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

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 Steps in Process Design and Retrofit

Assess Primitive
Problem

Detailed Process Plant-wide

Synthesis - Development Controllability
Algorithmic of Base-case Assessment
Methods

SECTION B
Detailed Design,
Equipment sizing, Cap.
Cost Estimation,
Profitability Analysis,
Optimization

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 Section B: Algorithmic Methods

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 Introduction
 Almost all chemical processes require the separation
of chemical species (components), to:
 purify a reactor feed
 recover unreacted species for recycle to a reactor
 separate 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

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 Instructional Objectives
When you have finished studying this unit, you should:
 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..

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 Example 1. Specification for Butenes Recovery

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 Design for Butenes Recovery System
100-tray column
C3 & 1-Butene in
distillate

Propane and
1-Butene recovery
Pentane
withdrawn as n-C4 and 2-C4=s
bottoms cannot be
separated by
ordinary
distillation
(=1.03), so 96%
2-C4=s withdrawn as furfural is added
distillate. Furfural is as an extractive
recovered as agent (  1.17).
bottoms and recycled n-C4 withdrawn as
to C-4 distillate.

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 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:
 the creation by heat transfer, shaft work, or pressure
reduction of a second phase that is immiscible with the feed
phase (ESA – energy separating agent)
agent
 the introduction into the system of a second fluid phase ( MSA
– mass separating agent).
agent This must be subsequently removed.
 the addition of a solid phase upon which adsorption can occur
 the placement of a membrane barrier

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 Common Industrial Separation Methods
Separation Phase of Separation Developed or Separation
Method the feed agent added phase principle
Equilibrium L and/or V Pressure V or L difference
reduction or
flash heat transfer
in volatility

Distillation L and/or V Heat transfer V or L difference

or shaft work
in volatility
Gas V Liquid L difference
absorbent
Absorption in volatility
Stripping L Vapor stripping V difference
agent
in volatility
Extractive L and/or V Liquid solvent V and L difference
and heat
Distillation transfer
in volatility

Azeotropic L and/or V Liquid V and L difference

entrainer and
Distillation heat transfer
in volatility

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 Common Industrial Sep.Methods (Cont’d)
Separation Phase of Separation Developed Separation
Method the feed agent or added principle
phase
Liquid-liquid L Liquid Second Difference in
Extraction solvent liquid solubility

Crystalli- L Heat Solid Difference in

zation transfer solubility or
m.p.
Gas V Solid Solid difference in
adsorption adsorbent adsorbabililty

Liquid L Solid Solid difference in

adsorption adsorbent adsorbabililty

Membranes L or V Membrane Membrane difference in

permeability
and/or
solubility

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 Common Industrial Sep.Methods (Cont’d)
Separation Phase of Separation Developed Separation
Method the feed agent or added principle
phase
Supercritical L or V Supercritical Supercritical Difference
extraction solvent fluid in solubility
Leaching S Liquid L Difference
solvent in solubility
Drying S and L Heat V Difference
transfer in volatility

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 Selecting Separation Method (1)
 The development of a separation process requires the
selection of:
 Separation methods
 ESAs and/or MSAs
 Separation equipment
 Optimal arrangement or sequencing of the equipment
 Optimal operating temperature and pressure for the equipment
 Selection of separation method largely depends of feed
condition –
 Vapor: partial condensation, distillation, absorption, adsorption,
gas permeation (membranes)
 Liquid: distillation, stripping, LL extraction, supercritical
extraction, crystallization, adsorption, and dialysis or reverse
osmosis (membranes)
 Solid: if wet  drying, if dry leaching

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 Selecting Separation Method (2)
 The separation factor,
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,
contacting is
defined as:
C = composition variable,
C 1I / C 2I
SF  I, II = phases rich in (5.1)
C 1II / C 2II 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:
y 1 / x1 K1  P1 s 
SF    1,2   s for ideal L and V 
 (5.2)
y2 / x2 K2  P2 

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 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):
1LP1 s
SF  1,2  L s (5.4)
2P2

 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:
1II /  2II
SF  1,2  (5.5)
1I /  2I

 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.

