PLANT DESIGN –

SEPARATION
Dr. Aqeel Ahmad TAIMOOR
GAS – GAS SEPARATION
Adsorption

 Irreversible
Adsorption

 Reversible
 Pressure swing adsorption
 Temperature swing adsorption
Membrane Separation
Absorption and Stripping
Economizing the Process
Air Separation – Cryogenic Distillation
Solid – Solid SEPARATION
Screening
Cyclones Classifiers Hydraulic Jigs
Wilfley riffled table
Magnetic Separators Electrostatic Separator
Solid – Liquid SEPARATION
Clarifiers
Filters
Filters
Centrifuges
Tray Dryers Conveyor Dryers Fluidized Bed Dryers
Pneumatic Dryers Spray Dryers Rotary Dryers
 Evaporators
Long Tube Forced Circulation
Crystallizers
Reverse Osmosis – Desalination
Ion Exchange
Liquid – Liquid SEPARATION
Three Phase Separators
Piping and Instrumentation Diagram
Distillation Tower Design Steps

1. Specify the degree of separation required: set product specifications.

2. Select the operating conditions: batch or continuous; operating pressure.
3. Select the type of contacting device: plates or packing.
4. Determine the stage and reflux requirements: the number of equilibrium stages.
5. Size the column: diameter, number of real stages.
6. Design the column internals: plates, distributors, packing supports.
7. Mechanical design: vessel and internal fittings.
Distillation Column Design
Distillation Column Design

 Reflux ratio
 Usually optimum reflux is 1.1 to 1.3 times of minimum reflux ratio
 Pressure is adjusted based on the dew point
Example – Manual

A feed to a column has the composition given in the table below, and is at a pressure
of 14 bar and a temperature of 60 °C. Calculate the flow and composition of the liquid
and vapour phases. Take the equilibrium data from the Depriester charts
Mccabe-Thiele Method – Binary Mixtures

 Yi = Kixi

 q = L/D
 Top line slope = q/(q + 1)
 Bottom line slope = (q + F/D)/(q+1)
Minimum Number of stages – Total Reflux
Example – Manual/Computer Aided Design

Acetone is to be recovered from an aqueous waste stream by continuous distillation.

The feed contains 10 mol% acetone. Acetone of at least 95 mol% purity is wanted,
and the aqueous effluent must not contain more than 1 mol% acetone. The feed will
be a saturated liquid. Estimate the number of ideal stages required.
Starting Equations

 Fenske’s Eq. Minimum number of stages

 Underwood Eq. for minimum reflux

 Theta is the root of the eq

Erbar-Maddox
correlation
Example – Computer Aided Design

100 kmol⋅h−1 of a mixture containing 10, 20, 30, and 40 mol% of propane, n-butane,
n-pentane, and n-hexane, respectively, is preheated before entering a distillation
tower. The liquid mole fraction of the mixture is thus 80%. Calculate the composition
of both liquid and vapor phases and the temperature of the vapor–liquid mixture at
700 kPa. Initial temperature of the mixture is 25 ◦C, and the pressure drop can be
neglected.
Example – Computer Aided Design

Gaseous reactor effluent contains in kmol⋅h−1: styrene (175), ethylbenzene (70),

toluene (55), water (245), methanol (55) and hydrogen (175), in total 775 kmol⋅h−1.
Using Aspen Plus, compute the equilibrium composition and amount of all phases at
35 ◦C and 300 kPa.
Estimate missing parameters by UNIFAC
Short Cut distillation Methods – Multicomponent Distillation

 Fenske equation
 Relative volatility is the geometric mean of the values at top and bottom of the
column
 For minimum Reflux ratio:

 Feed Point Location:

Example – Manual/Computer Aided Design

Estimate the minimum number of ideal stages needed in the butane-pentane splitter
defined by the compositions given in the table below. The column will operate at a
pressure of 8.3 bar. Evaluate the effect of changes in reflux ratio on the number of
stages required.
Example – Manual

Estimate the position of the feed point for the separation at a reflux ratio of 3
Example – Computer Aided Design

A preheated mixture from Problem 1 (stream F) has to be separated in a distillation

tower. The mole fraction of n-propane in the bottom product is 0.05 and that of n-
butane in the distillate is also 0.05. Using the Fenske–Underwood–Gilliland method,
calculate the minimum reflux ratio and the minimum number of theoretical stages
needed. Assuming a reflux ratio 1.5 times higher than the minimum reflux ratio,
calculate the actual number of trays, optimal feed stage, condenser and reboiler
temperature, and distribution of nonkey components into the distillate and bottom.
Consider a uniform pressure in the column of 700 kPa.
External Reflux ratio = 1.5 x Minimum reflux ratio
Rating Calculations – Algorithms Multicomponent Distillation

