ACBPD Lecture6 2017

Lecture 6: Separation process design, sizing & selection
Chapters 4, 7 (Textbook) plus additional material*

• Part-1: Introduction
• Part-II: Two-phase (equilibrium) separations
• Part-III: Separation of azeotropic mixtures
• Part-IV: Other separation processes
• See also ”Separation Process Principles” by Henley, Seader & Roper
Chapters 7, 11 & 13 of book for distillation & absorption, and
chapter 14 for membrane based separation
Course: Process Design Principles & Methods, L6 PSE for SPEED, Rafiqul Gani 1
Downstream Separations: The main issues
• When is separation necessary?

• What are the mechansims of separation?
• Which mechanisms and how many need to employed to
achieve a desired separation?
• How to configure/select/design the separation tasks?
• How to verify if the desired separation can be achieved?
This lecture will provide a quick overview of the above topics – more
details can be found in courses on separation process principles
When is separation necessary?
N2
N2, Argon H2
Crude
separation … Reactor NH3
processes
Argon
H2, Methane
Methane
Crude Oil Oil products
Separating Recovery &

different oil purification of
products from chemicals
crude oil (products)
Two Examples
Downstream Separation in Chemical Process Design - I
Chemical processes without reaction
Extraction Recovery Purification Finishing
• Crude oil based refinery for gasoline, and other fuel products
• Seeds and other biomass based edible oil extraction processes
• Herbs, plants based extraction of specialty chemicals
• ...........
Downstream Separation in Chemical Process Design - II
EL, Pl, M recycle
EL, Pl, M
EL, Pl, M
DEE
Reactor Separation
W EA
Waste
Water recycle
Identify and design the sequence of separation tasks that need to be performed
in order to recover and purify the products, recycle the reactants and purge the
inerts that enter the process
Which mechanisms of separation?
Phase 1 Phase 1 Phase 1
Feed Phase Feed Feed Barrier

Creation
(b)
(a) MSA (c)
Phase 2 (Solvent) Phase 2 Phase 2
Feed Phase 1
Phase 1
Feed Force field
or gradient
(d) Phase 2 (e)

Phase 2
a) Phase Creation (eg, distillation); b) Agent-based separation (eg,

extraction); c) Barrier (eg, pervaporation; filtration); d) Solid agent
(eg, adsorption); e) Force field or Gradient (eg, ion-exchange;
centrifuge)
How many mechanisms and which mechanisms?
A, B, C, D, E, F • Depends on how many

chemicals need to be
separated (NS)?
A, E, F / C, D, B • Minimum number of
A / B, C, D, E, F
separation tasks is NS-1
•For each separation task,
A, F / F C / D, B find the appropriate
separation mechanism
• Analyze mixture to be separated (collect data or predict behaviour)

• Identify relation between mechanism and system property (separation
principles)
• Generate and test alternatives (select, design, verify)
How to configure separation tasks? - Distillation Trains
Separation of propane (A), i-butane (B), butane (C), i-pentane (D),
pentane (E) A B
Secondary Separation Efficiencies at P=1 atm.
0.3
B/C
A
B
0.25 C
A/B D
E
0.2
C
Propane iButane
C/D
SSE
iButane nButane
0.15
iPentane nButane D
nPentane iPentane
0.1
0.05
0 D/E
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
E
Liquid composition, mole fractions of the lightest compounds
• Order the driving force diagrams in terms of fij| max = abs(yi – xi);
• Configure the distillation train in terms of fij| max (easiest separation first –
largest driving force equivalent to minimum energy);
• Design each distillation column such that it uses the maximum driving
force (note: only 4 separation tasks A-B; B-C; C-D; D-E)
How to configure separation tasks? – Extraction plus recovery
Main Features:
• Extraction (2-liquid
phases); use of
solvents
• Recovery of solvents
& solute (requires
energy for VL
separation)
• Other forms of
extraction could be
membrane-based, ion-
exchange, etc., that
does not require the
recovery step) 9
Part-II: Two-phase (equilibrium)
separations: Design issues
2-phase VLE based separation: design degrees of freedom?
Vapor, V
T, P
Feed, Z
Liquid, L
Typical 2-Phase VLE-Model

