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4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R.

Lewin 1
054402 Design and Analysis II

LECTURE 4: SEQUENCING OF
SEPARATION TRAINS

Daniel R. Lewin
Department of Chemical Engineering
Technion, Haifa, Israel


Ref: Seider, Seader and Lewin (1999), Chapter 5
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 2
Assess Primitive
Problem
Steps in Process Design and Retrofit
Development
of Base-case
Plant-wide
Controllability
Assessment
Detailed Design,
Equipment sizing, Cap.
Cost Estimation,
Profitability Analysis,
Optimization
Detailed Process
Synthesis -
Algorithmic
Methods
SECTION B
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 3
Section B: Algorithmic Methods
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 4
Introduction
Almost all chemical processes require the separation
of chemical species (components), to:
Opurify a reactor feed
Orecover unreacted species for recycle to a reactor
Oseparate and purify the products from a reactor
Frequently, the major investment and operating costs
of a process will be those costs associated with the
separation equipment
For a binary mixture, it may be possible to select a
separation method that can accomplish the
separation task in just one piece of equipment.
However, more commonly, the feed mixture involves
more than two components, involving more complex
separation systems
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 5
Instructional Objectives
Be familiar with the more widely used industrial
separation methods and their basis for separation.
Understand the concept of the separation factor and be
able to select appropriate separation methods for liquid
mixtures.
Understand how distillation columns are sequenced and
how to apply heuristics to narrow the search for a near-
optimal sequence.
Be able to apply systematic methods to determine an
optimal sequence of distillation-type separations..

When you have finished studying this unit, you should:
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 6
Example 1. Specification for Butenes Recovery
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 7
Design for Butenes Recovery System
100-tray column
C3 & 1-Butene in
distillate
Propane and
1-Butene recovery
Pentane
withdrawn as
bottoms
n-C4 and 2-C4=s
cannot be
separated by
ordinary
distillation
(o=1.03), so 96%
furfural is added
as an extractive
agent (o 1.17).
n-C4 withdrawn as
distillate.
2-C4=s withdrawn as
distillate. Furfural is
recovered as
bottoms and recycled
to C-4
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 8
Separation is Energy Intensive
Unlike the spontaneous mixing of chemical species, the
separation of a mixture of chemicals requires an
expenditure of some form of energy
Separation of a feed mixture into streams of differing
chemical composition is achieved by forcing the different
species into different spatial locations, by one or a
combination of four common industrial techniques:
Othe creation by heat transfer, shaft work, or pressure
reduction of a second phase that is immiscible with the
feed phase (ESA energy separating agent)
Othe introduction into the system of a second fluid phase
(MSA mass separating agent). This must be
subsequently removed.
Othe addition of a solid phase upon which adsorption can
occur
Othe placement of a membrane barrier
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 9
Common Industrial Separation Methods
Separation
Method
Phase of
the feed
Separation
agent
Developed or
added phase
Separation
principle
Equilibrium
flash
L and/or V
Pressure
reduction or
heat transfer
V or L difference
in volatility
Distillation L and/or V
Heat transfer
or shaft work
V or L difference
in volatility
Gas
Absorption
V
Liquid
absorbent
L difference
in volatility
Stripping

L
Vapor stripping
agent
V difference
in volatility
Extractive
Distillation
L and/or V
Liquid solvent
and heat
transfer
V and L difference
in volatility
Azeotropic
Distillation
L and/or V
Liquid
entrainer and
heat transfer
V and L difference
in volatility
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 10
Common Industrial Sep.Methods (Contd)
Separation
Method
Phase of
the feed
Separation
agent
Developed
or added
phase
Separation
principle
Liquid-liquid
Extraction
L Liquid
solvent
Second
liquid
Difference in
solubility
Crystalli-
zation
L Heat
transfer
Solid
Difference in
solubility or
m.p.
Gas
adsorption
V Solid
adsorbent
Solid
difference in
adsorbabililty
Liquid
adsorption
L Solid
adsorbent
Solid
difference in
adsorbabililty
Membranes L or V Membrane Membrane
difference in
permeability
and/or
solubility
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 11
Common Industrial Sep.Methods (Contd)
Separation
Method
Phase of
the feed
Separation
agent
Developed
or added
phase
Separation
principle
Supercritical
extraction
L or V
Supercritical
solvent
Supercritical
fluid
Difference
in solubility
Leaching S Liquid
solvent
L Difference
in solubility
Drying S and L Heat
transfer
V Difference
in volatility
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 12
Selecting Separation Method (1)
The development of a separation process requires the
selection of:
O Separation methods
O ESAs and/or MSAs
O Separation equipment
O Optimal arrangement or sequencing of the equipment
O Optimal operating temperature and pressure for the equipment
Selection of separation method largely depends of feed
condition
O Vapor: partial condensation, distillation, absorption, adsorption,
gas permeation (membranes)
O Liquid: distillation, stripping, LL extraction, supercritical
extraction, crystallization, adsorption, and dialysis or reverse
osmosis (membranes)
O Solid: if wet drying, if dry leaching
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 13
Selecting Separation Method (2)
The separation factor, SF, defines the degree of
separation achievable between two key components of he
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:
II II
I I
C C
C C
SF
2 1
2 1
/
/
= (5.1)
C = composition variable,
I, II = phases rich in
components 1 and 2.
SF is generally limited by thermodynamic equilibrium. For
example, in the case of distillation, using mole fractions as
the composition variable and letting 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:
|
|
.
|

