SKF 4513: Plant Design 1

SEQUENCING OF SEPARATION TRAINS

Edited and Presented by

Agus Arsad, PhD
Department of Gas Engineering
UTM

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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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 General Flowsheet with Reactors Feed and
Effluent Separation Systems

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 Example of feed Separation System
Removal of C3 from a stream of propylene/C3
mixture. C3 is not involved in polypropylene
production so it is removed using a distillation
unit.

Production of formaldehyde by air-oxidation

of MeOH using silver catalyst. Entering air is
scrubbed with aq NaOH to remove SO2 and
CO2 which are catalyst poisons

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 Phase-separation Equipment

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 Effluent Separation System and Recycle

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 Example of Effluent Separation System

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 Example 1. Specification for Butenes Recovery

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 Design for Butenes Recovery System

2 columns, C3 &
1-Butene in
distillate (Total
150 trays)

Depropanizer

Deoiler Unit: Extractive Dist Unit:

Pentane withdrawn n-C4 and 2-C4=s
as bottoms cannot be separated
by ordinary distillation
(=1.03), so 96%
furfural is added as an
extractive distillation
Furfural Stripper: agent ( 1.17).
2-C4=s withdrawn as
distillate. Furfural is n-C4 withdrawn as
recovered as distillate.
bottoms and recycled
to C-4
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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)
the introduction into the system of a second fluid (chemical)
phase (MSA mass separating agent). This must be subsequently
removed/recovered.
the addition of a solid phase upon which adsorption can occur
the placement of a membrane barrier for selective permeation

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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 (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.
(cooling)
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 (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

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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

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 Selecting Separation Method (1)
Selection of separation method largely depends of feed
condition
Vapor: partial condensation, distillation (cryogenic), gas
absorption, gas adsorption, gas permeation
(membranes), desublimation
Liquid: flash or partial vaporization, distillation,
extractive dist, azeotropic dist, stripping, LL extraction,
supercritical extraction, crystallization, liquid
adsorption, and dialysis, reverse osmosis, ultrafiltration
(membranes)
Solid: if wet drying, if dry leaching
If slurries.filtration or centrifugation to get a wet
cake.
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 Selecting Separation Method (2)
The separation factor, SF, defines the degree of separation
achievable between two key components of he feed.

SF is arranged (for calculation) to give value >1.0

The larger the SF, the easier is to separate the mixtures

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 /C C /C I I I II
C = composition variable,
(7.1)
SF 1 2 1 1
I, II = phases rich in components 1
C /C C /C
1
II II
2 2
I II
2 and 2 respectively.

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 Selecting Separation Method (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 /x K P s

SF 1

1
for ideal VLE
1 1

(7.2)
y /x K P
1, 2 s

2 2 2 2

Relative Volatility
1, 2

P vapor pressure of species 1

1
s

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 Selecting Separation Method (3)

For vapor-liquid separation operations that involve a non-ideal

liquid solution (e.g. extractive distillation):

1LP1 s
SF 1,2 (7.4)
2LP2s
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, b, where:

1II / 2II
SF b1,2
1I / 2I (7.5)

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. i.e
MSA could enhance the SF.

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 Relative volatilities for equal cost separators

Ref: Souders (1964)

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 Absorption, Stripping, Distillation
Should consider packed column if
Operate under vacuum
Corrosive system
Foaming system
Low liquid hold-up desired
2 type of packing: Structured or Random
Structured packing (more expensive, low P, high
efficiency, large capacity)

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 Absorption, Stripping, Distillation
Should consider tray column if
Large-diameter column (>3 ft)
Feed containing solid
High liq-to-gas ratio
Operate at wide range condition
Various types of tray to choose;
Sieve tray (cheap, low DP, but narrow operating
range
Bubble-cap (most expensive, preferred for high liq
hold-up)
Valve tray is generally most flexible

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 Sequencing of Ordinary Distillation Columns

Use a sequence of ordinary distillation (OD) columns to

separate a multicomponent mixture provided:
SF (or Rel. Vol.) in each column is > 1.05.
The reboiler duty is not excessive. Watch for LK with high latent heat
of vap.
The tower pressure does not cause the mixture to approach the TC
of the mixture.
Column P drop is tolerable, particularly if operation is under
vacuum.
The overhead vapor can be at least partially condensed at the
column P to provide reflux without excessive refrigeration
requirements.
The bottoms T 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

PD : Dist P
Assume cooling water available at 90oF
PB: Bottom P
PB=PD+10psia

End

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 Ordinary Distillations (ODs)
with 3 products

How many possible sequence of ODs?

Note: A product not necessarily have to be a pure component.
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 Number of Sequences for Ordinary Distillation

Equation for number of different sequences of ordinary

distillation (OD) columns, NS, to produce P products:

[2(P 1)]!
Ns (7.9)
P ! (P 1)!

P # of Separators Ns
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: Sequences for 4-component separation (4 products)

Direct sequence
-All final products but one are distillates.
-Widely used in industry as distillates are more
free of impurities (e.g. solids).

Indirect sequence
-All final products but one are bottoms products.
-Least desirable in industry as difficult to achieve
specified purity.

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 5 possible Sequences for 4-component separation (4 products)

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 Determine The Best Sequence OD
For mixture with wide distribution of
concentration or wide variation of volatility,
use direct sequence.
or do detail design and costing for all
sequences! but this is possible only for
number of product is small (< 4).
Otherwise, use heuristics to reduce the
number of sequences for detailed
examination
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 Identifying the Best Sequences using Heuristics

The following guidelines are often used to reduce the number

of OD sequences:
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 distillates
and bottoms in each column. The reboiler duty is not excessive. (especially
if energy cost high)

You will likely end up with more than one sequences for further examination.
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 Class Exercise: Paraffin Separation

Question:
Use heuristics to det. a
sequence of OD columns to
meet the given specifications.

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 Variation of range of relative volatility and also
wide variation in molar percentage
1st column should separate C3 , the most
volatile (Heuristics 4 and 2)
Note most difficult splits are iC4/nC4 and
iC5/nC5 (Heuristics 4), so two separate
columns for these separation
2nd column should be for separation of nC4
and iC5 as LK and HK respectively.
The resulting sequence is as follows,
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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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