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

1 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

2 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Section B: Algorithmic Methods

3 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

4 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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..

5 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Example 1. Specification for Butenes Recovery

6 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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withdrawn as n-C4 and 2-C4=s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2-C4=s withdrawn as furfural is added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bottoms and recycled n-C4 withdrawn as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.

7 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

8 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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 in volatility
heat transfer
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 in volatility
transfer
Azeotropic L and/or V Liquid V and L difference
entrainer and
Distillation in volatility
heat transfer

9 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Common Industrial Sep.Methods (Contd)
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

10 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Common Industrial Sep.Methods (Contd)
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

11 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

12 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Selecting Separation Method (2)
factor SF, defines the degree of separation
The separation factor,
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 / x 1 K1 P1 s
SF 1,2 s for ideal L and V
(5.2)
y2 / x2 K2 P2

13 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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 I I (5.5)
1 / 2

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.

14 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Relative volatilities for equal cost separators

Ref: Souders (1964)

15 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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.

16 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Algorithm to Select Pressure and Condenser Type

17 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

18 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Example 2 Sequences for 4-component separation

19 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Example 2 Sequences for 4-component separation

20 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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.

21 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Class Exercise

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

22 DESIGN AND ANALYSIS II - (c) 4 - Separation

 Class Exercise Possible Solution

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

23 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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)

24 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

25 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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).

26 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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 NS = 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.

27 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

28 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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

29 DESIGN AND ANALYSIS II - (c) 4 - Separation

 (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
30 DESIGN AND ANALYSIS II - (c) 4 - Separation
 (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
31 DESIGN AND ANALYSIS II - (c) 4 - Separation
 (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
32 DESIGN AND ANALYSIS II - (c) 4 - Separation
 (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
33 DESIGN AND ANALYSIS II - (c) 4 - Separation
 Lowest Cost Sequence

Sequence Cost, $/yr

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

34 DESIGN AND ANALYSIS II - (c) 4 - Separation

 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) 4 - Separation