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Module 4: Design of Separation Systems

Lecture-13
Design of separation processes
Course: Process Plant Design CE 1705/1701

Nandana Chakinala
Department of Chemical Engineering
Revisit: Level 1
• Input information required are:
1. Reactions and reaction conditions
2. Desired production rate
3. Desired product purity, or some information on price vs.
purity
4. Raw materials and/or some information about price vs.
purity
5. Information on rate of reaction and rate of catalyst
deactivation
………many more

2
Revisit: Level 2

1. Should we purify the feed streams before they

enter the process?
2. Should we remove or recycle a reversible by-
product?
3. Should we use a gas recycle and purge stream?
4. How many product streams will be there?
5. What are the design variables for the input-output
structure, and what economic trade-offs are
associated with these variables?

3
Revisit: Level 3

• Number of reactor systems required

– Is there any separation between the reactor systems?
• Number of recycle streams required
• Use of an excess of any one reactant at the reactor
inlet
• Gas compressors are required?
– What are the costs?
• Should the reactors be
– Operated adiabatically, or
– With direct heating or cooling, or
– Is a diluent or heat carrier required?
4
Contd..

• Is shift in equilibrium conversion required? If so

how?
• Effect of reactor cost on Economic Potential

5
Introduction
1. Separation and purification of products is important step of
process design as stream emerging from reactor is
multicomponent mixture
2. Separation of most of the reaction mixtures not spontaneous,
occurs at the expenditure of energy or use of other mechanical
forces
3. Homogenous single solution: A second immiscible phase is
generated by MSA or ESA
1. Absorption, Distillation, extraction perhaps most common
2. Besides these azeotropic, extractive distillation, crystallization
3. More recently, use of microporous and non porous semi permeable
membranes received considerable attention.
▪ Ultra filtration
▪ Osmosis
▪ Gas separation
▪ Pervaporation
4. Removal of certain compounds by solid MSA
▪ Adsorption
▪ Chromatography
▪ Ion exchange resin
CE 1705/1701 Process Plant Design

Introduction

5. Evaluation and selection of separation process for a

particular mixture depends on the overall economics of
the process
6. Other measures for separation evaluation: Percentage
recovery, product purity

7
CE 1705/1701 Process Plant Design

Heterogenous separation

The phase separation likely to be carried out:

• Gas–liquid (or vapor–liquid)
• Gas–solid (or vapor–solid)
• Liquid–liquid (immiscible)
• Liquid–solid
• Solid–solid

Principles methods for heterogenous mixture separation

– • Settling and sedimentation
– • Inertial and centrifugal separation
– • Electrostatic precipitation
– • Filtration
– • Scrubbing
– • Flotation
– • Drying.

8
Settling/Sedimentation
CE 1705/1701 Process Plant Design

Settling/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
➢ The velocity of the gas or vapor through the vessel must be
less than the settling velocity of the liquid drops
➢ Force balance (Assuming sphere), valid when no turbulence
in settler

10
CE 1705/1701 Process Plant Design

Inertial/Centrifugal separation
• Separation of particles in the fluid through centrifugal force
• Useful when gravity separation is too slow because of close densities
of particles
Inertial or momentum separators, giving the particles downward
momentum, in addition to the gravitational force
Use of centrifugal force increases force acting on the particles. Eg:
Cyclone separator for separation of solid/liq particles from gas/vapor
The design of cyclones is normally based on collection efficiency curves,

11
CE 1705/1701 Process Plant Design

Electrostatic precipitation
• generally used to separate particulate
matter that is easily ionized from a gas
stream
• particulate-laden gas stream passes
through the space,
• ionizes molecules of gases such as O2
and CO2 present in the gas stream.
These charged molecules attach
themselves to particulate matter,
thereby charging the particles.

12
CE 1705/1701 Process Plant Design

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).
• Cake filtration: Particles retained on the
surface of the filter medium, scraped
continuously to control ∆P across the
filter

13
Flotation
• Solid-solid mixture separation
• Gas bubbles generated in the liquid, gets attached to
solid surfaces, allowing them to rise to the liquid surface
• Then solid particles removed by overflow weir or
mechanical scraper
• Separation dependant on the surface properties which
govern the attachment of solid particles to the bubble
surface

14
CE 1705/1701 Process Plant Design

Homogenous separation

15
Guidelines for separation process
selection for heterogeneous mixtures
Distillation
• feed condition – L/V
• Mass fraction key component 10-95%
• Normal feed capacity 1-100 kg/s
• Adv: Simple flowsheet, easily scalable, low capital investment
• Limitation: Need adequate volatility and thermal stability of component
Azeotropic Distillation
• feed condition – L/V
• Separating agent: Liquid entrainer + heat transfer
• Normal feed capacity 1-60 kg/s
• Adv: Breaks azeotrope and operates at normal P
• Limitation: More complex system design, requires recovery of entrainer and
hence increased capital investment