Equilibrium relation xi gi jisat Pisat = yi jiVP i = 1,2,….c
Condition Si xi = Si yi = Si zi = 1
Mass Balance Z zi = V yi + L xi i = 1,2,….c
Degree of Freedom Analysis F = c - p +2
For p = 2, F = c. There are 2c+3 Equations and 3c + 5
variables (not counting gi , ji , Pisat ). Therefore, c + 2
variables need to be specified. For example, specify Z, T, P
and (c-1) z compositions.
Some Definitions
Equilibrium Constant (VLE) Ki = yi/xi
•Ideal System Ki = Pisat (T) / P
•Non-ideal Liquid & Vapor Ki = gi jisat Pisat /( jiVP)
•Non-ideal Liquid, ideal vapor Ki = gi Pisat /P
•Any P & T Ki = j iL / j iV
Relative volatility ij = yj xi / (xj yj) = Pisat/Pjsat

Rewriting in terms of yi yi = xi ij/[1+ xi(ij - 1)]
Driving Force Dij = yi - xi

Rewriting in terms of yi Dij = xi ij/[1+ xi(ij - 1)] - xi
Binary systems with different volatility
0.30 Distillation, 1 atm.

Distillation, 5 atm.
Pervaporation
0.25 Extractive distillation
Driving Force, FDi

0.20
0.15
0.10
0.05
0.00
0.0 0.2 0.4 0.6 0.8 1.0
Liquid composition, xi
DX-(PT) phase diagram (in

XY-(PT) phase diagram (in terms of driving force) – shown
terms of relative volatility) for different separation types)
VLE based separation: Model w.r.t. ij or Dij
Vapor, V
T, P
Feed, Z
Liquid, L
Typical 2-Phase VLE-Model

Equilibrium condition yi = xi ij/[xi (ij - 1) + 1] w.r.t. relative volatility
or (eq.1) Dij = xi ij /[xi (ij - 1) + 1] - xi w.r.t. driving force
Mass Balance Z zi = V yi + L xi i = 1,2,….c

or yi = (R + 1) zi – R xi where R = L/V
or (eq. 3) Dij = (R + 1) (zi –xi)
Graphical calculation technique for V-L based separation
Dij = yi - xi = xi ij / (1 + xi (ij - 1)) - xi
Dij = (R+1)(zi – xi)
When Dij = 0, there is no separation and zi = xi

When xi = 0 or L= 0; R= L/V= 0 & Dij = yi - xi = zi (everything is vaporized)
When R = specified; xi = Dij /(R + 1) + zi (point of intersection of Eqs. 1 & 3)
Visualization of 2-phase separations: P-XY & T-XY diagrams
P-xy diagram at constant T T-xy diagram at constant P
Dew point
L A C
V&L
B V
A
V&L
C B Bubble point
V
L
x1 and y1 x1 and y1
For a feed at C, L/V = CB/AC; at constant T, if you compress a vapor you

get a liquid and vice versa. At constant P if you heat a liquid you get a
vapor and vice versa. If you have a feed mixture in the 2-phase (V&L)
region, it will split into a liquid and a vapor
VLE - Binary Systems: Azeotropic systems
Ethanol - Water Methanol - Toluene
y1 y1
x1
x1
XY-PT phase diagrams. At the azeotrope, xi= yi,
therefore, Ki=1 and/or ij = 1. Separation beyond the
azeotropic point is not possible
Visualization of 2-phase separations: azeotrope systems
T
P
x1, y1 x1, y1
Methanol-Toluene T-xy & P-xy diagrams

