326 1.823834258 2.839359168
0.6 0.00217 1.215889505 6.388558129
0.8 0.00109 0.607944753 25.55423252
1 0. 0 0
-1/rA vs XA
30
25
20
15
-
10
0
0 0.2 0.4 0.6 0.8 1 1.2
XA
Area under curve = 5.983476
Therefore, V/ Fo = 5.983476
Fo = 92375.84 mol/s
V = 74.4826 m3
46
CHAPTER 7 : PROCESS EQUIPMENT DESIGN
7.1 Major Equipment Design : Reactor
7.1.1 Shell
Operating Temperature (T) 249

C o
Operating Pressure 14.064 N/mm2

Design Pressure (P) 15.470 N/mm2
Internal Diameter (Di) 3.645 m
Corrosion Allowances (CA) 2.000 mm
High Tensile Steel
Material Of Construction (Cr, Mo, V)
Permissible Internal Stress (UTS) 500 N/mm2
Permissible Stress (YS) 700 N/mm2
Modulus Of Elasticity E 200000 N/mm2
L/D 2
Length Of Reactor (L) 7.29 m
V 76 m3
Joint Efficiency (J) 1
External Pressure (Po) 0.1 N/mm2
Vessel Radius (R) 1822 mm
Vessel Diameter (Di) 3644.5 mm
Vessel Outer Diameter (Do) 3768.5 mm
Density Of MOC () 7850 kg/m3
Torque about Vertical Axis 100 N m
Poison Ratio () 0.3
According to Indian Standard 2825, taking 10% extra pressure for
design, P = 1.1 × 14.064 = 15.470 N/mm2
47
Thickness of Vessel,
𝑓𝐽+
0.
𝑡 = 𝑅𝑖 × [{(
𝑃
�5 − 1] + C.A.
𝑓𝐽−
𝑃𝑖 )}
Putting all values from table,
t = 59.28 mm
Now, based on market availability, nearest highest thickness available, t = 62 mm
R2 = R + t = 1884 mm
K = 𝑅2 = 1.03
𝑅1
Variation of Stress along the thickness :

𝑝𝑖−𝑝𝑜
𝐾2 = 222
𝐾2−1
A=
(𝑝𝑖−𝑝𝑜)
𝑅 2 𝐾2 1 = 788532720.24
𝐾2−1
B=
𝐵
Tangential Stress, fp = A +
1
= 459.46 N/mm2
�
𝐵
Radial Stress, fR = A -
1
= -15.47 N/mm2
�
𝑝𝑖
Longitudinal Stress,
= 𝐾2−
fa = 223.54 N/mm2
1
𝑝𝑖
Average Stress,
= 𝐾−
fav = 454.69 N/mm2
1
The Extent of prestressing,
fp-fav = 459.46 – 454.69 = 4.77 N/mm2 (Compressive)
48
Maximum Stress Theory :
P = 15.470 – 0.1 = 15.37 N/mm2
K=( 0.
5
𝑓 )
= 1.0197
(𝑓−𝑝𝑖 √3)
R2 = 1.0197 × 15.470 = 1858.16 mm

Thickness, t = 1858.16 – 1822 = 35.91 mm
So, for safe designing, taking thickness t = 62 mm
Combined Loading Calculation :

𝑡′ = corroded thickness = 62-2 = 60 mm
1) Tangential Stress
𝑝(𝐷𝑖+𝑡𝘍)
2𝑡𝘍
t
f
= 15.470 × (3644.5 + 60) /(2×60)
ft = 477.58 N/mm2 (Tensile)
2) Longitudinal Stress
(a) Due to internal pressure
𝑝𝐷𝑖
f1 =
4𝑡𝘍
= 15.470 × 3644.5/(4×60)
= 234.92 N/mm2 (Tensile)
(b) Due to Vessel and Contents
𝑊
f2 =
𝜋𝑡𝘍(𝐷𝑖+𝑡𝘍)
× (𝐷2 − 𝐷2) × h × moc
𝜋
Weight of vessel =
4 𝑜 𝑖
= 41287.92 kg
Weight of material = 1590 × 76 = 120840 kg
Weight of head = 20997.11 kg
Taking 60% extra weight for Nozzle,
Total Weight of reactor (W) = 1.6 × 183125.03
= 293000.048 kg
f2 = 4.118 N/mm2 (Compressive)
49
(c) Due to wind or piping
𝑀
f3 =
𝜋𝐷
𝑖
=0
Total Stress in the longitudinal direction,
fa = f1+f2+f3
= 234.92 – 4.118
fa = 230.80 N/mm2
3) Stresses Due to offset or piping
2𝑇
fs =
𝜋𝐷𝑖𝑡𝘍(𝐷𝑖+𝑡𝘍)
fs = 0.0000786 N/mm2
𝑓𝑅 = √(𝑓2 + 𝑓2 + 2𝑓2 − 𝑓 𝑓 )
Resultant Stress,
𝑡 𝑎 𝑠 𝑡 𝑎
= 413.67 N/mm2
𝑓 =𝐸
1 2𝑡𝘍
𝑐,𝑝𝑒𝑟𝑚𝑖𝑠𝑠 12 3 𝐷𝑜
𝑖𝑏𝑙𝑒 1−µ2)
√3(
𝑓𝑐,𝑝𝑒𝑟𝑚𝑖𝑠𝑠𝑖𝑏𝑙𝑒 = 321.20 N/mm2

 Satisfying Conditions :
1.
fr ≤ ft,permissible : 413.67 ≤ 500
2.
fa,tensile ≤ ft,permissible : 234.92 ≤ 500
3.
fa,compressive ≤ fc,permissible : 4.118 ≤ 321.20
All conditions are satisfied. So, design of reactor with thickness 62 mm is safe.
7.1.2 Head
Here, pressure is greater than 15 atm. So, Hemispherical Head is used.
𝑃𝐷𝑖
Thickness of Head,
𝑡 + 𝐶. 𝐴.
= 4𝑓𝐽 −
𝑃
Putting values,
We get, t = 30.4 mm
Now, based on market availability, nearest highest thickness available, t = 34 mm
50
Total volume of head,
V = 2×2
× 𝜋 × 𝐷𝑂
3 3
3 𝑖
8
= 2×2
3
× 𝜋 3×−3644.53 × 10−9
3768.5
8
3
= 2.67 m
Total Weight of Head = V × moc
= 2.67 × 7850
= 20997.11 kg
7.1.3 Flange Design

Choosing Asbestos Gasket,
Gasket Width (N) 20 mm
Gasket Seating Stress (Ya) 11.2 N/mm2
Atmospheric Stress (f) 58.7 N/mm2
Operating Stress (f) 56.2 N/mm2
Gasket Factor (m) 2
Inside diameter of flange = Radius of Vessel = Gi = 1822 mm

Outside diameter of flange Go = Gi + 2N = 1862 mm
Diameter of Gasket Load Reaction, G = (Gi + Go)/2 = 1842 mm
Basic gasket seating width bo = (Go - Gi)/4 = 10 mm
Effective Gasket seating width b = 2.5√𝑏𝑜 = 7.91 mm

Wm,atm = πbG Ya = 3.14 ×7.91×1842×11.2 = 512196.1 N/mm2
𝑊𝑎𝑡𝑚
Aatm = = 512196.1/58.7 = 8725.66 mm2
𝑓
𝐺2𝑃 = 44045915.7 N/mm2

𝜋
Wm,operating = 2πbGmP +
4
𝑊𝑜𝑝𝑒𝑟𝑎𝑡𝑖𝑛𝑔
Aoperating = = 44045915.7/56.2 = 783735.2 mm2
𝑓
𝐺
Number of bolts Nb =
25.4
= 1842/25.4
= 73
Choosing M-18 size of bolt, X=18 mm
Area per one bolt, Y = 0.51 ×
51
(𝑋)2.09
= 0.51 × (18)2.09 = 214.33 mm2
52
Area of bolt, A = Nb × 𝑌 = 73 × 214.33 = 3858 mm2
2𝜋𝑌𝑎𝐺𝑁
𝑓𝑎𝑡𝑚
Maximum Permissible bolt Area Ab =
= 2×3.14×11.2×1842×20/58.7
= 44148.7 mm2
Here, Ab > A
So, design is safe.
7.1.4 Flange Thickness