 Usually the minimum stages are calculated and then tower is rated for initial
problem to optimization
 Linear Algebra Simultaneous Equation Solution
 MESH – Material, equilibrium, summation and heat (enthalpy) balances
Rigorous Distillation Method

 Material balance (M)

 phase Equilibrium (E)
 Summation equations for theoretical stage (S)
 Heat balance (H)
 MESH (material-equilibrium-summation- heat)
 Non linear equations
 Simultaneous two nested solution
 Inside Out distillation Algorithm
 Applicable to ideal and non-ideal distillation
Problem 4

Using the rigorous inside-out method, calculate the dependence between the number
of theoretical stages and the reflux ratio, if the preheated mixture from Problem 1
(stream F) is separated in a distillation tower, the distillate contains 99 mol% of light
components (propane and n-butane) and at the same time common recovery of
propane and n-butane is more than 99%. Use the Full Reflux condenser type and
neglect the pressure drop in the column and heat exchangers.
Problem 5

3.5 kg⋅s−1 of an equimolar binary mixture of n-heptane and toluene is separated by

extractive distillation at atmospheric pressure using n-methylpyrrolidone (NMP) as the
selective solvent. A column with the separation ability of 10 theoretical stages, a total
condenser and a kettle reboiler are used. The boiling point feed with the pressure of
110 kPa enters the eighth stage from the top starting by a condenser. The selective
solvent removes toluene, and they are obtained in the bottom product. Thus, n-
heptane has to be recovered in the distillate (distillate flow rate equals to the mole
flow of n-heptane in the feed). The reflux ratio is 3. Toluene is separated from NMP in
a second atmospheric distillation column with six theoretical stages, where the reflux
ratio is 2.5, and the distillate rate equals to the mole flow rate of toluene in the feed.
The feed enters the middle stage of the column. Using Aspen Plus, calculate the
composition of products from both columns if the NMP mole flow is 630 kmol⋅h−1, its
temperature is 100 ◦C, and pressure is 110 kPa, and it enters to the optimum stage;
find the optimum feed stage for NMP considering the maximum purity of n-heptane in
the distillate product of the first column. Find the dependence of products (n-heptane
and toluene) purity and specific requirement of NMP (kmol of NMP per kmol of feed).
Problem 6

50 kmol⋅h−1 of an azeotropic mixture of benzene and cyclohexane is separated by

azeotropic distillation using acetone. Azeotropic feed enters the column as a liquid–
vapor mixture with the liquid to vapor mole ratio of 1:1 at atmospheric pressure.
Acetone enters the column at 50◦C and atmospheric pressure. Using Aspen HYSYS,
design the distillation process considering maximization of benzene purity and
benzene recovery in the bottom product.
Azeotrope
xbenzene=0.55
xcyhexane=0.45
Problem 7

Reactive distillation is a common method to be used in the ethyl acetate process

described in previous chapters. 60 kmol⋅h−1 of a solution containing 85 mol% of ethanol
and 15 mol% of water enters to the 10th theoretical stage of a distillation column with 12
theoretical stages. Acetic acid stream with the flow of 50 kmol⋅h−1 containing 96 mol% of
acetic acid and 4 mol% of water enters to the eighth theoretical stage. Both inlet streams
enter the column as bubble point liquids at 1 bar. Reactive stages are 8–10, where the
chemical reaction

CH3COOH + CH3CH2OH → CH3COOC2H5 + H2O

takes place in the liquid phase, forming the ternary azeotrope of ethyl acetate, ethanol,
and water, mole flow of the bottom product is set to 30 kmol⋅h−1. Vapor from the column
top is cooled to 25 ◦C and led to a decanter where 120 kmol⋅h−1 of water is added to
create two liquid phases; the aqueous phase is removed from the system. From the
organic phase, 40 kmol⋅h−1 of distillate product is obtained and the remaining part is
returned to the top stage of the column as reflux. Using Aspen Plus, calculate the
composition of products and composition and temperature profiles in the column.
 Reactive Distillation

 Reactive distillation is a term used when a distillation tower is also used as a reactor
 Reactive distillation can be exploited for many applications like
 Azeotrope separation
 Utilizing in-situ heat of reaction
 Increasing yield of equilibrium reaction
 Azeotropic Distillation