Generate these diagrams as a function of P to see if the location
of the azeotrope can be moved
Types of VLE-phase separation models & solution approaches
Problem Specification Isothermal flash: fast solution
Isothermal flash (T, P, F, z) Specified: F, z1, z2, ..zc-1, T, P
*Bubble-point T (P, x) Solve for  = V/F with fixed Ki
*Dew-point T (P, y) 1. Calculate Ki = Pisat(T)/P
*Bubble-point P (T, x) 2. f = Si zi(1-Ki)/[1+ (Ki-1)] = 0
*Dew-point P (T, y) 3. V = F ; L = F - V
Adiabatic flash (Q=0, P, F, z) 4. xi = zi / [1+ (Ki-1)]
Non-adiabatic flash (Q, P, F, z) 5. y = z K / [1+ (K -1)] = x K
i i i i i i
% Vaporization (V/F, P) 6. Q = hV V + hL L – hF F
* Note: Degrees of freedom = c + 1
Separation of Binary Mixtures by Distillation: review
V1
Component Mass Balance
QC Condenser
1
Overall
Recycle, L0 Distillate, D, xD F zF = D xD + B xB
V2 L1
Rectifying section
Feed
VNF LNF-1
F, zF yn+1= Ln/Vn+1 xn + D/Vn+1xD
NF
y = [R/(R+1)] x + [1/(R+1)]xD
VNF+1 LNF Stripping section
VNP LNP-1 ym+1= Lm/Vm+1 xm - B/Vm+1xB
Vapor boilup VNP+1
NP
QR Reboiler y = [(VB+1)/VB] x - 1/(VB+1)]xB
Equilibrium relation
Bottom product, B, xB
yi = xi ij / (1 + xi (ij - 1))
•Equilibrium relation
•yi = xi ij / (1 + xi (ij - 1))
•Component Mass Balance
•Overall
•F zF = D xD + B xB
•Rectifying section
•yn+1= Ln/Vn+1 xn + D/Vn+1xD
•y = [R/(R+1)] x + [1/(R+1)]xD
•Stripping section
•ym+1= Lm/Vm+1 xm - B/Vm+1xB
•y = [(VB+1)/VB] x - 1/(VB+1)]xB
Driving force based design - I
•Given a mixture to be separated into two products in a distillation
column with N trays. What is the optimal (with respect to the costs of
operation) feed plate location and the corresponding reflux ratio for
different product purity specifications ?
0.4
A
A
Pinch point
0.3 Slope correponding
DY D to RRmin
Driving Force, FDi
Slope correponding I
to RR > RRmin
I
0.2 D'
D D’ NF
Dx NF = N(1-Dx)
0.1 II II
A DX F ' F B
X X
0.0 B
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
B
Light compound composition, x i
Relation between ij, Dij(max), Xi (max)
0.6 0.6
Xi Max
0.5 Max FDi 0.5
0.4 0.4
Xi Max
Max FDi
0.3 0.3
0.2 0.2
0.1 0.1
0.0 0.0
0 2 4 6 8 10 12
Alfa (Constant)
Identification of design targets
24
Simple and fast reverse design method
Problem Solution
Driving force based design - II
Part-III: Separation of azeotropic mixtures
(chapter X of textbook, see also chapter 11 of
Seader & Henley book)
Separation of an azeotropic mixture
• Mixture analysis
Identification of an azeotrope.
• Possible separation techniques
Pressure swing.
Extractive/azeotropic distillation.
• Solvent identification and validation
• Flowsheet configuration
Mixture analysis
Whenever you have the problem of separating a mixture, a good starting
point is always to do a mixture anaysis.
This can include both pure component and mixture properties.
The mixture analysis will imediately give information both intuitively
and to a computer aided system on what kind of separation is possible.
Binary Azeotrope:
A binary azeotrope is when a 2 component, 2 phase system of gas and liquid in
chemical equilibrium has the same composition in both phases.
Azeotropic condition: Gas phase, composition: ya, yb

xa = ya, xb = yb
Liquid phase, composition: xa, xb
Identification of an azeotrope
Azeotropes is found by VLE (Vapor-Liquid Equilibria) mixture
analysis.
This can be either database lookup for VLE datapoints or the
datapoints can be calculated with a thermodynamic model.
Comp A 1
By the definition of an azeo-

trope, in a x-y plot the curve
y
crosses the diagonal, at the
azeotrope composition.
0
0 x 1
Comp A
Possible separation techniques
Conventional distillation not possible, if 2 pure products are desired.
Possible solutions to this problem:

• Use separation techniques which are not exploiting
differences in vapor vs. liquid phases, i.e. membranes or liquid-
liquid extraction.
• Pressure swing.
• Extractive / azeotropic distillation.
Acetone - chloroform
VLE-PhaseDiagram: Pres.= 1.00 atm VLE-PhaseDiagram: Pres.= 1.00 atm
ACETONE
Temperature (°C)
100
64
90
ACETONE
80 62
70
60
mole %
60
58
50
40 56
CHCl3
30
54
20
52
10
0 50
0 20 40 60 80 100 0 20 40 60 80 100
CHCl3 mole % ACETONE
CHCl3 CHCl3 ACETONE
Azeotrope ~ 38 mole% acetone, 64.5 °C, maximum boiling
Pressure swing
Pressure swing distillation is exploiting the fact that for
some azeotropes the composition changes with pressure
VLE- PhaseDiagram: Pres.= 1.00 atm VLE-PhaseDiagram: Pres.= 6.00 atm
CH3-ACETATE
CH3-ACETATE
100 100
CH3-ACETATE CH3-ACETATE
80 80
mole %
mole %
60 60
40 40
METHANOL
METHANOL
20 20
0 0
0 20 40 60 80 100 0 20 40 60 80 100
METHANOL mole % CH3- ACETA TE METHANOL mole % CH3-ACETATE
METHANOL METHANOL
System: methanol – methyl acetate