𝜋
𝐺2𝑃
4
Total Hydraulic End force H =
=� × 1842 × 15.470
2
�
4
= 41215977.2 N
Bolt Circle Diameter B = Go + 2 X + 12
= 1862 + (2 ×18) + 12
= 1910.3 mm
𝐵−𝐺
Radial Distance From Gasket Load Reaction to Bolt Circle hG =
2
= (1910.3-1842)/2
= 34 mm
1
𝑘 1.5 × 𝑊 ×ℎ
=
0.3 + ( )
𝑚,ℎ𝑖𝑔ℎ𝑒𝑟 𝐺
𝐻
Putting all values and Wm,higher = 44045915.7
N/mm2 We get, k = 3.034
Flange plate thickness,
tf = 𝐺 √ + 𝐶. 𝐴.
𝑃
𝑘𝑓
Putting all values,

We get tf = 188.036 mm
𝐵×𝜋
Bolt Pitch bp =
𝑁𝑏
= 1910.3×3.14/73
= 82.7 mm
53
𝐵𝑜𝑙𝑡
𝑃𝑖𝑡𝑐ℎ = 82.7/18 = 4.6
𝐵𝑜𝑙𝑡
𝐷𝑖𝑎𝑚𝑒𝑡
𝑒𝑟
which is in the range of 3.5 to 5, so SATISFACTORY

Flange Outer Diameter = B + (2X)
= 1910.3 + (2×18)
= 1946.25 mm
7.1.5 Nozzle Design of Maleic Acid

Velocity of Maleic Acid (v) 5 m/s
Mass flow rate 9279.76 kg/h
Density of Maleic Acid 560.078 kg/m3
9279.76
𝑚̇ ( 3600
𝜌 560.078×
Area of nozzle = = 0.00092 m2
𝑣 5
=
√
𝐴𝑟𝑒𝑎×4
Diameter of Nozzle, dn = = 34.24 mm
𝜋
𝑃𝑑𝑛
Thickness of nozzle, tn =
4𝑓𝐽−𝑃
= 0.267 mm
According to market availability, taking thickness = 10 mm
As calculated above, thickness of shell ts = 62 mm
The maximum horizontal distance AB = 2d = 2×34.24 = 68.47 mm
The maximum vertical distance AD = 6𝑡𝑠 = 6×62 = 372 mm
Or
The maximum vertical distance AD = 3.5𝑡𝑠 + 2.5𝑡𝑛
= (3.5 × 62) + (2.5 × 10)
= 242 mm
Taking minimum vertical distance, AD =242 mm
If the compensation is only provided by nozzle then,
𝐻1 = 𝐻2 = 2.5𝑡𝑠
𝐻1 = 𝐻2 = 2.5 × 62 = 155 𝑚𝑚
The area for which compensation is required,
𝐴 = 𝑑 × 𝑡𝑠
54
= 34.24×62
A = 2123.07 mm2
55
Area available for compensation,.
(i) The portion of the shell or head as excess thickness,
𝐴𝑠 = 𝑑 (𝑡𝑠 − 𝑡′ − 𝐶. 𝐴. )
�
= 34.24 ( 62 - 57.28 - 2)
= 93.09 mm2
(ii) The portion of the nozzle external to the vessel,
𝐴𝑜 = 2𝐻1 (𝑡𝑛 − 𝑡′ − 𝐶. 𝐴. )
�
= 2×155 × ( 10 - 0.267 – 2)
= 2397.25 mm2
(iii) The portion of the nozzle inside the vessel,
𝐴1 = 2𝐻2 (𝑡𝑛 − 2 𝐶. 𝐴. )
=0
Additional compensation required A’= 𝐴 − (𝐴𝑠 + 𝐴𝑜 + 𝐴1)
= 2123.07 − (93.09 + 2397.25 + 0)
= -367.27 mm2
As A”< 0, Area available is higher than area provided. So, there is no need for compensation
through extra ring pad.
7.1.5 Nozzle Design of Hydrogen

Velocity of H2 (v) 10 m/s
Mass flow rate 89466.05 kg/h
Density of Maleic Acid 6.0863 kg/m3
89466.05
(
3600
𝑚 )=
Area of nozzle = = 0.4083 m2
𝜌𝑣 6.0863×5
√
𝐴𝑟𝑒𝑎×4
Diameter of Nozzle, dn = = 721.22 mm
𝜋
𝑃𝑑𝑛
Thickness of nozzle, tn =
4𝑓𝐽−𝑃
= 5.62 mm
According to market availability, taking thickness = 10 mm
As calculated above, thickness of shell ts = 62 mm
The maximum horizontal distance AB = 2d = 2×721.22 = 1442.44 mm
56
The maximum vertical distance AD = 6𝑡𝑠 = 6×62 = 372
mm Or
The maximum vertical distance AD = 3.5𝑡𝑠 + 2.5𝑡𝑛
= (3.5 × 62) + (2.5 × 10)
= 242 mm
Taking minimum vertical distance, AD =242 mm
If the compensation is only provided by nozzle then,
𝐻1 = 𝐻2 = 2.5𝑡𝑠
𝐻1 = 𝐻2 = 2.5 × 62 = 155 𝑚𝑚
The area for which compensation is required,
𝐴 = 𝑑 × 𝑡𝑠
= 721.22×62
A = 44715.5 mm2
Area available for compensation,.
(i) The portion of the shell or head as excess thickness,
𝐴𝑠 = 𝑑 (𝑡𝑠 − 𝑡′ − 𝐶. 𝐴. )
�
= 721.22 ( 62 - 57.28 - 2)
= 1960.71 mm2
(ii) The portion of the nozzle external to the vessel,
𝐴𝑜 = 2𝐻1 (𝑡𝑛 − 𝑡′ − 𝐶. 𝐴. )
�
= 2×155 × ( 10 – 5.62 – 2)
= 737.8 mm2
(iii) The portion of the nozzle inside the vessel,
𝐴1 = 2𝐻2 (𝑡𝑛 − 2 𝐶. 𝐴. )
=0
Additional compensation required A’= 𝐴 − (𝐴𝑠 + 𝐴𝑜 + 𝐴1)
= 44715.5 − (1960.71 + 737.8 + 0)
= 42017.67 mm2
As A” > 0, Area available is lower than area provided. So, there is need for compensation
through extra ring pad.
57
7.2 Major Equipment Design : Distillation Column
Total Feed rate F = 542.62+4457.832+10.435+1665.916
= 6676.803 kg/h
Column Efficiency = 60%
1.2 X-Y Diagram

1
0.8
Y
0.6
0.4
0.2
0
0 0.2 0.4X 0.6 0.8 1 1.2
No. of stages = 10
Actual Number of stages required = 10 / 0.6 =17
Material Balance Equations :
𝑭=𝑫+𝑾
𝑭𝒙𝑭 = 𝑫𝒚𝑫 + 𝑾𝒙𝑾
𝑳
𝑹=
𝑫
𝑽=𝑳+𝑫
𝑳′ = 𝑾 + 𝑽′
𝒎 𝒎
58
TOP :
From top of the Distillation Column, 95.14% THF is obtained.
yD = 0.9514
From bottom of the Distillation Column, almost 100% water is obtained.
xw = 0
D 10466.19 kg/h 150.635 kmole/h

y 0.9514
M.W. 69.48025 kg/kmole
R 0.9
V 19885.76 kg/h 286.207 kmole/h
L 9419.571 kg/h 135.572 kmole/h
Bottom :
W 1675.976 kg/h 93.1098 kmole/h

x 0
M.W. 18 kg/kmole
Lm'/Vm' 1.5
Lm' 5027.928 kg/h 279.329 kmole/h
Vm' 3351.952 kg/h 186.22 kmole/h
Assuming Sieve Tray,
Pressure drop per tray = 100 mmH2O
Column Pressure = N × × g × h
= 17 ×1000×9.81×100×10-3
= 16.35 kPa
Top Pressure = 1.02 atm = 103.3515 kPa
59
Bottom Pressure = 16.35 + 103.3515
= 119.7015 kPa
From steam table, we get
Bottom Properties :
Bottom
T 377.15 K
l 955.11 kg/m3
v 0.682 kg/m3
 0.057 N/m
7.2.1 Column Diameter
√( �)
𝜌
𝐹𝐿𝑉 =
Liquid-Vapor flow factor,
𝐿𝑊 𝜌𝐿
𝑉
𝑤
= √(955.11 )
279.329 0.682
186.22
= 0.04
Assuming Tray spacing = 0.5 m

60
From above graph, K1 = 0.09
Correction for Surface Tension, 𝐾′ =

𝐾 ×( 𝜎 0.2
1 1
)
0.02
= 0.09 × (0.057/0.02)0.2
= 0.11097
𝑢
= 𝐾 ′ 𝜌𝐿−𝜌𝑣
1 √( 𝜌
𝑣 )
Flooding Velocity,
𝑓
= 0.11097 √( )
955.11−0.682
0.682
= 4.15 m/s
For design, 80-85% of flooding velocity is used.
Taking 85%,
uf = 0.85 ×4.15 = 3.528 m/s
𝑉𝑎𝑝𝑜𝑟 𝐹𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 × 𝑀.𝑊.