\
|
= o = = = V and L ideal for
/
/
2
1
2 , 1
2
1
2 2
1 1
s
s
P
P
K
K
x y
x y
SF (5.2)
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 14
Selecting Separation Method (3)
For vapor-liquid separation operations that use an
MSA that causes the formation of a non-ideal liquid
solution (e.g. extractive distillation):
(5.4)
s L
s L
P
P
SF
2 2
1 1
2 , 1

= o =
In general, MSAs for extractive distillation and liquid-liquid
extraction are selected according to their ease of recovery
for recycle and to achieve relatively large values of SF.
If the MSA is used to create two liquid phases, such as in
liquid-liquid extraction, the SF is referred to as the
relative selectivity, | , where:
I I
II II
SF
2 1
2 1
2 , 1
/
/


= | =
(5.5)
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Relative volatilities for equal cost separators
Ref: Souders (1964)
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 16
Sequencing of Ordinary Distillation Columns
o in each column is > 1.05.
The reboiler duty is not excessive.
The tower pressure does not cause the mixture to
approach the T
C
of the mixture.
Column pressure drop is tolerable, particularly if operation
is under vacuum.
The overhead vapor can be at least partially condensed at
the column pressure to provide reflux without excessive
refrigeration requirements.
The bottoms temperature for the tower pressure is not so
high that chemical decomposition occurs.
Azeotropes do not prevent the desired separation.
Use a sequence of ordinary distillation (OD) columns to
separate a multicomponent mixture provided:
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 17
Algorithm to Select Pressure and Condenser Type
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 18
Number of Sequences for Ordinary Distillation
Equation for number of different sequences of P 1 ordinary
distillation (OD) columns, N
S
, to produce P products:
)! 1 ( !
)]! 1 ( 2 [

=
P P
P
N
s
(5.7)
P # of Separators N
s

2 1 1
3 2 2
4 3 5
5 4 14
6 5 42
7 6 132
8 7 429
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 19
Example 2 Sequences for 4-component separation
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 20
Example 2 Sequences for 4-component separation
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 21
Identifying the Best Sequences using Heuristics
O Remove thermally unstable, corrosive, or chemically reactive
components early in the sequence.
O Remove final products one-by-one as distillates (the direct
sequence).
O Sequence separation points to remove, early in the sequence,
those components of greatest molar percentage in the feed.
O Sequence separation points in the order of decreasing relative
volatility so that the most difficult splits are made in the absence
of other components.
O Sequence separation points to leave last those separations that
give the highest purity products.
O Sequence separation points that favor near equimolar amounts of
distillate and bottoms in each column. The reboiler duty is not
excessive.
The following guidelines are often used to reduce the number
of OD sequences that need to be studied in detail:
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 22
Class Exercise
Design a sequence of
ordinary distillation
columns to meet the
given specifications.
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 23
Class Exercise Possible Solution
Guided by Heuristic 4,
the first column in
position to separate the
key components with the
greatest SF.
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 24
Complex Columns for Ternary Mixtures
Ref: Tedder and Rudd (1978)
In some cases, complex rather than simple distillation columns should
be considered when developing a separation sequence.
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 25
Regions of Optimality
ESI s 1.6 ESI > 1.6
As shown below, optimal regions for the various configurations
depend on the feed composition and the ease-of-separation index:
ESI = o
AB
/ o
BC
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 26
Sequencing of V-L Separation Systems
When simple distillation is not practical for all separators
in a multicomponent mixture separation system, other
types of separators must be employed and the order of
volatility or other separation index may be different for
each type.
For example, if P = 3, and ordinary distillation, extractive
distillation with either solvent I or solvent II, and LL
extraction with solvent III are to be considered, then T =
4, and applying Eqns (5.7) and (5.8) gives 32 possible
sequences (for ordinary distillation alone, N
S
= 2).
(5.8) s
P T
s
N T N
1
=
If they are all two-product separators and if T equals the
number of different types, then the number of possible
sequences is now given by:

4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 27
Example 3 (Example 1 Revisited)
Species b.pt.(C) Tc (C) Pc, (MPa)
Propane A -42.1 97.7 4.17
1-Butene B -6.3 146.4 3.94
n-Butane C -0.5 152.0 3.73
trans-2-Butene D 0.9 155.4 4.12
cis-2-Butene E 3.7 161.4 4.02
n-Pentane F 36.1 196.3 3.31
For T = 2 (OD and ED), and P = 4, N
S
= 40.
However, since 1-Butene must also be separated (why?), P = 5,
and N
S
= 224.
Clearly, it would be helpful to reduce the number of sequences
that need to be analyzed.
Need to eliminate infeasible separations, and enforce OD for
separations with acceptable volatilities.
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 28
Example 3 (Example 1 Revisited)
Adjacent Binary Pair o
ij
at 65.5
o
C
Propane/1-Butene (A/B) 2.45
1-Butene/n-Butane (B/C) 1.18
n-Butane/trans-2-Butene (C/D) 1.03
cis-2-Butene/n-Pentane (E/F) 2.50
Splits A/B and E/F should be by OD only (o ~ 2.5)
Split C/D is infeasible by OD (o = 1.03). Split B/C is feasible,
but an alternative method may be more attractive.
Use of 96% furfural as a solvent for ED increases volatilities of
paraffins to olefins, causing a reversal in volatility between 1-
Butene and n-Butane, altering separation order to ACBDEF, and
giving o
C/B
= 1.17. Also, split (C/D)
II
with o = 1.7, should be used
instead of OD.
Thus, splits to be considered, with all others forbidden, are:
(A/B)
I
, (E/F)
I
, (B/C)
I
, (A/C)
I
, (C/B)
II
, and (C/D)
II


4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 29
Estimating Annualized Cost, C
A
For each separation, C
A
is estimated assuming 99 mol %
recovery of light key in distillate and 99 mol % recovery
of heavy key in bottoms. The following steps are followed:

O Estimate number of stages and reflux ratio by FUG method
(e.g., using HYSYS.Plant Shortcut Column).
O Select tray spacing (typically 2 ft.) and calculate column
height, H.
O Compute tower diameter, D (using Fair correlation for flooding
velocity, or HYSYS Tray Sizing Utility).
O Estimate installed cost of tower (see Unit 6 and Chapter 9).
O Size and cost ancillary equipment (condenser, reboiler, reflux
drum). Sum total capital investment, C
TCI
.
O Compute annual cost of heating and cooling utilities (COS).
O Compute C
A
assuming ROI (typically r = 0.2). C
A
= COS + r C
TCI
O Set distillate and bottoms column pressures using
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 30
Sequence Cost, $/yr
1-5-16-28 900,200
1-5-17-29 872,400
1-6-18 1,127,400
1-7-19-30 878,000
1-7-20 1,095,600
1
st
Branch of Sequences
Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F
(A/B)
I
, (E/F)
I
, (B/C)
I
, (A/C)
I
, (C/B)
II
, and (C/D)
II

4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 31
Sequence Cost, $/yr
2-(8,9-21) 888,200
2-(8,10-22) 860,400
2
nd
Branch of Sequences
Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F
(A/B)
I
, (E/F)
I
, (B/C)
I
, (A/C)
I
, (C/B)
II
, and (C/D)
II

4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 32
Sequence Cost, $/yr
3-11-23-31 878,200
3-11-24 1,095,700
3-12-(25,26) 867,400
3-13-27 1,080,100
3
rd
Branch of Sequences
Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F
(A/B)
I
, (E/F)
I
, (B/C)
I
, (A/C)
I
, (C/B)
II
, and (C/D)
II

4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 33
Sequence Cost, $/yr
4-14-15 1,115,200
4
th
Branch of Sequences
Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F
(A/B)
I
, (E/F)
I
, (B/C)
I
, (A/C)
I
, (C/B)
II
, and (C/D)
II

4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 34
Lowest Cost Sequence
Sequence Cost, $/yr
2-(8,10-22) 860,400
4 - Separation Trains DESIGN AND ANALYSIS II - (c) Daniel R. Lewin 35
Separation Trains - Summary
Be familiar with the more widely used industrial
separation methods and their basis for separation.
Understand the concept of the separation factor and be
able to select appropriate separation methods for liquid
mixtures.
Understand how distillation columns are sequenced and
how to apply heuristics to narrow the search for a near-
optimal sequence.
Be able to apply systematic B&B methods to determine an
optimal sequence of distillation-type separations..

On completing this unit, you should:
Next week: Azeotropic Distillation