Extractive distillation
The addition of a third component (solvent/entrainer) to the
binary system in order to facilitate the separation by distillation.
VLE-PhaseDiagram: Pres.= 1.00 atm solvent mole %
ACETONE
100 Vapour
Diagonal
90 Vapour 60.0
ACETONE
80
70
60
mole %
50
40
30
20
CHCl3
10
0
0 20 40 60 80 100
CHCl3 mole % ACETONE
CHCl3
Hybrid Separation: Driving force
Secondary Separation Efficiency, Methanol MTBE
0.30 Solvent based

separation
0.25
0.20
ABS(yi-xi)
0.15
Pervapo- 0.10
Distillation
ration column 1
0.05
0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
Liquid Composition, Mole Fraction Methanol
Column 2 at P2 Column 1 at P1
Separation by single distillation operation not feasible;

hybrid separation schemes (solvent based extraction or
distillation plus pervaporation or pressure swing
distillation) feasible
Solvent identification (I)
The solvent can be found in a solvent database or by the use
of a computer tool.
The computer tool must be able to solve the following problem:

Given: A set of desired properties (pure and mixture)
Needed: Description of compounds with these properties
Computer Aided Molecular Design (CAMD) programs can solve

this.
General functionality:
1. Combine molecular fragments to describe complete molecules
2. Predict the properties of the molecular descriptions
3. Reject descriptions with undesired properties
Solvent identification (II)
Desired properties for the entrainer:
1. If it is a minimum boiling azeotrope the boiling point of
the entrainer should be lower than the azeotropic
temperature and vice versa.
2. The boiling point should not be to high in order to have
small energy consumption.
3. Should not be harmful to the environment.
4. Should not form azeotropes with any of the two
compounds.
g jS
5. High selectivety: Ss  
g iS
1
6. Low solvent loss: Ssv.L 
g sJ
7. ...
Solvent validation (I): Identify distillation boundaries
1-PROPANAL
( 321.5 K)
1.0
0.9
Azeotrope
0.8
0.7
0.6
0.5
Residue curve
0.4
0.3
0.2
Distillation boundary
0.1
0.0
( 331.0 K) 0.0
0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0( 338.0 K)
METHYL-ACETATE METHANOL
328.1 K
Solvent validation (II): Separation feasibility
1-PROPANAL
( 321.5 K)
1.0 D2
0.9
Azeotrope
0.8
0.7
0.6
0.5 D1, Feed 2
0.4
Feed 1
0.3
0.2
0.1
B2 B1
0.0
( 331.0 K) 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0( 338.0 K)
328.1 K
Solvent validation (III): Flowsheet configuration
D2
1-PROPANAL
( 321.5 K)
1.0 D2
D1
0.9
Azeotrope
S2
0.8
0.7
D3
0.6
mixer S1
0.5 D1, Feed 2
0.4
Feed 1
B2
S3
0.3
B1
0.2
0.1
B3 B2 B1
0.0
( 331.0 K) 0.0 0.1 0.2
D3 B3
0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0( 338.0 K)
328.1 K
Another flowsheet configuration: High boiling azeotrope
How to identify feasible configurations & design?
4
feed
3
2 5
1
Identify the azeotropes, determine the distillation boundaries,

generate the residue curves, design and analyze the separation
scheme
Other flowsheet configurations
For different types of