Maximum flow rate Q =𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑣𝑎𝑝𝑜𝑟×3600
186.22 × 18
= 0.682 ×3600
= 1.365 m3/s
𝑄
𝑢𝑓
Net Area requirement =
= 0.387 m2
Downcomer area is 12% of actual area.
𝑁𝑒𝑡 𝐴𝑟𝑒𝑎 0.387

0.88 0.88
Actual Area = = = 0.4398 m2
Diameter of column, 𝑑 = √
4×𝐴
=√
4×0.4398
𝜋
= 0.748 m
According to market availability,
Nearest standard pipe size dc = 0.79 m
61
7.2.2 Provisional Plate Design
Column Diameter dc 0.79 m

Column Area Ac 0.49 m2
Downcomer Area Ad 0.0588 m2
Net Area An 0.431 m2
Active Area Aa 0.3723 m2
Hole Area Ah 0.03723 m2
Weir Length (lw) 0.6004 m
Weir Height (hw) 50 mm
Diameter Of Hole (dh) 5 mm
Plate Thickness 5 mm
Active Area, Aa = Ac – (2dc)
= 0.49 – (2×0.79)
= 0.3723 m2
Hole Active area Ah is taken as 10% of Active area Aa.
Hole area Ah = 0.10 ×0.3723 = 0.03723 m2

From the graph of
𝐴𝑑 × 100 vs 𝑙𝑤 ,
𝑑𝑐
𝐴𝑐
𝐴𝑑
𝐴𝑐 × 100 = 12%
𝑙𝑤
= 0.76
𝑑𝑐
lw = 0.76 ×0.79 = 0.6004 m
62
7.2.3 Check for Weeping
Maximum liquid rate Lm' = 1.397 kg/s
At 70% Turn-down, Minimum Liquid rate = 0.7 ×1.397 = 0.978 kg/s
The height of liquid crest over the weir,
ℎ𝑜𝑤 = 750 × (𝐿𝑚 0.2

𝐿 )
�×
𝑙𝑤
Putting 𝜌𝐿 = 995.11 kg/m3, lw =0.6004 m, hw = 50 mm, we get
Maximum how 13.58 mm

Minimum how 10.70 mm
hw+how (minimum) 60.70 mm
From below graph of ( hw+how ) vs K2 ,
we get K2 = 30.3
63
Minimum design velocity,
𝐾2 − 0.90 × (25.4 − 𝑑ℎ)

𝑢~ =
√𝜌𝑣
ℎ
Putting K2 = 30.3, dh = 5 mm, v = 0.682 kg/m3
𝑢~ = 14.46 m/s
ℎ
𝑄
𝐴ℎ
Minimum Operating velocity = 0.7 ×
1.365
= 0.7 × 0.03723
= 25.66 m/s
So, minimum operating range will be well above weep point.
So, weeping is prevented.
64
7.2.4 Plate Pressure Drop
Maximum vapor velocity through holes,

𝑄
uh =
𝐴ℎ
1.365
= 0.03723
= 36.66 m/s
=1
𝑃𝑙𝑎𝑡𝑒 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠 5
Here, 𝐻𝑜𝑙𝑒 𝐷𝑖𝑎𝑚𝑒𝑡𝑒𝑟 = 5
× 100 ≈ 𝐴ℎ × 100 = 0.03723 ×100 = 10%

𝐴ℎ
𝐴𝑝 𝐴𝑎 0.3723
65
From above graph,
Orifice coefficient Co = 0.84
𝑢ℎ 2 𝜌𝑣
ℎ𝑑 = 51 [ ]
Pressure drop through dry plate,
𝑜
� 𝜌𝑙
Putting all values, we get,
hd = 69.38 mm
Residual head,
ℎ𝑟
=
12500
𝜌𝑙
Putting l = 995.11 kg/m3 , we get
hr = 13.0875 mm
Total pressure drop ht = hd + hr + hw + how
= 69.38+13.0875+ 50 +13.58
= 146 mm
100 mm was assumed to calculate the base pressure. Here, we get 146 mm pressure drop.
This value is acceptable.
7.2.5 Downcomer Liquid Back-up
Height of bottom-edge of apron above
plate, hap = hw – (5 to 10 mm)
= 50 – 10
= 40 mm
Area under apron, Aap = hap ×lw
= 40 ×0.6004
= 0.024 m2
Downcomer Area Ad = 0.0588
66
m2 Ad > Aap
67
So, taking Aap = Am = 0.024 m2
Head Loss in the downcomer,
ℎ𝑑𝑐 = 166 ×
[ 𝐿𝑚 ]2
�𝑙 × 𝐴𝑚
Putting Lm = 1.397 kg/s, we get,
hdc = 0.6154 mm
Back-up in downcomer,
hbc = hw + how + ht +hdc
= 50 + 13.58 + 146 + 0.6154
= 210.2 mm
1
× (𝑙
+ ) = 2 × (0.5 + 0.050) = 0.275 m
1
2
ℎ𝑤
�
< 1 × (𝑙 + ℎ𝑤)
ℎ𝑏𝑐
Here,
2 �
So, plate spacing is acceptable.
Residence time,
𝑡𝑟 𝐴𝑑 × ℎ𝑏𝑐 ×
= 𝜌𝑙
𝐿𝑚
0.0588 × 0.2102 × 955.11

=
1.397
= 8.452 s > 3 s
So, this is Satisfactory.
7.2.6 Check Entrainment
68
𝑄
Entrainment velocity uv =
𝐴𝑛
1.365
= 0.43 = 3.167 m/s
1
69
% Flooding = 𝑢𝑣
𝑢𝑓 × 100
× 100
3.167
= 4.15
= 76.28 %
FLV = 0.04
From the above graph,
Fractional Entrainment Ψ = 0.05 < 0.1
So, Entrainment is prevented.
70
7.2.7 Number of Holes
× 𝑑2
Area of one hole =
𝜋
4 ℎ
× 0.0052
=�
�
4
= 1.96 × 10-5 m2
Total area of hole, Ah = 0.03723 m2
0.03723
1.96 × 10−5
Total Number of holes =
= 1900
7.2.8 Plate Specification
Column Diameter (dc) 0.79 m

Diameter Of Hole (dh) 5 mm
Active Number Of Holes 1897.264
Pitch Triangular
70% max
Turndown rate
Plate Material Mild Steel
Downcomer Material Mild Steel
Plate Thickness 5 mm
Plate Spacing 0.5 m
71
7.3 Minor Equipment Design : Heat Exchanger
Shell side fluid is THF, which is needed to be cooled and Tube side fluid is water.
Thi = 77.4 oC
Tho = 40 oC
Tci = 32.2 oC
Tco = 42 oC
mh = 5000 kg/h
Cph = 5.52 kJ/ kg K
Cpc = 4.2 kJ/ kg K
Heat Load Q = mCpT
= 5000 × 5.52 ×(77.4 - 40)
= 286.73 kW
Mass Flow rate of Cold stream = 286.73 = mc × 4.2 × (42 - 32.2)
mc = 14629.2517 kg/s
Heat Exchanger is of 2 shell, 4 tube type.
Ch = mh × Cph = 5000 × 5.52 = 27600 kJ/ h K
Cc = mc × Cpc = 14629.2517 × 4.2 = 61442.86 kJ/ h K
Cr = Cmin /Cmax = 27600/ 61442.86 = 0.4491
= 61442.86 × (42 – 32.2) / ( 27600 × (77.4 – 32.2 ))
= 0.8274
72
= 1.908
= 0.6224
= 1.6089
= 1.327
NTU = n × (NTU)1 = 2 × 1.327 = 2.654
Assume U = 120 W /( m2 K)
𝑈𝐴
𝑁𝑇𝑈
= 𝐶𝑚𝑖𝑛
A = 2.654 × 27600 /120 = 169.587903 m2
Choosing Cupro Nickel tubes having 20 mm OD and 16 mm ID .