16
CE 1705/1701 Process Plant Design

Guidelines for separation process

selection for heterogeneous mixtures
Absorption
• Solute separation from gas streams
• Absorption factor L/mG for relatively dilute component in gas phase
determines how readily that component is absorbed
• Large absorption factors implies large liquid flow rates diminish economy
• Optimum value of 1.4
Stripping
• Stripping factor optimum value 1.4

17
CE 1705/1701 Process Plant Design

Guidelines for separation process

selection for heterogeneous mixtures
Extraction
• Distribution coefficient
• Adv: Can handle azeotropes, can be operated at low T, recovery of
thermally sensitive products
• Supercritical solvents have enhanced properties in addition to higher
equilibrium ratios and separation factors larger than normal solvents
• Extractor should be maintained at high P to keep solvent in supercritical
state, high operating cost

18
CE 1705/1701 Process Plant Design

Guidelines for separation process

selection for heterogeneous mixtures
Crystallization
• Recovery of dissolved materials in solution in solid form by precipitation
upon cooling or removal of solvents or addition of precipitating agents
• Design based on phase equilibria, solubility rates, and amount of nuclei
generated, rate of crystal growth
• For this operation, pilot plant design required to establish critical design
parameters

19
CE 1705/1701 Process Plant Design

Guidelines for separation process

selection for heterogeneous mixtures
Membrane separations
• Selectively permit flow of one or more components
• Permeate and retentate, Driving force difference in pressure
• Can separate molecular levels
• Limitation: Cant operate at high T, Difficult to stage membrane process

20
CE 1705/1701 Process Plant Design

Guidelines for separation process

selection for heterogeneous mixtures
Adsorption
• Selective adsorption of one or more components from the mixture on a
suitable adsorbent and regeneration of the loaded adsorbent
• Adsorbent is MSA, hence its movement from one location to other is difficult
• Hence, regeneration can be done by temperature swing or pressure swing
• Wide application in gas separations
Ion exchange
• Similar to adsorption except chemical reaction is involved
• Wide application in water softening, where a solid organic polymer in its
sodium form exchanges calcium and magnesium ions from water
• Ion exchange column can be regenerated by using concentrated sodium
salt solution

21
Selection of suitable
separation process
Factors to be considered in selecting separations for
particular application
• Exploitable property differences
• Feed and product conditions
• Flow rate, composition of key components to be recovered
• Characteristics of separation process
• More dilute the key component in the reaction mixture
greater the cost of separation

22
Design suitable separation
process- General guidelines
• A separation system well understood can be
mathematically modelled and scaled up to handle
industrial flow rates
• Some separations require a pilot plant testing before
final design with some assurance of final success
• Operations based on barrier separations are more
expensive to stage than based on creation or addition of
second phase
• Some separations are limited to maximum size, hence
use of parallel units is necessary

23
Separation System

• Synthesis of a separation system to recover

gaseous and liquid components

• 3 parts:
1. General Structure
2. Vapor Recovery System (VRS)
3. Liquid Separation System (LSS)

• Before deciding VRS & LSS, we should decide on

General Structure
24
Contd..

• Also, we need to determine the best separation

system
– As a function of the design variables
– i.e., the range of design variables where we obtain
profitable operation

25
General Structure of the
Separation System
• First determine the phase of the reactor effluent
stream

Fig: Phase of Reactor effluent

stream
Crucial stream for deciding on general structure
Douglas, J. M. Conceptual Design of Chemical Processes, 1988, pp. 164
26
Contd..

• For vapor-liquid processes

1. Reactor effluent is a liquid

2. Reactor effluent is a two-phase mixture
3. Reactor effluent is all vapor

(1) If the reactor effluent is a liquid

– We assume that we only need a liquid separation
system
– The system might include distillation columns, extraction
units, etc.
– Normally there will not be any gas absorber, gas
adsorption units etc.

27
Contd..

Fig: Rector exit is liquid

Douglas, J. M. Conceptual Design of Chemical Processes, 1988, pp. 164

28
Contd..

(2) If the reactor effluent is a two-phase mixture

• Put a flash drum after the reactor
– liquids to a liquid separation system
– If the reactor is operated above cooling water
temperature
– We usually cool the reactor vapour stream to 100 0F (35
0C - 370C)

• And phase split this stream (stream 1)

29
Contd..

Fig: Rector exit is vapor and liquid

Douglas, J. M. Conceptual Design of Chemical Processes, 1988, pp. 164
30
Contd..