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 Relative volatilities for equal cost separators

Ref: Souders (1964)

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 Sequencing of Ordinary Distillation Columns
Use a sequence of ordinary distillation (OD) columns to
separate a multicomponent mixture provided:
  in each column is > 1.05.
 The reboiler duty is not excessive.
 The tower pressure does not cause the mixture to approach
the TC 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.

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 Algorithm to Select Pressure and Condenser Type

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 Number of Sequences for Ordinary Distillation
Equation for number of different sequences of P  1 ordinary
distillation (OD) columns, NS, to produce P products:
[2(P  1)]!
Ns  (5.7)
P ! (P  1)!
 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

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 Example 2 – Sequences for 4-component separation

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 Example 2 – Sequences for 4-component separation

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 Identifying the Best Sequences using Heuristics
The following guidelines are often used to reduce the number
of OD sequences that need to be studied in detail:
 Remove thermally unstable, corrosive, or chemically reactive
components early in the sequence.
 Remove final products one-by-one as distillates (the direct
sequence).
 Sequence separation points to remove, early in the sequence, those
components of greatest molar percentage in the feed.
 Sequence separation points in the order of decreasing relative
volatility so that the most difficult splits are made in the absence
of other components.
 Sequence separation points to leave last those separations that give
the highest purity products.
 Sequence separation points that favor near equimolar amounts of
distillate and bottoms in each column. The reboiler duty is not
excessive.

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 Class Exercise

Design a sequence of
ordinary distillation
columns to meet the
given specifications.

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 Class Exercise – Possible Solution

Guided by Heuristic 4,
the first column in
position to separate the
key components with the
greatest SF.

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 Complex Columns for Ternary Mixtures
In some cases, complex rather than simple distillation columns should
be considered when developing a separation sequence.

Ref: Tedder and Rudd (1978)

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 Regions of Optimality
As shown below, optimal regions for the various configurations
depend on the feed composition and the ease-of-separation index:
ESI = AB/ BC

ESI  1.6 ESI  1.6

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 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.
 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:
NsT  T P 1Ns (5.8)
 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, NS =
2).

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 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, NS = 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.

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 Example 3 (Example 1 Revisited)
Adjacent Binary Pair ij at 65.5 oC
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 (  2.5)
 Split C/D is infeasible by OD ( = 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 C/B =
1.17. Also, split (C/D)II with  = 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

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 Estimating Annualized Cost, CA
 For each separation, CA 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:
 Set distillate and bottoms column pressures using
 Estimate number of stages and reflux ratio by FUG method
(e.g., using HYSYS.Plant “Shortcut Column”).
 Select tray spacing (typically 2 ft.) and calculate column height,
H.
 Compute tower diameter, D (using Fair correlation for flooding
velocity, or HYSYS Tray Sizing Utility).
 Estimate installed cost of tower (see Unit 6 and Chapter 9).
 Size and cost ancillary equipment (condenser, reboiler, reflux
drum). Sum total capital investment, CTCI.
 Compute annual cost of heating and cooling utilities (COS).
 Compute CA assuming ROI (typically r = 0.2). CA = COS + r CTCI

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 (A/B…)I, (…E/F)I, (…B/C…)I, (A/C…)I , (…C/B…)II, and (…C/D…)II

1st Branch of Sequences

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

Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F

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 (A/B…)I, (…E/F)I, (…B/C…)I, (A/C…)I , (…C/B…)II, and (…C/D…)II

2nd Branch of Sequences

Sequence Cost, $/yr

2-(8,9-21) 888,200

2-(8,10-22) 860,400

Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F

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 (A/B…)I, (…E/F)I, (…B/C…)I, (A/C…)I , (…C/B…)II, and (…C/D…)II

3rd Branch of Sequences

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

Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F

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 (A/B…)I, (…E/F)I, (…B/C…)I, (A/C…)I , (…C/B…)II, and (…C/D…)II

4th Branch of Sequences

Sequence Cost, $/yr

4-14-15 1,115,200

Species
Propane A
1-Butene B
n-Butane C
trans-2-Butene D
cis-2-Butene E
n-Pentane F

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 Lowest Cost Sequence

Sequence Cost, $/yr

2-(8,10-22) 860,400

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 Separation Trains - Summary
On completing this unit, you should:
 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..

Next week: Azeotropic Distillation

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