Taking Length of Tube = 5 m
According to market availability, Length of tube L = 4.88 m
Effective length for heat transfer = 4.88 – 0.025 – 0.025 = 4.83 m
For Number Of tubes N,
A = N × π × do × L
N = 559
Taking Extra Tubes, Total number of tubes Nt = 610
1
×[
𝑁𝑡
=
𝑑𝑏 𝑑𝑜 ]𝑛1
Tube Bundle Diameter,
𝐾1
73
For 2 shell, 4 tube passes,
K1 = 0.249
n1 = 2.207
Tube Bundle Diameter, Db = 0.686
Selecting Split-ring Floating head,
Clearance = 63 mm
Shell Diameter Ds = 0.686 + 0.063 = 0.749 mm
74
Calculation Of Inside ( Tube Side ) Heat Transfer Coefficient :
Properties :
T 40.6 o
C
 994 kg/m3
 0.00079 Pa s
kf 0.58 W/(moC)
𝒅 µ 𝟎.𝟏𝟒
𝒉𝒊 × = 𝒋𝑯 × 𝐑𝐞 × 𝟎.𝟑 ×( )
𝟑 µ
𝐏𝐫
𝒊
𝒌 𝒘
Mass Flow Rate m = vt
14629.2517/3600 = 994 × (π/4) × 0.0162 × 610/4 × vt
vt = 0.1334 m/s
𝜌 𝑣 𝑑𝑖
µ
Re = = 994 × 0.1334 ×0.016/0.00079 = 2685.55
𝐶𝑝
µ
Pr =
= 4.2 ×1000 ×0.00079/0.58 = 5.72069
𝑘𝑓
From Graph for L/di = 240,
jH = 0.028
75
Putting Values in above equation, we get,
hi = 4846.82 W/(m2 K)
Calculation Of Outside ( Shell Side ) Heat Transfer Coefficient :
Properties :
T 58.7 o
C
 889 kg/m3
 0.000423 Pa s
kf 0.0115 W/(moC)
𝒉𝒐 𝒅 = 𝒋 × 𝐑𝐞 × 𝟎.𝟑𝟑 𝟎.𝟏𝟒
×( )
× 𝐏𝐫 µ
𝑯
𝒌
𝒆
𝒇 µ𝒘
Assuming Triangular Pitch,
Tube Pitch Pt = 1.25 × (Tube Diameter) = 1.25 × 0.02 = 0.025 m
(𝑃2 − 0.917𝑑2) = 0.0142 m

1.10
Equivalent Diameter, de =
𝑑𝑜 𝑡 0
Baffle Spacing lB = 0.2 × Ds = 0.149 m
(𝑃𝑡 − 𝑑𝑜)
Cross Section Area for shell side fluid,
𝐴𝑆 × 𝐷𝑠 × 𝑙𝑏
= 𝑃𝑡
= 0.0224 m2
Mass Flow Rate, m = svs
5000/3600 = 889 × 0.0224 × vs
vs = 0.0695 m/s
𝜌 𝑣 𝑑𝑜
µ
Re = = 889 × 0.0695 ×0.02/0.000423 = 2922.28
76
𝐶𝑝
µ
Pr =
= 5.52 ×1000 ×0.000423/0.0115 = 203.04
𝑘𝑓
77
At 25% Baffle Cut,
From Graph,
jH = 0.01
Putting Values in above equation, we get,
ho = 136.648 W/(m2 K)
Overall Heat Transfer Coefficient :
Thermal Conductivity of wall material kf = 50 W/(m K)
𝟏 𝟏 𝒅 𝟏 𝟏 𝒅 𝒅𝒐
= 𝟏 + 𝒅𝒐
𝒐 + + 𝒐 + ×
𝑼𝒐 𝒉 𝒉× 𝒉 𝒉 𝟐𝑲
𝒅
𝒐 𝒊 ×
𝒅 𝐥𝐧 𝒅𝒊
𝒐
𝒊 𝒅 𝒅 𝒘
𝒊 𝒊
Taking dirt factor, hod = hid = 5800 W/(m2 K)
78
Putting values in above equation,
U = 124.867 W/(m2 K)
Pressure Drop Calculation :
Shell Side Pressure Drop,
∆𝑃 = 8 × 𝑗 × 𝐷
( 𝑠 ) × (𝐿 𝜌 𝑣2 )
0.14
µ
) × ( �) × (
𝑠 𝐻
𝑑 𝑙𝐵 2 µ𝑤
𝑒
At 25% baffle cut, and Re = 2922.28328 from above graph,

jH = 0.06
Putting Values in above equation,

Ps = 0.2458 psi
79
Tube Side Pressure Drop,
𝐿
∆𝑃 = × [8 × ) + 2.5 ] ×𝜌( 𝑣
�)
−m 2
𝑁 𝑗
µ
×( )×(
µ𝑤 2
𝐻
𝑑𝑖
𝑡 𝑡
From above graph for Re =2685.55, we get

jH =0.006
Putting all values in above equation.
Pt = 1.2845 psi
OD of Tube 0.02 m
Nt (Actual Number Of
Tubes) 610
L (Tube Length) 4.83 m
hi 4846.82 W/(m2 K)
ho 136.648 W/(m2 K)
U 124.867 W/(m2 K)
80
Heat Load (Q) 286.73 Kw
81
CHAPTER 8 : P & ID DIAGRAM
8.1 Introduction :
Instruments are provided to monitor the key process variables during plant
operation. Instruments monitoring critical process variables will be fitted with
automatic alarms to alert the operators to critical and hazardous situations. The
primary objectives of the designer when specifying instrumentation and control
schemes are:
8.1.1 Safe Plant Operation:

 To keep process variables within known safe operating limits.
 To detect dangerous situations as they develop and to provide alarms and
 Automatic shutdown systems.
 To provide interlocks and alarms to prevent dangerous operating procedures.
8.1.2 Production Rate and Quality:

 To achieve the designed product output.
 To maintain the product composition within the specified quality standards.
8.1.3 Cost:
 To operate at the lowest production cost and to compensate with
other objectives. Process instrumentation is thus brain and nerves of a
process plant.
The instrumentation can be pneumatic, hydraulic or electric. The recent trend is to go

for electronic instrumentation, but pneumatic instrumentation is still in use. The
instrumentation is required to measure temperature, pressure, flow rate, level,
physical properties as density, pH, humidity, chemical composition etc.
82
8.2 TYPICAL MONITORING SYSTEMS :
8.2.1 Flow Measurement:
Due to nature of flow it is necessary to provide effective flow measuring devices in

each supply lines. The various types of flow meters available are orifice meter,
venturi meter, pitot tube etc. In spite of these the various types of area flow meters
can also be used.
Depending on temperature and velocity condition the suitable meter is selected for
measurement of flow rates and velocity.
8.2.2 Temperature Measuring Devices:
Many devices are used to measure the temperature variations in the process such as
mercury in glass thermometer, bimetallic thermometer, pressure spring thermometer,
thermocouples, resistance thermocouples, radiation pyrometers and optical pyrometers are
used.
Out of all these the industrial thermocouples are competitively good as they
provide large measuring range, without introducing error. Automatic control is also
possible with such devices.
Table - 8.1 List of Thermometers with temperature Range
Measuring Instrument Temp. Range ºC

Mercury in glass – thermometer -27 to 400
Mercury in pressure thermometer -40 to 540
Vapor pressure thermometer -85 to 425
Resistance -200 to 1700
Thermocouple -250 to 1700
Thermistor Up to 300
Pyrometer 1300 to 2500
83
8.2.3 Pressure Measuring Devices:
Equipment in which the important monitoring parameter is pressure, pressure

measuring device like pressure gauge is widely used. Safety of chemical plants
depends up on the timely measurement of pressure and its control at a specified
level. Any excess pressure development than the design pressure may damage the
equipment in addition to the fire and other explosion hazard.
Mainly in filter pressures where the pressure is an important criterion, this
device is used. Various pressure measuring devices are:
 U – Tube Manometer
 Differential Manometer
 Inclined Manometer
 Diaphragm valve
In addition to all measuring devices described above various measurements like

