Plant and Design Project Level 4

BTEN 3292 PROCESS PLANT DESIGN AND SAFETY
Process Design Development
Level 4 Decision
(Recycle Structure of the Flowsheet)
1
Hierarchy of decisions
0 Input Information
1 Batch versus Continuous
2 Input- Output Structure
3 Recycle structure of the Flowsheet
4 Separation System
5 Heat Exchanger Network
2
Hierarchy of Decisions
1. Batch versus continuous
2. Input-output structure of the flowsheet
3. Recycle structure of the flowsheet
4. General structure of the separation system
a. Vapor recovery system
b. Liquid recovery system
5. Heat-exchanger network
3
Level 4: General structure of the separation system
LEVEL 3
purge
feeds reactor separator products
Liquid ?
Liquid / Vapor ?
Vapor ?
4
1 ) Liquid
LEVEL 3
liquid liquid
feeds reactor separation products
system
Liquid recycle
Liquid separation system: Colum, extraction, azeotropic

distillation etc.
5
2 ) Liquid / Vapor purge
vapor Vapor
gas recycle Recovery
35C system
vapor
Phase
Split liq.
liq.
liquid liquid
system
Liq. recycle
LEVEL 3
Two phase: use reactor as a phase splitter or cool down to 35oC 6

purge
3 ) Vapor
gas recycle
Heuristic: vapor Vapor
phase split is cheap Recovery
35C system
Phase
Split liquid
liquid
vapor
liquid
system
Liquid recycle
Steps: 1. Cool down to 35C
2. A. phase split exists == Step 3 LEVEL 3
B. no phase split
i. Pressurize
ii. refrigerated partial condenser
iii. to vapor recovery system
7
3. Design vapor recovery system and liquid separation systems.
LOCATIONS OF VAPOR RECOVERY SYSTEM
Gas Purge
2 1
Recycle
vapor from phase split
• Location 1: The purge stream - If significant amount of valuable materials are

being lost in the purge.
• Location 2: The gas-recycle stream - If materials are deleterious to the reactor
operation.
• Location 3: The flash vapor stream - Both factors are valid.
8
• None - Both factors do not exist
TYPE OF VAPOR RECOVERY SYSTEM
1 ) Condensation - low. T and/or high P
2 ) Absorption
3 ) Adsorption
4 ) Membrane separation
5 ) Reaction
ADJUST MATERIAL BALANCE ?
9
DECISION IN SYNTHESIZING LIQUID SEPARATION SYSTEM

1. How should light ends be removed, if they might contaminate
the product ?
2. What should be the destination of light end ?
3. Do we recycle components that form azeotropes with reactants,
or do we split the azeotropes ?
4. What separations can be made by distillation ?
5. What sequence of columns do we use ?
6. How should we accomplish separations if distillation is not
feasible ?
10
1 ) ALTERNATIVES FOR LIGHT-ENDS REMOVAL

 Phase Splitter — T or P and remove LE in phase splitter
Lower
cost  Partial Condenser on Product Column
 Pasteurization Section on Product Column
Higher
cost  a Stabilizer Column before the Product Column
lights
lights lights
product
product
Product
Partial condenser Pasteurization Section Stabilizer Column
11
1 ) ALTERNATIVES FOR LIGHT-ENDS REMOVAL (cont.)

• Pasteurization Columns:
For the special case of side-stream columns where the desired
product is the intermediate boiler and there is a waste or fuel
byproduct that is ether much lighter than product (so we recover
the product as a side stream above the feed) or else is much
heavier than the product (so we recover the product as a side
stream below the feed).
K. Glinos and M. F. Malone have published a shortcut design

procedure for pasteurization columns. (see Appendix A.5).
• Stabilizer Columns:
This is a normal distillation column that recovers light ends
12
2 ) DESTINATION OF LIGHT ENDS

a ) vent or flare stacks - if light ends have very little value.
b ) fuel - if light ends are flammable.
c ) vapor recovery system - if light ends are valuable.
3 ) AZEOTROPES WITH REACTANTS

- recycle the azeotropes
- oversize equipment
- split the azeotrope (need two columns for a binary azeotrope)
- Needs two columns and therefore is expensive
- There is no general heuristic available for making this decision

and so we usually need to evaluate both alternatives.
13
4 ) APPLICABILITY OF DISTILLATION
Why
- handle wide range of throughput
- handle wide range of feed composition
- ability to produce high purity product
Cases not suited
- relative volatility < 1.1
(column can become very expensive)
- low molecular weight
- high molecular weight heat sensitive materials
14
5 ) SEQUENCING OF SIMPLE COLUMNS
15
5 ) SEQUENCING OF SIMPLE COLUMNS (cont.)