– If the low-temperature flash liquid obtained from phase

split contains mostly reactants (and no product
components that are formed as intermediates in a
consecutive reaction scheme)
• then we recycle them to the reactor (stream 2)

– However if the low-temperature flash liquid contains

mostly products
• we send this stream to the liquid recovery system (stream 3)

– The low-temperature flash vapor is usually sent to a

vapor recovery system (stream 4)

31
Contd..

– If the reactor effluent stream contains only a small

amount of vapor
• we often send the reactor effluent (stream 5) directly to a liquid
separation system (i.e. distillation train)
(3) If reactor effluent is all vapor
– We cool the stream to 100oF (cooling-water temperature)
– We attempt to achieve a phase split or to completely
condense this stream
– The condensed liquid is sent to a liquid recovery system,
and the vapor is sent to a vapor recovery system

32
Contd..

Fig: Rector exit is vapor

33 Douglas, J. M. Conceptual Design of Chemical Processes, 1988, pp. 165
Heuristic

The design of separation systems is based on that

“ Phase splits are the cheapest method of separations and
assumption that some type of distillation separation is
possible”

34
Approximate Flash
Calculations
• To determine the phase of the reactor effluent, in
some cases
– use a sharp-split approximation procedure to avoid the
trial-and-error solutions associated with flash
calculations
• The flash equations can be written as

35
Contd..

• Overall balance:
F=V+L (7.1.1)

• Component balance:
Fzi = Vyi + Lxi (7.1.2)

• Equilibrium:
yi = Kixi (7.1.3)

36
Contd..

• From Eqs. (7.1.2) & (7.1.3)

L  L 
Fz = Vy +
i yi = V +  yi
i
K i  Ki 
V L 1   V F −V 1 
=  +  y = + y
zi  F F  i  F F  i
 Ki   Ki 
 V  V  1  z
=  +  −   y y = i
zi  F  F   i
1 i V  V 1 (7.1.4)
(7.1.4)
  K i  + 1 − 
F  F  Ki
37
Rachford-Rice eqn

• Or,

38
Contd..

• If Ki>>1, from Eq. (7.1.4)

(7.1.6)

• If Ki<<1, from Eq. (7.1.5)

(7.1.7)

39
Contd..

• Thus, as a first estimate of the vapor and liquid

flow rates, we can write:
(7.1.8) (7.1.8)

• for all components, where Ki > 10, and

(7.1.9) (7.1.9)
• for all components, where Ki < 0.1
• Where,

40
Contd..

• These equations (7.1.8 & 7.1.9) are equivalent to a

perfect split
– Providing there are no components with a Ki value
between 0.1 and 10
• The perfect split expressions ignore the vapor-
liquid equilibrium

41
Exact Flash Calculation

• Thus, the liquid composition in equilibrium with a

vapor component having a mole fraction

(7.1.10)

is

(7.1.11)

42
Contd..

• The liquid flow of this component is then

(7.1.12)

• Now adjusting the vapor flow for this loss

(7.1.13)

43
Contd..

• The corresponding expressions for components

that are predominant in the liquid phase are

(7.1.14)

(7.1.15)

44
Contd.. Douglas, J. M. Conceptual Design of Chemical Processes, 1988, pp. 167

• Table 7.1-1 compares the approximate and exact

solutions for the HDA process

gas

liquid

45
Vapor Recovery Systems

• To synthesize a vapor recovery system, we need to

make two decisions

1. What is the best location?

2. What type of vapor recovery system is cheapest?

46
Location of Vapor recovery
system
• There are four choices
1. The purge stream
a. If significant amount of valuable material is being lost is in the
purge stream, then place the vapor recovery system in the
purge stream.
2. The gas-recycle stream
b. If recycling some components degrades the product distribution.
The recycle stream normally has second smallest flow rate
3. The flash vapor stream
c. If both item 1 and 2 are valid
4. Do not use VRS if neither item 1 and 2 are important

47
Contd..
• The rules we use to make this decision are as
follows

Fig: Vapor Recovery System Location

48 Douglas, J. M. Conceptual Design of Chemical Processes, 1988, pp. 169
Do we need a vapor recovery system
for HDA process?