density, viscosity, pH measurements etc. are installed. For measuring quality
standards in laboratory various laboratory instruments are also necessary.
8.2.4 Liquid Level :
Liquid level detectors measure either the position of a free liquid surface above a
datum level or the hydrostatic head developed by the liquid is measured.
The liquid level is measured both by direct and indirect means. Direct methods
involve direct measurement of the distance from the liquid level to a datum level.
Indirect method follows changing liquid surface position on bubble tube method,
resistance method, radiation method, etc.
8.3 CONTROLLERS POSITIONING :
Over the whole process above mentioned controller were used, the below are
the listed controllers used at different location and why they were opted :
84
8.3.1 Across Reactor :
1. Ratio Controller :
Added to control the inlet compositions of the reactants on the reactor, which is
subsequently attached to Flow controller. Depending upon the value calculated
by the Flow meter, the two values of flow will be considered and according the
inlet feed will be controlled.
2. Temperature Controller :
Added across the reactor for controlling the system temperature to 40 °C. Here by
the reactor temperature is measured and this signal is forwarded to the fixed set
temperature meter. If there is a deviation of the temperature then inlet chilling
water is controlled accordingly by Flow-meter.
3. Pressure Controller :
Our reactor consists gases as primary reactants and so maintaining adequate
pressure is very important. Here we need to maintain high enough to pump the
gases in and out.
8.3.2 Across Distillation columns :
1. Pressure Controller :
Added at the enriching section to control the quality of out-coming distillate, which
is subsequently controlled by controlling the L/D ratio. Which is, in turn is
controlled by the valve.
2. Temperature Controller :
Added at the Stripping Section to control the rate of heating of the residue. The
particular control plays vital role in deciding the product purity and yield during
physical separation by boiling the feed to desirable given temperature. Depending
upon the temperature indicated the inlet flow to the reboiler is controlled by the
valve.
85
3. Level Controller :
Level controller has been connected to the bottom section of the distillation
column before the reboiler so that if required, liquid can be easily drawn out or the
flowrate can be decreased so that the bottom liquid builds up.
86
CHAPTER : 9 PLANT LOCATION
9.1 Introduction
In the discussion of process and equipment design given in the previous chapters no reference
was made to the plant site. A suitable site must be found for a new project, and the site and
equipment layout planned. Provision must be made for the ancillary buildings and services
needed for plant operation; and for the environmentally acceptable disposal of effluent. These
subjects are discussed briefly in this chapter.
9.2 Plant location and site selection
The location of the plant can have a crucial effect on the profitability of a project, and the
scope for future expansion. Many factors must be considered when selecting a suitable site,
and only a brief review of the principle factors are given below. The principle factors to
consider are:
1. Location, with respect to the marketing area.
2. Raw material supply.
3. Transport facility.
4. Availability of labor.
5. Availability of utilities: water, fuel, power.
6. Availability of suitable land.
7. Environmental impact and effluent disposal.
8. Local community considerations.
9. Climate.
10. Political and strategic considerations
87
9.2.1 Marketing area
For materials that are produced in bulk quantities; where the cost of the product per ton is
relatively low and the cost of transport a significant fraction of the sales price, the plant
should be located close to the primary market. This consideration will be less important for
low volume production, high-priced products; Pharmaceuticals. In an international market,
there may be an advantage to be gained by locating the plant within an area with preferential
tariff agreements.
9.2.2 Raw materials
The availability and price of suitable raw materials will often determine the site location.
Plants producing bulk chemicals are best located close to the source of the major raw
material; where this is also close to the marketing area.
9.2.3 Transport system
The transport of materials and products to and from the plant will be an overriding
consideration in site selection. If practicable, a site should be selected that is close to at least
two major forms of transport: road, rail, waterway (canal or river), or a sea port. Road
transport is being increasingly used, and is suitable for long- distance transport of bulk
chemicals. Air transport is convenient and efficient for the movement personnel and essential
equipment and supplies, and the proximity of the site to a major airport should be considered.
9.2.4 Availability of Labor
Labor will be needed for construction of the plant and its operation. Skilled construction
workers will usually be brought in from outside the site area, but there should be an adequate
pool of unskilled labor availability locally; and labor suitable for training to operate the plant.
Skilled tradesmen will be needed for plant maintenance. Local trade union customs and
restrictive practices will have to be considered when assessing the availability and suitability
of the local labor for recruitment and training.
9.2.5 Utilities
Chemical processes invariably require large quantities of water for cooling and general
process use, and the plant must be located near a source of water of suitable quality. Process
water may be drawn from a river, from wells, or purchased from a local authority y. At some
sites, the cooling water required can be taken from a river or lake, or from the sea; at other
88
locations
89
cooling towers will be needed. Electrical power will be needed at all sites. Electrochemical
processes that require large quantities of power; need to be located close to a cheap source of
power. A competitively priced fuel must be available on site for steam and power generation.
9.2.6 Impact on environment and waste disposal
All industrial processes produce waste products, and full consideration must be given to the
difficulties and cost of their disposal. The disposal of toxic and harmful effluents will be
covered by local regulations, and the appropriate authorities must be consulted during the
initial site survey to determine he standards that must be met. An environmental impact
assessment should be made for each new project or major modification or addition or an
existing process.
9.2.7 Local community considerations
The proposed plant must be fit in with and be acceptable to the local community. Full
consideration must be given to the safe location of the plant so that it does not impose a
significant additional risk to the community. On a new site, the local community must be able
to provide adequate facilities for the plant personnel: schools, banks, housing, and
recreational and cultural facilities.
9.2.8 Land
Sufficient suitable land must be available for the proposed plant and for future expansion.
The land should ideally be flat, well drained and have suitable load-bearing characteristics. A
full site evaluation would be made to determine the need for piling or other special
foundations.
9.2.9 Climate
Adverse climatic conditions at a site will increase costs. Abnormally low temperatures will
require the provision of additional insulation and special heating for equipment and pipe runs.
Stronger structures will be needed at locations subject to high winds (cyclone/hurricane) or
earthquakes.
90
9.2.10 Political and strategic considerations
Capital grants, tax concessions, and other inducements are often given by governments to
direct new investment to preferred locations; such as areas of high unemployment. The
overriding of such grants can be the overriding considerations in site selection.
9.3 PLANT LOCATION : OPTIONS

1. Ankleshwar, Gujarat – GIDC INDUSTRIAL AREA
2. Ratnagiri, Maharashtra – LOTE PARSHURAM INDUSTRIAL AREA
3. Kota, Rajasthan – INDRAPRASTHA INDUSTRIAL AREA
GIDC Industrial Lote Parshuram

Indraprastha
Estate, Industrial Area,
Factors Industrial Area,
Ankleshwar, Ratnagiri,
Kota, Rajasthan
Gujarat Maharashtra
Area
Available 1,31,514 29,750 21,900
(m2)
Land Price
₹ 2332 ₹ 9570 ₹ 10,875
(per m2)
1. Pharmaceutical
1. Chemical
2. Chemical
Industry
1. Multi
Types Of Industry
2. Wooden Services
Industry 3. IT Industry
Industry Industry
4. Engineering 3. Food Industry
Industry
1. EASON
Raw 1. Ratnagiri Gas & 1. DCM
Industrial
Material Power Pvt. Ltd. ShriRam
Chemicals
Supplier
2. Chemspec India 2. Indian Oil
2. Jackfeel
91
Chemical Pvt. Ltd. Corporation
3. Vijay 3. Vinati Organics 3. Truchem

Chemicals Ltd. Industries
4. Reliance
Industries
1. Mumbai Port
1. Dahej Port
(245 km)
(60km) 1. Liquid
Port 2. Dighi Port (131
2. Gujarat Chemical
Facilities km)
Maritime Port Terminal
3. Jaigad Port (85
(GMP)
km)
1. Pune
International
Airport
1. Vadodara
2. Mumbai
Airport
1. Maharana
International
Airport 2. Bhavnagar Pratap
Airport
Facilities Airport Airport,
3. Navi Mumbai
Udaipur
3. Ahmedabad
International
Airport
Airport
4. Ratnagiri
Airport
1. Mumbai-Goa
National 1. National
1. National
Highway (NH- Highway
Road Highway 8
17) No. 12
Facilities (Delhi-
(Jaipur-
Mumbai) 2. Guhagar-
Jabalpur)
Chiplun-Karad-
Vijapur (SH
92
136)
1. Connected to 1. Konkan
Delhi-Mumbai Railways 1. Kota has
Broad Gauge Connecting direct trains
Railway railway line at western to Kolkata.
Facilities Bharuch Maharstra to It has 4
2. Bharuch- Goa and Railway
Ankleshwar Banglore via stations.
Railway line Ratnagiri station
1. CGWA provides
water supply
1. GIDC Water through ground
1. Cypriot
reservoir water sources.
Company
2. GWSSB Vishisthi River, Hydro
provides Chiplun- Water Company
Water
drinking water Treatment Plant
Supply 2. Gandhi
through of 24 MLD
Sagar Dam
Narmada capacity to cater
Canal 3. Chambal
to the water
River
3. Ukai Canal need of Lote-
Parshuram
Industrial Area
Tariff for
Water
₹ 23.87 ₹ 25 ₹ 21.6
Supply
( per m3 )
1. Two 220 KV 1. Maharashtra