ternary diagrams, the Solvent
flowsheet can be fixed in
A, Solvent
advance, consisting of
minimum two
distillation columns.
What kind of distillation
boundary and residue A, B, Solvent
curves are needed to get A
the flowsheet shown on
the right?
B
Part-IV: Other separation processes
Graphical Design Technique
Draw the ternary LLE
diagram
Locate F (feed) & S
(solvent) streams & join
them in a straight line
Locate any point M that
determines the mixing
F point between F and S.
E
M Locate a tie-line that
passes through M. The
R
end-points of the tie-line
S indicates the composition
of E and R streams
Graphical Design Technique for LL-extraction
Modelling and design of counter-current LL-extraction systems
Ternary saturation diagrams at
Binary T-x diagram constant T & solvent-free
Equipment design parameters
(to be covered in next lecture)
• Distillation Column Design - Determine, Reflux ratio,
Number of stages, Column diameter, Tray height, Heat
duties for reboiler & condenser (following the example in
the book)
• Use the lk/hk, lk, hk to calculate Ni & Ri
• Calculate Nt = 0.8 maxi(Ni) + (1-0.8) mini(Ni); use efficiency of 80%
• Calculate R = 0.8 maxi(Ni) + (1-0.8) mini(Ni)
• Calculate L´ and V´ and from it, Flv
• Use Flv and Fig 4.4 to obtain Csb,t (for a selected tray spacing)
• Calculate flooding velocity, Unf, and from it, the area A and
diameter D of the column (use Eqs. 4.7 or 4.8 and 4.9)
• Determine Tray stack height, extra feed space, disengagement
space (top & bottom), skirt height
• Qcond = HV V – hL L
• Calculate Qreboil from total energy balance 52
• Distillation Column Design - Determine, Reflux ratio,
Number of stages, Column diameter, Tray height, Heat
duties for reboiler & condenser (Using PRO-II)
• Use Short-Cut Fractionation (for column design)
• Use rigorous simulation model to obtain the final design
• Use the “sizing” calculation option for the column design
• Select the column diameter, tray spacing, etc., from the output of
PRO-II
• For condenser duty = Qcond (given by PRO-II), size a heat
exchanger (determine area A)
• For reboiler duty = Qreboil (given by PRO-II), size a heat exchanger
(kettle-type) – determine area
• Absorption Column Design - Determine, absorption
factor, Number of stages, Column diameter, Tray height,
Heat duties for reboiler & condenser
• Use the lk/hk, lk, hk to calculate Nt
• Calculate Nt from Kremser equation (approx = 10)
• Use efficiency of 20%
• Calculate L´ and V´ and from it, Flv
• Use Flv and Fig 4.4 to obtain Csb,t (for a selected tray spacing)
• Calculate flooding velocity, Unf, and from it, the area A and
diameter D of the column (use Eqs. 4.7 or 4.8 and 4.9)
• Packed columns can also be calculated from the number of
transfer units and height of transfer units
• Pumps, Compressors, Heat Exchangers, ….
• The sizing parameters for each of these equipments can be
obtained from PRO-II or calculated through the method
used in the book (see the ethanol case study in chapter 4)
• Pump – find the power needed (based on work)
• Compressor - find the power needed (based on work)
• Tank – volume (area and height) based on residence time
• Heat Exchangers – area of the heat exchanger based on U,
T, Q, Flowrate
• …..
•Ethanol Process: Case Study (from Textbook)
•We have now
performed mass and
energy balance.
•We have added
pumps/compressors,
heat exchangers
wherever necessary.
•Now we need to do the
sizing calculations for
all unit operations in
the flowhseet.
•Costing & Economic
analysis
•Sizing & Costing Calculations
• Prepare a list of unit operations found in the flowsheet
• For each unit operation, find a design that matches the
calculated input-output conditions to obtain the sizing
parameters
• Use the sizing parameters to determine the cost of each
unit operation
•Decisions that need to be made
•Choice of equipment type
•Choice of pressure (already made)
•Choice of material
•Other parameters specific to the unit operation

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Lecture 6: Separation process design, sizing & selection

Chapters 4, 7 (Textbook) plus additional material*

• When is separation necessary?

Separating Recovery &

Chemical processes without reaction

Extraction Recovery Purification Finishing

Feed Phase Feed Feed Barrier

(d) Phase 2 (e)

a) Phase Creation (eg, distillation); b) Agent-based separation (eg,

A, B, C, D, E, F • Depends on how many

• Analyze mixture to be separated (collect data or predict behaviour)

Typical 2-Phase VLE-Model

Relative volatility ij = yj xi / (xj yj) = Pisat/Pjsat

Driving Force Dij = yi - xi

0.30 Distillation, 1 atm.

Driving Force, FDi

DX-(PT) phase diagram (in

Typical 2-Phase VLE-Model

or (eq.1) Dij = xi ij /[xi (ij - 1) + 1] - xi w.r.t. driving force

Mass Balance Z zi = V yi + L xi i = 1,2,….c

Dij = yi - xi = xi ij / (1 + xi (ij - 1)) - xi

Dij = (R+1)(zi – xi)

When Dij = 0, there is no separation and zi = xi

For a feed at C, L/V = CB/AC; at constant T, if you compress a vapor you

Methanol-Toluene T-xy & P-xy diagrams

Azeotropic condition: Gas phase, composition: ya, yb

Liquid phase, composition: xa, xb

By the definition of an azeo-

Possible solutions to this problem:

Azeotrope ~ 38 mole% acetone, 64.5 °C, maximum boiling

System: methanol – methyl acetate

0.30 Solvent based

Separation by single distillation operation not feasible;

The computer tool must be able to solve the following problem:

Computer Aided Molecular Design (CAMD) programs can solve

0.5 D1, Feed 2

Identify the azeotropes, determine the distillation boundaries,

For different types of

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