Dehydration of ethanol using benzene as entrainer Pressure-swing distillation

Extractive distillation Membrane distillation

 Plate Efficiency
 Murphree Plat Efficiency

 Overall Efficiency
O’Connell’s Correlations – Plate Efiiciency

 Correlations
Example

Using O’Connell’s correlation, estimate the overall column efficiency and the number
of real stages required for the separation given in Example 11.3, when the reflux ratio is
2.0.
Plate Efficiency

 Van Winkle’s Correlation

Entrainment, Weeping and Froth
Column Diameter, Downcomers and Wier

 Correlation:

Vertical apron

Inclined apron

Inlet weir

Recessed well
Truncated
downcomer
Types of Plates
Bubble cap Plate
Sieve Plate Valve Plate
For low vapor rates
Typical Plate Construction
Typical Stacked Plate Column
Sieve Plate Performance
 Plate Hydraulic Design

 Design Velocity is 80 –
85% of the flooding
 Calculate entrainment
with help of charts
 Weep point calculations
 Weir Liquid Height
 Holes / Area
 Holes pitch
 Froth Height
 Final Plate Pressure
drop
 Column Pressure drop
Packed Columns
 Plate columns can be designed to handle a wider range of liquid and gas flow-rates
than packed columns.
 Packed columns are not suitable for very low liquid rates.
 The efficiency of a plate can be predicted with more certainty than the equivalent
term for packing.
 Plate columns can be designed with more assurance than packed columns. Good
liquid distribution throughout a packed column is difficult.
 It is easier to make provision for cooling in a plate column; coils can be installed on
the plates.
 It is easier to make provision for the withdrawal of side-streams from plate columns.
 If the liquid causes fouling, or contains solids, it is easier to make provision for
cleaning in a platecolumn
Packed Columns

 For corrosive liquids a packed column will usually be

cheaper than the equivalent plate column.
 The liquid hold-up is appreciably lower in a packed
column than a plate column.
 Packed columns are more suitable for handling
foaming systems.
 The pressure drop per equilibrium stage can be
lower for packing than plates; and packing should
be considered for vacuum columns.
 Packing should always be considered for small
diameter columns, say less than 0.6 m,
Types of Packing

Raschig rings Pall rings Berl saddle INTALOX® saddle

SUPER INTALOX
Metal HY-PAK
Height of a absorption column

 Correlations:
 Example – Computer Aided Design
To an absorber with 30 stages, 1,970 kmol⋅h−1 of gas with the following composition
(g⋅Nm−3 of gas) enter: methane (594), ethane (112.7), propane (94.45), i-butane (23.34), n-
butane (44.084), i-pentane (12.88), and n-pentane (25.75). As the absorbent, paraffin oil
with the same properties as n-dodecane is used. Molar flow of the absorption oil is 3,000
kmol⋅h−1. Efficiency of the column is 20%. Pressure at the column bottom is 0.51 MPa,
and at the column top it is 0.495 MPa. Temperature of both gas inlet stream and solvent
stream is 32 ◦C. The absorbent is regenerated in a desorber with six theoretical stages.
Using Aspen HYSYS, calculate the composition of the gas and liquid phases leaving the
absorber. Calculate also the amount and composition of gas from the desorber.
Select all plates then
specify the efficiency
Column is not converging
because of tolerance in Specs
Ternary Diagram
Example
Solution
Ternary Diagram
Example
Ternary Diagram
Example
Ternary Diagram

1.57 kg

0.43 kg
Liquid Liquid Extraction
Problem 9

Benzene is extracted from 1,000 kmol⋅h–1 of its solution with heptane (55 mol% of
heptane + 45 mol% of benzene) using dimethylsulfoxide (DMSO). Liquid–liquid
extraction is carried out at 20◦C in a countercurrent extractor with six theoretical
stages. A regenerated solvent used in this process contains 2 mol% of benzene and
98 mol% of DMSO. Calculate the solvent requirement for a 90-mol recovery of
benzene in the extract phase. Determine the amount and composition of the final
extract and raffinate phases.
Problem 10

For the distillation of the hydrocarbon mixture from Example 6.4, select an appropriate
distillation system. Estimate the cost of the unit operations (column, condenser, and
reboiler) when tray or packed columns are used. Compare different tray types (sieve,
bubble, valve) and the cost of the column when packed types 1.0PPR (propylene Pall
rings) and 1.0-CRR (ceramic Raschig rings) are used.