1. Kota Super
Electricity substations State Electricity
Thermal
Supply located at Distribution Co.
Power Plant
Dahej & Ltd. (MSEDCL)
93
Vilayat within
PCPIR
2. Three 66 KV
substations
located at
Dahej, Luna &
Vilayat within
PCPIR
Tariff for
Electricity
₹ 3.2 ₹ 6.7 ₹ 6.4
Supply
(per kWh)
SELECTION
ANKLESHWAR RATNAGIRI KOTA
CRITERIA
Raw Material
Better Better Good
Availability
Transportation Best Best Best
Utilities Best Best Better
Manpower
Best Better Best
Availability
Availability of Land
Best Best Better
and Price
Political and Strategic
Best Better Better
Considerations
Total Best Better Better
 Thus, as our analysis suggests, the plant location will be GIDC area of
Ankleshwar, Gujarat.
94
CHAPTER 10 : PLANT LAYOUT
The process units and auxiliary buildings should be laid out to give the most economical flow
of materials and personnel around the site. Hazardous processes must be located at a safe
distance from other buildings. Consideration must be given to the future expansion of the site.
The ancillary buildings and services required on a site, in addition to the main processing
units (buildings), will include:
1. Storages for raw materials and products: tank farms and warehouses.
2. Maintenance workshops.
3. Stores, for maintenance and operating supplies.
4. Laboratories for process control.
5. Fire stations and other emergency services.
6. Utilities: Steam boilers, compressed air, power generation, refrigeration, transformer

station
7. Effluent disposal plant.
8. Offices for general administration.
9. Canteens and other amenity buildings, such as medical centre.
10. Car parks
When roughing out the preliminary site layout, the process units will normally be sited first
and arranged to give a smooth flow of materials through the various processing steps, from
raw materials to final product storage. Products units are normally spaced at least 30 m apart;
grater spacing may be needed for hazardous processes. The location of the principal ancillary
buildings should then be decided. They should be arranged so as to minimize the time spent
by personnel in traveling between buildings. Administration offices and laboratories, in
which a relatively large number of people will be working, should be located well away from
potentially hazardous processes. Control rooms will normally be located adjacent to the
processing units, but with potentially hazardous processes may have to be sited at a safer
distance. The siting of the main process units will determine the layout of the plant roads,
95
pipe alleys and drains.
96
Access roads will be needed to each building for construction, and for operation and
maintenance. Utility buildings should be sited to give the most economical run of pipes to
and from the process units. Cooling towers should be sited so that under the prevailing wind
the plume of condensate spray drifts away from the plant area and adjacent properties. The
main storage area should be placed between the loading and unloading facilities and the
process units they serve. Storage tanks containing hazardous materials should be sited at least
70 m (200 ft.) from the site boundary.
Plant Layout :
The economic construction and efficient operation of the process unit will depend on how
well the plant and equipment specified on the process flow-sheet is laid out. The principal
factors to be considered are:
1. Economic considerations: construction and operating costs.
2. The process requirements.
3. Convenience of operation.
4. Convenience of maintenance
5. Safety.
6. Future expansion.
7. Modular construction.
These principles are detailed below.
1. Costs
The cost of construction can be minimized by adopting a layout that gives the shortest
run of connecting pipe between equipment, and the least amount of structural steel work.
However, this will not necessarily be the best arrangement for operation and maintenance.
2. Process requirements
An example of the need to take into account process considerations is the need to elevate
the base of columns to provide the necessary net positive head to a pump or the operating
head for a thermo syphon reboiler.
97
3. Operation
Equipment that needs to have frequent operator attention should be located convenient to
the control room. Valves, sample points and instruments should be located at convenient
positions and heights. Sufficient working space and headroom must be provided to allow easy
access to equipment.
4. Maintenance
Heat exchangers need to be sited so that the tube bundles can be easily withdrawn for
cleaning and tube replacement. Vessels that require frequent replacement of catalyst or
packing should be located on the outside of buildings. Equipment that requires dismantling
for maintenance, such as compressors and large pumps, should be placed under cover.
5. Safety
Blast walls may be needed to isolate potentially hazardous equipment, and confine the
effects of an explosion. At least two escape routes for operators must be provided from
each level in process buildings.
6. Plant expansion
Equipment should be located so that it can be conveniently tied in with any future
expansion of the process. Space should be left on pipe alleys for future needs, and service
pipes over- sized to allow for future requirements.
7. Modular construction
In recent years, there has been a move to assemble sections of plant at the plant
manufacturer’s site. These modules will include the equipment, structural steel, piping and
instrumentation. The modules are then transported to the plant site, by road or sea.
The advantages of modular construction are:
1. Improved quality control.
2. Reduced construction cost.
3. Less need for skilled labour on site.
4. Less need for skilled personnel on overseas sites.
98
Some of the disadvantages are:
1. Higher design costs.
2. More structural steel work.
3. More flanged connections.
4. Possible problems with assembly, on site.
99
CHAPTER 11 : COST ESTIMATION
An estimate of the capital investment for a process may vary from a predesign estimate based
on little information except the size of the proposed project to a detailed estimate prepared
from complete drawings and specifications. Between these two extremes of capital-
investment estimates, there can be numerous other estimates which vary in accuracy
depending upon the stage of development of the project. These estimates are called by a
variety of names, but the following five categories represent the accuracy range and
designation normally used for design purposes:
1. Order-of-magnitude estimate (ratio estimate) based on similar previous cost data;

probable accuracy of estimate over + 30 percent.
2. Study estimate (factored estimate) based on knowledge of major items of equipment;

probable accuracy of estimate up to 30 percent.
3. Preliminary estimate (budget authorization estimate; scope estimate) based on sufficient

data to permit the estimate to be budgeted; probable accuracy of estimate within +20 percent.
4. Definitive estimate (project control estimate) based on almost complete data but before
completion of drawings and specifications; probable accuracy of estimate within f 10 percent.
5. Detailed estimate (contractor’s estimate) based on complete engineering drawings,