For sharp splits of a three component mixture (with no
azeotropes) we can use:
a) Direct sequence
b) Indirect sequence A
A B
C C B
Design 1 : Direct Sequence Design 2 : Indirect Sequence 16
• General Heuristics for Column Sequencing

1. Remove corrosive components as soon as possible.
2. Remove reactive components such as monomers as soon as
possible.
3. Remove products as distillates.
4. Remove recycle streams as distillates, particularly if they are
recycled to a packed bed reactor
• Column Sequencing Heuristics for Simple Columns

Simple Columns: columns with one top an d one bottom stream.
1. Most plentiful first.
2. Lightest first.
3. High recovery separation last.
4. Difficult separation last.
5. Favor equimolar split.
6. Next separation should be cheapest.
17
6 ) COMPLEX COLUMNS
A B A
C C B
Design 1 : Direct Sequence Design 2 : Indirect Sequence
18
6 ) COMPLEX COLUMNS (cont.) A

A B
C C B
Design 3 : Side-stream rectifier Design 4 : Side-stream Stripper
A
A, A A
B
B
B
B
B, C C
C C Design 6 Design 7 19
Design 5 : Prefractionator arrangement side stream
Other types of liquid separations

If distillation is too expensive to use to separate liquid mixtures,
that is , α <1.1, the other choices that are normally the next least
expensive can be used are as follow:
1. Extraction
2. Extractive distillation
3. Azeotropic distillation
4. Reactive distillation
5. Crystallization
6. Adsorption
7. Reaction
20
Extraction
21
Azeotropic Distillation
Occasionally, you will confront mixtures which are hard to separate due to very close
relative volatility or due to formation of azeotrope. A slightly different configuration of
distillation column is required.
i. Use of two columns with different

operational pressure pure A
P1
pure B
P2
maximum boiling
azeotrope
P1
Temp.
P2
B A
Azeotropic Distillation
ii. Use of entrainer which forms binary or ternary azeotrope with the top product
components but upon condensation, forms a two phase liquid layer which can be
separated in the decanter.
B = Ethanol
C = Water
S = Benzene - relatively light component that changes the vapor-liquid equilibrium
23
Extractive Distillation
iii. Use of solvent to break the azeotrope by increasing the relative volatility
between the component to be separated.
B = HNO3
C = H2 O
S = H2SO4 (heavy component) - changes the vapor-liquid equilibrium which is in some
cases will simplify the separation.
(pure)
Recycle extractive entrainer (H2SO4) 24

Reactive Distillation
• Addition of an entrainer that reacts with one component in a mixture that is difficult to
separate.
• Example - the relative volatility between meta and para-xylene is only 1.03 . However, if
sodium cumene is added to a mixture of the xylene isomers, it reacts with the para
isomer, and then the relative volatility between the meta-xylene and the organometallic
complex that is produced becomes 30.
• The reaction can be reversed in a second column and the entrainer is recycled
25
Crystallization
• The separation of xylene isomers is difficult by distillation

• often it is cheaper to use the difference in freezing points to separate
the mixture.
• By freezing, separation of the liquid-solid mixture, and often using
some recycle, the desired separation can be achieved
26
HDA Process
The flows of flash liquid stream that is fed to the distillation train is given in
Table (100 °F and 465 Psia). If we let the light ends leave with the product and
recover all the product, the composition of the product stream will be:
Less than the required product purity

of 0.997 - must remove the light ends
27
Purge
Compressor
H2, CH4
Reactor Flash
Toluene
Benzene H2, CH4
Stablizer
Product
Recycle
Diphenyl
28
29
Level 4: General structure of the separation system (Homogeneous Fluid Mixtures – Other Methods)
2. ABSORPTION
In the absorbtion process, solvent is used to dissolves certain preferential component termed as
the solute, which normally appears as minor component. The mixture of solvent and solute is
then separated in the stripping process to recover the solvent.
The amount of solvent
Absorber Stripper used have an impact on:
product free of
solute
I. The separation
High P Low P
Why? capability
Low T High T ii. The amount of
solute
P1
energy required to
i. Decide by the equilibrium property recover the solvent
between the solvent and the system
which gives the best extraction performance.
ii. Decide by the condition of which the solvent P2
can be vaporised and condensed to recover it. solvent + B
Some quick guideline based

on past operational experience
Absorption Factor for component i (L/VKi)
is within the range of 1.2 - 2.0. solvent Temp.
Stripping Factor for component i (VKi/L)
is within the range of 1.2 - 2.0. The typical value
is about 1.4
EVAPORATORS COST Capital
Similar to distillation, only uses

heat for separation of material.
TOTAL
4 different arrangement ;
1. Forward feed operation

2. Backward feed operation
Energy
3. Parallel feed operation
4. Mixed feed operation
optimum
area of
AREA OF
What about other parameters ? evaporator EVAPORATOR UNIT
Pressure/Temperature; For a single evaporator !