49
Specification

Conversion yPH Purge flow Recycle

(x) rate flow rate
(mol/h) (mol/h)
0.75 0.4 496 3371

Benzene loss in Toluene loss Loss in

purge (mol/h) in purge Economics
(mol/h) ($/yr)
3.79 0.46 0.304 × 106

50
Types of Vapor Recovery System
• The most common choices (with current
technology) are
1. Condensation – By compression or cooling or both
2. Absorption
3. Adsorption
4. Membrane separation processes
5. Reactive systems

The choice of vapour recovery system depends on the physical and

chemical characteristics of the system in addition to the economic
trade off
The strategy is that vapor recovery system generates liquid stream
that needs to be further purified. Therefore, before designing of the
liquid separation system, the vapor recovery system needs to be
designed
51
Strategy

• Design the vapor recovery system (VRS) before we

consider the liquid separation system (LSS)
– Because each of the vapor recovery processes usually
generates a liquid stream that must be further purified

52
Combined vapor recovery and
liquid separation system
HDA Case study

53
Separation Factor

• The separation factor, SF, defines the degree of

separation achievable between two key
components of the feed
• This factor, for the separation of component 1 from
component 2 between phases I and II, for a single
stage of contacting, is defined as:

C 1I / C 2I C = composition variable, I, II =
SF = phases rich in components 1 and 2
C 1II / C 2II
Cond..

• SF is generally limited by thermodynamic

equilibrium
– For example, in the case of distillation,
mole fractions as the composition variable
phase I be the vapor and phase II be the liquid
– the limiting value of SF is given in terms of vapor-liquid
equilibrium ratios (K-values) as:

y1 / x1 K1
SF = = = 1, 2
y 2 / x2 K 2
Combining VRS with LSS

• If we use a partial condenser and a flash drum to

phase split the reactor effluent
– some of the lightest liquid components will leave with the
flash vapor
– and therefore will not be recovered in the liquid recovery
system
– Flash drum is not perfect split

56
Combining VRS with LSS

• However, if there is only a small amount of vapor in

the stream leaving the partial condenser
– And if the first split in the liquid separation is chosen to
be distillation
• We could eliminate the phase splitter and feed the reactor
effluent stream directly into the distillation column
• In this case, diameter of the distillation column with the two
phase feed will have to be larger to handle vapour load
• However, this increased cost may be less than cost associated
with using VRS to remove liquid components from flash vapour
stream
• No heuristic available for this decision and hence we need to add
another process alternative to our list

57
Liquid Separation System

• The decisions that we need to synthesize the liquid

separation system:
1. How should the light ends be removed if they might
contaminate the product?
2. What should be the destination of the light ends?
3. What about azeotropes – do we recycle components
forming azeotropes or do we split them?
4. What separations can be made by distillation?
5. What sequences of columns do we use?
6. How should we accomplish separations if distillation is
not feasible?

58
Contd..

• Make these decisions

– as a function of the design variables
– over the range of potentially profitable operation

59
Light Ends

• Some light ends will be dissolved in the

– liquid leaving the phase splitters
– normally some will be dissolved in the liquid stream
leaving the vapor recovery systems
• If these light ends might contaminate the products
– they must be removed

60
LSS: How to remove Light
ends?
• Alternatives for light ends removal – Listed in the
order of increasing cost
1. Drop the pressure of a stream and remove the light
ends in a phase splitter
2. Use a partial condenser on the product column
3. Use a pasteurization section on the product column
4. Use a stabilizer column before the product column
• Normal distillation column that removes light ends
Contd..
• Pasteurization column
For the special case of side-stream columns where the
desired product is the intermediate boiler and there is a
waste or fuel by-product that is either 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).

62
LSS: Destination of Light Ends
1. Vent , if the light ends have very little value. Also if
this venting causes air pollution problems, we try to
vent them through a flare system.
2. Fuel , if most of the light ends are flammable, we
try to recover the fuel value.
3. Recover and recycle to the vapor recovery system
, if the light ends are valuable, we want to retain
them in the process.

63
LSS: Summary of Light Ends
• If light ends do not contaminate the product
– recycle them to the reactor with a reactant recycle stream
– or remove them from the process with a by-product
stream that is sent to the fuel supply
• If the light ends contaminate the product
– they must be removed from the process
• The method of removal and destination of the light
ends
– depends on the amount of light ends
Determination of amount of light ends as a function of
design variables is must before making a final
decision

64
Azeotropes with reactants

If a component forms an azeotrope with a reactant, we have

two choices:
1. Recycling the azeotrope (over sizing all the equipments in
the recycle loop to handle the incremental flow of the extra
components).
2. Splitting the azeotrope and just recycling the reactant
(requires 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.

65
LSS: Applicability of Distillation

• In general, distillation is the least expensive means

of separating mixtures of liquids
– However, if the relative volatilities (α) of the components
with close boiling points is less than 1.1 (i.e., α < 1.1) or
so
– Then, distillation becomes very expensive
1. i.e., large reflux ratio
2. large condensers and reboilers
3. large steam and cooling water costs

66
Contd..

• Whenever we encounter two neighbouring

components having a relative volatility of less than
1.1 in a mixture
– we group these components together and treat this
group as a single component in the mixture

67