specifications, and site surveys; probable accuracy of estimate within +5 percent.
As we are on the initial stages of design we can use first two techniques; however for study
estimate we will be requiring the capacity of each equipment which is possible only after
designing every equipment so we shall be using Order of magnitude here.
10
For the year 2001, THF plant of capacity Q1=136.035 TPD had total capital cost,
C1 = ₹ 195,60,32,046
Our plant capacity = 120 TPD = 39600 tons/year (Assuming 330 working days of the
plant)
C2 = C1 × (Q2/Q1) n
Where C2 = cost of our plant in 2001 with 136.035 TPD capacity,
N = 0.6
Given capacity, Q2 =120 TPD
C2 = 195,60,32,046 × (120/136.035)0.6
= ₹ 181,42,38,240
CEPCI = Chemical Engineering Plant Cost Index
Cost index in the year 2001 (CEPCI) = 397
Cost index is the year 2018 (CEPCI) = 564.8
n = fixed capital investment
Fixed Capital Investment (FCI) required:
n2 = n1 × (CI2018/CI2001)
= 181,42,38,240 × (557/389.9)
= ₹ 259,29,38,222
Thus, fixed capital investment for 120 TPD capacity is ₹ 259,29,38,222
10
(The data for range of all costs calculated below, is taken from Book ‘ Plant design &
economics’ by Peters and Timmerhaus)
7.1 Estimation of total capital investment:
I. Direct cost:
A. Equipment, installation, piping etc.
1. Purchased equipment (15-40 % of Fixed-capital investment)
Assuming 20% of fixed capital investment
= 0.2 × 259,29,38,222
= ₹ 51,85,87,644.4
2. Installation, including insulation and painting (6-14 % of fixed capital investment)
= 0.1 × 259,29,38,222
= ₹ 25,92,93,822.2
3. Instrumentation and controls, installed (2-8% of fixed capital
investment) Assuming 6% of fixed capital investment
= 0.06 × 259,29,38,222
= ₹ 15,55,76,293.3
4. Piping, installed (3-20% of fixed capital investment)
= 0.05 × 259,29,38,222
= ₹ 12,96,46,911.1
10
5. Electrical, installed (2-10% of fixed capital investment)
= 0.05 × 259,29,38,222
= ₹ 12,96,46,911.1
6. Buildings (3-18% of fixed capital investment)
= 0.1 × 259,29,38,222
= ₹ 259,29,38,222
7. Service facilities and yard improvements: (8-20% of fixed capital investment)
= 0.18 × 259,29,38,222
= ₹ 46,67,28,880
8. Land (1-3% of fixed capital
investment) Assuming 1% of fixed capital
investment
= 0.01 × 259,29,38,222
= ₹ 2,59,29,382.22
Direct cost = ₹ 194,47,03,667 (75% of FCI adding all)
II. Indirect cost
1. Engineering and supervision (4-21% of fixed capital investment)
= 0.06 × 259,29,38,222
= ₹ 15,55,76,293.3
10
2. Construction expense (4-16% of fixed capital investment)
= 0.12 × 259,29,38,222
= ₹ 31,11,52,586.6
3. Contractor’s fee (2-6% of fixed capital
investment
= 0.04 × 259,29,38,222
= ₹ 10,37,17,528.9
4. Contingency (5-15% of fixed capital
investment
= 0.06 × 259,29,38,222
= ₹ 15,55,76,293.3
Indirect cost = ₹ 64,82,34,555 (25% of FCI adding all above four)
To find the Working Capital, we will use Lang Multiplication Factor of Fluid-Fluid type
Industry.
For fluid-fluid processing plant, FCI:TCI=4.8:5.7
Thus, TCI = 2592938222 × (5.7/4.8)
TCI = ₹ 307,91,14,139
Total capital investment (TCI) = fixed capital investment + working capital
307,91,14,139 = 259,29,38,222 + working capital
Working Capital = ₹ 48,61,75,917
10
7.2 Estimation of total product cost:
I. Manufacturing cost
A. Fixed charges:
1. Depreciation (depends on life period, salvage value, and method of calculation- about 10%
of Fixed-capital investment for machinery and equipment and 2-3% of building value for
buildings)
The assumed value is (13% of fixed capital investment + 3% of building value found in direct
costs)
= 0.13 × 259,29,38,222 + 0.03 × 25,92,93,822.2
= ₹ 34,48,60,783.5
2. Local taxes (1-4% of fixed capital
investment
= 0.03 × 259,29,38,222
= ₹ 7,77,88,146.67
3. Insurance (0.4-1% of fixed capital
investment) Assuming 0.8% of fixed capital
investment
= 0.008 × 259,29,38,222
= ₹ 1,81,50,567.55
Therefore, Fixed charges = ₹ 44,07,99,497.7 (adding above
three) The fixed charge is 10-20% of total product cost
Assuming 15% of total product cost
Total product cost = 44,07,99,497.7/0.15
=₹ 293,86,63,318
10
B. Direct Production Cost:
1. Raw materials (10-50% of total product
cost) Assuming 25% of total product cost
= 0.25 × 293,86,63,318
= ₹ 73,46,65,829.5
2. Operating labor (10-20% of total product
cost) Assuming 11% of total product cost
= 0.11 × 293,86,63,318
= ₹ 35,26,39,598.2
3. Direct supervisory and clerical labor (10-25% of operating labor)
Assuming 15% of operating labor cost
= 0.15 × 35,26,39,598.2
= ₹ 4,23,16,751.8
4. Utilities (10-20% of total product
cost) Assuming 12% of total product
cost
= 0.12 × 293,86,63,318
= ₹ 35,26,39,598.2
5 .Maintenance and repairs (2-10% of fixed capital investment)
= 0.05 × 259,29,38,222
= ₹ 12,96,46,911.1
10
6. Operating supplies (10-20% cost of maintenance and
repairs) Assuming 15% of maintenance and repairs
= 0.15 × 12,96,46,911.1
= ₹ 1,94,47,036.67
7. Laboratory charges (10-20% of operating
labor) Assuming 15% of operating labor
= 0.15 × 1,94,47,036.67
= ₹ 5,28,95,939.73
8. Patents and royalties (0-6% of total product cost)
Assuming 0.4% of total product cost
= 0.004 × 293,86,63,318
= ₹ 1,17,54,653.27
C. Plant Overhead Costs :
(50-70% of cost for labor, supervision and maintenance, or 5-15% of total product cost);
includes costs for the following: general plant upkeep and overhead, payroll overhead,
packaging, salvage, laboratories and storage facilities)
Assuming Plant overhead cost as 60% of OL, DS & CL and M&R
= 0.6 × [35,26,39,598.2+4,23,16,751.78+12,96,46,911.1]
= ₹ 31,47,61,956.6
I. Manufacturing cost = Fixed charges + direct production cost + plant overhead cost
= ₹ 369,42,24,772
10
II. General Expenses = Administrative costs + Distribution costs + Research and
development costs
A. Administrative costs (2-6% of total product cost)
= 0.05 × 293,86,63,318
= ₹ 14,69,33,165.9
B. Distribution and selling costs (2-20% of total product cost)
= 0.15 × 293,86,63,318
= ₹ 44,07,99,497.7
C. Research and development costs (about 5% of total product cost)
= 0.05 × 293,86,63,318
= ₹ 14,69,33,165.9
D. Financing (0-10% of total capital
investment) Assuming 5% of total product cost
= 0.05 × 307,91,14,139
= ₹ 15,39,55,707
General expenses = ₹ 580710122.2 (totaling all above
four) Total product cost = manufacturing cost + general
expenses
= 369,42,24,772 + 58,07,10,122.6
= ₹ 351,93,73,441
Cost of the product = Total product cost/ our plant capacity in kg
= (351,93,73,441)/(3,96,00,000)
≈ ₹ 88.873 per kg
10
We will sell the product at a price of 112 per kg which is not only less than our global
competitors but also with a profit percentage of just above 26%.
Turnover = ₹ 112 per kg × 39600 × 103
kg Turnover = ₹ 443,52,00,000
Gross annual earning (GAE) = 443,52,00,000-351,93,73,441
GAE = ₹ 91,58,26,559
Sr. No. Taxable Income Tax Rate Tax value

1 Gross Income 30% 27,47,47,967
2 Surge charge tax 12% 3,29,69,756.12
3 Education cess 2% 54,94,959.4
4 Secondary and Higher Secondary Cess 1% 2,77,479.68
Net annual earnings = GAE – Total tax
Net annual earnings = 91,58,26,559-31,59,60,163
Net annual earnings = ₹ 59,98,66,396
Fixed capital investment

Payback period = Avg. annual profit + Annual depreciation
259,29,38,222
= 59,98,66,396+34,48,60,783
= 2.7446 year
Rate of return = (net annual earnings) / (fixed capital investment)
= 59,98,66,396 / 307,91,14,139
≈ 0.19481
Rate of return is about 19.481%
10
Turnover
FCI
Turnover Ratio
=
443,52,00,000
= 259,29,38,222
= 1.7105
Breakeven Analysis:
Production cost = ₹
293,86,63,318 Fixed cost = ₹
44,07,99,497.7 Turnover = ₹
443,52,00,000 Selling price per kg
THF = ₹ 112
293,86,63,318
396,00,000
Direct production cost per kg =
= ₹ 74.209
Let NBP be the breakeven point.
112× NBP = 74.209×NBP + 44,07,99,497.7
NBP = 35.345 tons per day
11
CHAPTER 12 : SAFETY ISSUED ADAPTED
THF is a colourless liquid, highly flammable liquid with an ether like odor that can be
detected as low as 4 ppm (odor threshold). It is a polar solvent and can dissolve a wide range
of nonpolar and polar chemical compounds.
12.1 Potential Hazards
 THF is a highly flammable, Its vapor can travel a significant distance through the air
to an ignition source and flash back.
 A 5% solution of THF in water is flammable. THF vapors may form explosive air
mixtures at concentrations of 2-12% by volume.
 THF reacts violently with strong oxidizers.
 THF is a severe eye irritant and skin irritant. Prolonged or repeated eye exposure may
cause conjunctivitis, prolonged skin contact can cause defatting.
 When THF is exposed to air, it forms explosive peroxides if concentrated by
distillation or evaporation.
Occupational Exposure Limits (OELs)
MISOSHA ( Michigan Occupational Safety and Health Administration ) :
200 ppm, 8 hrs
12.2 Work Practice Controls
 THF is kept in a closed container when not is use to minimize creation of flammable
vapor concentrations.
 Ignition sources such as open flames, hot surfaces, steam baths and operation of
mechanical and electrical equipment that is not intrinsically safe, are eliminated.
 Recommended gloves include Polyvinyl alcohol (PVA), Teflon. Butyl or natural
rubber offer short term protection and should be removed and discarded when
material is spilled on them.
 THF permeates standard nitrile laboratory gloves in less than one minute and
neoprene or latex in less than 2 minutes, thus task should be planned to minimize
glove contact with THF. If gloves become contaminated, gloves are changed and
hands are washed immediately to avoid skin exposure.
11
12.3 Transportation and Storage
 THF is transported in secondary containment, preferably a polyethylene or other non-

reactive acid or solvent bottle carrier.
 THF is stored with inhibitors.
 THF must be stored in an air-impermeable container and placed in a dark area to
prevent further promotion of the peroxide forming reaction.
 Suitable fire control devices such as fire extinguishers must be available at locations
where flammable or combustible liquid are stored.
 THF is stored protected from moisture.
 Containers should be dated when opened and tested periodically for the presence of
peroxides.
12.4 Spill Procedure
 When a spill occurs, personal safety should always come first.