Decide by vaporisation ability at the given
temperature of the heating media.
No. of Evaporator Unit

Decide by amount of feed material
and the area requirement of the evaporator.
Difficult to decide !
COST
Capital
TOTAL
Remember
Q = UADT
Energy
optimum AREA OF
area of EVAPORATOR
evaporator UNIT
T T T
2 evaporator H
3 evaporator
Questions. 4 evaporator
What can you say the relation between No. of evaporator unit and the two cost components ?
Do you expect the overall cost curve to be smooth ?
LIQUID–LIQUID EXTRACTION
• Like gas absorption, liquid–liquid extraction separates a homogeneous mixture by
the addition of another phase – in this case, an immiscible liquid.
• Liquid–liquid extraction carries out separation by contacting a liquid feed with
another immiscible liquid.
• The equipment used for liquid–liquid extraction is the same as that used for the
liquid–liquid reactions
33
ADSORPTION
34
MEMBRANES
35
Level 4: General structure of the separation system (Heterogeneous Fluid Mixtures – Other Methods)
Principal methods for the separation of heterogeneous

mixtures are
• Settling and sedimentation

• Inertial and centrifugal separation
• Electrostatic precipitation
• Filtration
• Scrubbing
• Flotation
• Drying.
36
SETTLING AND SEDIMENTATION

• Particles are separated from a fluid by gravitational forces acting on the particles.
• The particles can be liquid drops or solid particles. The fluid can be a gas, vapor or
liquid.
37
SETTLING AND SEDIMENTATION (cont.)
38
INERTIAL AND CENTRIFUGAL SEPARATION

• Sometimes gravity separation may be too slow because of the closeness of
the densities of the particles and the fluid, because of small particle size
leading to low settling velocity or, in the case of liquid–liquid separations,
because of the formation of a stable emulsion
• Inertial or momentum separators improve the efficiency of gas–solid settling
devices by giving the particles downward momentum, in addition to the
gravitational force
39
INERTIAL AND CENTRIFUGAL SEPARATION (cont.)

• Centrifugal separators take the idea of an inertial separator a step further and
make use of the principle that an object whirled about an axis at a constant
radial distance
from the point is acted on by a force.
• Use of centrifugal forces increases the force acting on the particles.
• Particles that do not settle readily in gravity settlers often can be separated
from fluids by centrifugal force.
• The simplest type of centrifugal device is the cyclone separator for the
separation of solid particles or liquid droplets from a gas or vapor (Figure 8.6).
This consists of
a vertical cylinder with a conical bottom.
• Centrifugal force is generated by the motion of the fluid. The mixture enters
through a tangential inlet near the top, and the rotating motion so created
develops centrifugal force that throws the dense particles radially toward the
wall. The entering
fluid flows downward in a spiral adjacent to the wall. When the fluid reaches
the bottom of the cone, it spirals upward in
40
INERTIAL AND CENTRIFUGAL SEPARATION (cont.)
41
ELECTROSTATIC PRECIPITATION
• Electrostatic precipitators are generally used to separate particulate matter
that is easily ionized from a gas stream
• This is accomplished by an electrostatic field produced between wires or grids
and collection plates by applying a high voltage between the two, as
illustrated in Figure 8.9
42
FILTRATION
• In filtration, suspended solid particles in a gas, vapor or liquid are removed
by passing the mixture through a porous medium that retains the particles
and passes the fluid (filtrate).
• The solid can be retained on the surface of the filter medium, which is cake
filtration, or captured within the filter medium, which is depth filtration.
The filter medium can be arranged in many ways.
43
SCRUBBING
Scrubbing with liquid (usually water) can enhance the collection of particles when
separating gas–solid mixtures
44
FLOTATION
• Gravity separation process that exploits the differences in the surface properties of particles.
• Gas bubbles are generated in a liquid and become attached to solid particles or immiscible
liquid droplets, causing the particles or droplets to rise to the surface.
• Used to separate mixtures of solid–solid particles after dispersion in a liquid, or solid
particles already dispersed in a liquid or liquid–liquid mixtures of finely divided immiscible
droplets.
• The liquid used is normally water and the particles of solid or immiscible liquid will attach
themselves to the gas bubbles if they are hydrophobic (e.g. oil droplets dispersed in water).
45
DRYING
• Removal of water from a substance through a whole range of processes,
including distillation, evaporation and even physical separations such as
centrifuges.
• Here, consideration is restricted to the removal of moisture from solids into a
gas stream (usually air) by heat, namely, thermal drying.
• Four of the more common types of thermal dryers used in the process
industries.
1. Tunnel dryers - Wet material on trays or a conveyor belt is passed through
a tunnel, and drying takes place by hot air. The airflow can be countercurrent,
cocurrent or a mixture of both. This method is usually used when the product
is not free flowing
46
2. Rotary dryers – a cylindrical shell mounted at a small angle to the horizontal is rotated at
low speed. Wet material is fed at the higher end and flows under gravity. Drying takes place
from a flow of air, which can be countercurrent or cocurrent. The heating may be direct to
the dryer gas or indirect through the dryer shell. This method is usually used when the
material is free flowing. Rotary dryers are not well suited to materials that are particularly
heat sensitive because of the long residence time in the dryer.
3. Drum dryers - consists of a heated metal roll. As the roll rotates, a layer of liquid or slurry
is dried. The final dry solid is scraped off the roll. The product comes off in flaked form.
Drum dryers are suitable for handling slurries or pastes of solids in fine suspension and are
limited to low and moderate throughput
47
4. Spray dryers - a liquid or slurry solution is sprayed as fine droplets into a hot gas
stream. The feed to the dryer must be pumpable to obtain the high pressures
required by the atomizer.The product tends to be light, porous particles. An
important advantage of the spray dryer is that the product is exposed to the hot gas
for a short period. Also, the evaporation of the liquid from the spray keeps
the product temperature low, even in the presence of hot gases. Spray dryers are
thus particularly suited to products that are sensitive to thermal decomposition,
such as food products.
48
Generalized block diagram of downstream processing
49
Semester 2 2015/16

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BTEN 3292 PROCESS PLANT DESIGN AND SAFETY

Process Design Development

1 Batch versus Continuous

2 Input- Output Structure

3 Recycle structure of the Flowsheet

5 Heat Exchanger Network

Level 4: General structure of the separation system

feeds reactor separator products

Level 4: General structure of the separation system

Liquid separation system: Colum, extraction, azeotropic

Level 4: General structure of the separation system

2 ) Liquid / Vapor purge

Level 4: General structure of the separation system

Level 4: General structure of the separation system

LOCATIONS OF VAPOR RECOVERY SYSTEM

vapor from phase split

• Location 1: The purge stream - If significant amount of valuable materials are

Level 4: General structure of the separation system

TYPE OF VAPOR RECOVERY SYSTEM

1 ) Condensation - low. T and/or high P

ADJUST MATERIAL BALANCE ?

Level 4: General structure of the separation system

DECISION IN SYNTHESIZING LIQUID SEPARATION SYSTEM

Level 4: General structure of the separation system

1 ) ALTERNATIVES FOR LIGHT-ENDS REMOVAL

Level 4: General structure of the separation system

1 ) ALTERNATIVES FOR LIGHT-ENDS REMOVAL (cont.)

K. Glinos and M. F. Malone have published a shortcut design

Level 4: General structure of the separation system

2 ) DESTINATION OF LIGHT ENDS

3 ) AZEOTROPES WITH REACTANTS

- There is no general heuristic available for making this decision

Level 4: General structure of the separation system

Level 4: General structure of the separation system

5 ) SEQUENCING OF SIMPLE COLUMNS

Level 4: General structure of the separation system

5 ) SEQUENCING OF SIMPLE COLUMNS (cont.)

Level 4: General structure of the separation system

• General Heuristics for Column Sequencing

• Column Sequencing Heuristics for Simple Columns

Level 4: General structure of the separation system

Level 4: General structure of the separation system

6 ) COMPLEX COLUMNS (cont.) A

Level 4: General structure of the separation system

Other types of liquid separations

Level 4: General structure of the separation system

Level 4: General structure of the separation system

i. Use of two columns with different

Level 4: General structure of the separation system

Level 4: General structure of the separation system

Recycle extractive entrainer (H2SO4) 24

Level 4: General structure of the separation system

Level 4: General structure of the separation system

• The separation of xylene isomers is difficult by distillation

Level 4: General structure of the separation system

Less than the required product purity

Level 4: General structure of the separation system

Level 4: General structure of the separation system