 Alert and clear everyone in the immediate area where the spill occurred.
 Use the personal protective equipment.
 Since THF is a peroxide forming material, do not allow clean-up materials to dry, seal
them inside a compatible container.
 Turn off ignition and heat sources. Don’t light Bunsen burners or turn on other
switches.
 Open outside windows if possible.
 Do not attempt to clean up a tetrahydrofuran spill that occurs outside a fume hood, or
a major spill.
11
CHAPTER 13 : ENVIRONMENTAL ISSUES
Environmental issues in India are many. Air pollution, water pollution, garbage pollution and
wildlife natural habitat pollution challenge India. The situation was worse between 1947
through 1995. According to data collection and environment assessment studies of World
Bank experts, between 1995 through 2010, India has made one of the fastest progress in the
world, in addressing its environmental issues and improving its environmental quality. Still,
India has a long way to go to reach environmental quality similar to those enjoyed in
developed economics. Pollution remains a major challenge and opportunity for India.
Waste generated from industries is serious threat to environment. The environmental pollutions
(through under permitted levels) caused by the industry is:
 Air Pollution :
 Low emission of Gases like
 Other Volatile Organic Compounds Escape into the environment while
material handling and thereby cause pollution.
 Water Pollution :
Contaminated water originates from-
1. Process condensate
2. Closed-loop cooling tower blow down.
3. Closed-loop boiler blow down Main
4. By product water from the reactor.
The industry therefore mainly causes water pollution, However there is a set up of waste
water treatment plant in the plant according to the norms and rules of the authorities
industrial society or corporation.
Therefore the setup of Effluent Treatment Plant (ETP) is a must before the water is sent off
for disposal.
11
EFFLUENT TREATMENT PLANT :
The effluent treatment plant therefore treats the acidic water before disposal. The process of
treatment is as follows :
1. Oil and Grease Settling :

Initially the mother liquor i.e. the initial effluent from industry is allowed to settle in
the three oil and grease settling tanks. After the entire oil and grease is settled and
effluent water is separated on the basis of density difference; this liquid is then sent to
effluent collection tank. Here the effluent is collected from settling tanks and stored
for
11
further treatment.
2. Neutralization :
From the effluent collection tank the effluent is sent to neutralization tank where the
effluent is neutralized with the help of calcium carbonate and lime. (Ca(OH) 2). Soda
ash can also be used but it is very costly. After neutralization of acidic water effluent
the pH should be 7, water should become neutral.
3. Filtration and removal of solids :

Filtration is carried out by press filter removing all the solids material. The sludge
which is a powder is then sent to sludge collection tanks and the finally disposed off
at proper place and the treated water is stored in a tank which is sent to the tankers
which transport water for treatment by government agencies in industrial zone before
final disposal.
11
APPENDIX
I:
MALEIC
ACID
11
APPENDIX
II :
HYDROGEN
11
APPENDIX
III :
TETRAHYDROFURAN
11
REFERENCES :
1) European patent application. Publication number: 0322140
2) New Process for Production of Tetrahydrofuran Junichi Kanepaka, Taisuke Asano,

Shinobu Masamune.
3) NPTEL Module:7, Lecture:38
4) Kirk-Othmer Encyclopaedia of Chemical Technology.
5) United States Patent, Patent Number: 4810807
6)https://webbook.nist.gov/cgi/cbook.cgi?ID=C513859&Mask=4&Type=ANTOINE&Plot=o
n
7) http://www.ddbst.com/en/EED/PCP/HCP_C159.php
8) http://homepages.ed.ac.uk/jwp/Chemeng/Chemeng/azeotrope_bank.html
9) http://www.ddbst.com/en/EED/VLE/VLE%20Tetrahydrofuran%3BWater.php
10)https://webbook.nist.gov/cgi/cbook.cgi?ID=C109999&Mask=4&Type=ANTOINE&Plot=
on#ANTOINE
11) Separation of tetrahydrofuran and water using pressure swing distillation. Korean J.
Chem. Eng., 28(2), 591-596 (2011) DOI: 10.1007/s11814-010-0467-1
12)http://www.chemengonline.com/maleic-anhydride-n-butane-fixed-bed-process-intratec-
solutions/
13)http://www.technobell.eu/chemical-process-technologies/maleic-anhydride/
14) https://www.transparencymarketresearch.com/tetrahydrofuran-market.html
15) https://ihsmarkit.com/products/tetrahydrofuran-chemical-economics-handbook.html
16) Handbook of Thermodynamic Diagram Volume 1 Organic Compound C1to C4by Carl L
Yaws
17) MV Joshi, V.V. Mahajani, Process Equipment Design 3rd Edition
11
18) Coulson and Richardson’s Chemical Engineering Volume 6, 4rth Edition ( Page Number
634-675)
19) Max S. Peters, Klaus D. Timmerhaus, Plant Design and Economics for
Chemical Engineers, 4rth Edition
20) www.engineeringtoolbox.com
21) http://terpconnect.umd.edu/~choi/MSDS/Airgas/HYDROGEN.pdf
22) https://www.cdhfinechemical.com/images/product/msds/18_776366528_MaleicAcid-
CASNO-110-16-7-MSDS.pdf
23)https://www.cdhfinechemical.com/images/product/msds/123_86293100_Tetrahydrofuran-
CASNO-109-99-9-MSDS.pdf
12

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A

Dr. SANJAY R. PATEL

Sardar Vallabhbhai National Institute Of Technology

Dept. Of Chemical Engineering

Examiner signature with date

AMEY KALBHOR (U15CH002) and PRASIL KAPADIYA(U15CH003), registered in

The Project preliminary report entitled “Production of TETRAHYDROFURAN” is

Dr. Sanjay R. Patel

I express my sincere thanks to Dr. Mausumi Mukhopadhyay, Head of Department of

1.1 PROPERTIES [3]

Molecular Formula C4H8O

Molecular Weight 72.11 gm/mole

Appearance Colourless Liquid

Melting Point -108.4 oC

Vapor Pressure 190.7 kPa at 20 oC

Flash Point -14 oC

Density 0.889 gm/cm3 at 20 oC

Upper Explosive Limits 11.8 %

Solubility Miscible with water

Tetrahydrofuran (THF) has many industrial applications as a solvent, reaction medium, or

Figure 2.1 : World Consumption Of THF [15]

Figure 2.2 : Import Data of THF[15]

Figure 2.3 : Import Volume and Value data for THF[16]

Table 2.1 : Import Data for THF [16]

Date Origin Port of Unit Quantity Value Per Unit

Nov 22, Malaysia Nhava KGS 14,400 1,661,565 115

Nov 22, Germany Vizac Sea KGS 28,800 3,374,209 117

Nov 22, Malaysia Vizac Sea KGS 14,400 1,651,733 115

Nov 21, Taiwan Chennai KGS 19,550 2,031,249 104

Nov 21, Malaysia Nhava KGS 14,400 1,724,884 120

Nov 19, Malaysia Nhava KGS 2,492 287,525 115

Nov 19, Malaysia Nhava KGS 14,400 1,661,565 115

Nov 19, Malaysia Nhava KGS 14,400 1,661,565 115

Nov 19, Malaysia Nhava KGS 14,400 1,374,039 115

Nov 19, Malaysia Nhava KGS 14,400 1,661,565 115

Nov 19, Malaysia Chennai KGS 11,908 1,661,565 115

Nov 18, Taiwan Nhava KGS 14,400 1,494,425 104

Nov 18, Malaysia Nhava KGS 14,400 1,265,038 116

Nov 18, Malaysia Nhava KGS 10,899 406,358 116

Nov 18, Malaysia Chennai KGS 3,501 1,622,238 113

Nov 17, Malaysia Vizac Sea KGS 14,400 1,611,213 112

Nov 12, Malaysia Nhava KGS 14,400 1,661,565 115

Nov 11, Taiwan Chennai KGS 19,580 2,034,157 104

Nov 10, Germany Chennai KGS 14,400 1,523,920 106

3.1 Available Processes

3.1.1 By Acetoxylation of Butadiene

3.1.2 From propylene oxide

3.1.3 From Acetylene and Formaldehyde

3.1.4 By Hydrogenation of Maleic Acid

3.2 Process Selection

Process Acetoxylation From From Hydrogenation

Raw 1. Butadiene 1. Propylene 1. Acetylene 1. Maleic

Materials 2. Acetic Oxide Gas Acid

Catalyst - Tri-Lithium - Palladium-rhenium

Operating 70 oC 250-300 oC 100 oC 250 oC

Operating 70 atm 9.89 atm 5 atm 7 atm

Units 2. Reactor tion 2. Hydrogen Reactor

Products THF THF THF THF

By Products : By Products : By Products : By Products :

1. Acetic 1. Water 1. Water 1. Water

542.62 + 4457.832 + (A0.907) = (B 0.9514) + 0