Aspen Hysys Azeo Distillation With LL Extractor PDF

Azeo Distillation with LL Extractor
Azeo Distillation with LL

Extractor
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Workshop
An azeotropic mixture of Benzene and Cyclo-Hexane is to be separated
in a distillation column using Acetone as the entrainer. Nearly pure
Benzene is produced from the bottom of the column, while a near
azeotropic mixture of Acetone and Cyclo-Hexane is produced
overhead. The overhead mixture will be separated in a Liquid-Liquid
extractor using water as the solvent, with Cyclo-Hexane being
recovered as the overhead product. The Acetone/Water mixture will
then be separated in a vacuum tower with the Acetone and Water
products being recycled through the flowsheet.
The process will be separated into four sections, the Azeotrope tower,
the Liquid-Liquid extractor, the Solvent Recovery tower and finally the
recycling system.
The problem could be solved with a single set of interaction

parameters. However, the problem may be solved more accurately by
using one set of binary coefficients which will predict the liquid phase
splitting in the Extractor, and another set which will predict VLE
behaviour in the Distillation Columns.
Learning Objectives
Once you have completed this section, you will be able to:
Import Fluid Packages

Model Azeotropic Distillation Columns
Model Liquid-Liquid Extraction Columns
Process Overview
Azeotropic Distillation Column
Solvent Recovery Tower
Building the Simulation

Defining the Simulation Basis
Two Fluid Packages will be used in this example. Both Fluid Packages
will use the UNIQUAC Activity Model, and contain the components
Benzene, Cyclohexane, Acetone and H2O. The first Fluid Package (VLEBASIS), will use the default library VLE binary interaction parameters
and UNIFAC estimated parameters. The second Fluid Package (LLEBASIS), will replace those interaction coefficients with UNIFAC LLE
estimated binary coefficients and those regressed from HYSYS
Conceptual Design Application.
1.
2.
Add the first Fluid Package in the usual manner and change the
default name to VLE Basis.
On the Binary Coeffs tab, view the binary coefficients for the
UNIQUAC activity model.
The binary coefficients for the Cyclohexane/Water pair are not

available from the database, so it is necessary to obtain them by
estimation or from another source.
In this example, the binary coefficients for the Cyclohexane/Water pair
in the VLE Basis will be estimated by the UNIFAC VLE estimation
method. Press the Unknowns Only button to estimate this pair.
The second Fluid Package (for the Liquid-Liquid Extractor) will be
imported.
Ensure that VLE Basis is the

Default Fluid Package when
you leave the Basis
Environment.
1.
On the Fluid Pkgs tab of the Simulation Basis Manager, press the
Import button and import the Fluid Package LLEBasis.fpk. This
file should be located on the course disk supplied with this
material.
2.
Press the View button to see the new Fluid Package. Go to the
Binary Coeffs tab to view the binary coefficients.
If you examine the LLE Coefficients for VLE Basis and LLE Basis you will
see they are different, because they have been taken from different
sources.
VLE Basis will be used for most of the simulation, while LLE Basis will
be used as the Fluid Package for the Liquid-Liquid Extractor.
Enter the Simulation Environment.
Adding the Feed Stream

1.
Enter the following stream Azeo Feed as follows:
In this cell...
Enter...
Conditions
Stream Name
Azeo Feed
Temperature
77C (170F)
Pressure
101.3 kPa (14.7 psia)
Mass Flow
85 kg/h (190 lb/hr)
Composition - Mass Frac

Benzene
0.518
Cyclohexane
0.482
2.
Enter the stream Acetone as follows:
In This Cell...
Enter...
Conditions
Stream Name
Acetone
Temperature
55C (130F)
Pressure
101.3 kPa (14.7 psia)
Mass Flow
95 kg/h (215 lb/hr)
3.
Enter a mass fraction of 1.0 for Acetone.
Azeotrope Tower
Published documentation on this process indicates that the overhead
composition from the Azeotrope Tower is a near azeotropic mixture of
Acetone and Cyclohexane. Using less Acetone than is necessary to
produce the azeotrope will prevent the original Benzene/Cyclohexane
azeotrope from being separated.
The Binary extension is

available on our website.
www.aeat.software.com
The flow of Acetone required to separate this azeotrope and produce a

mixture near azeotropic Cyclo-Hexane/Acetone, can be calculated
from the azeotrope composition, (0.688 Acetone and 0.312 CycloHexane mass fractions). These values can be obtained through HYSYS
Conceptual Design Application or the HYSYS Extension Binary Plots.
The T-x-y diagrams for the Benzene/Cyclo-hexane and Acetone/Cyclohexane binaries are shown here:
Calculation for Required Acetone Flow

Then, for an initial mass flowrate of the Azeo Feed stream of 85 kg/h
with the given composition, the amount of Acetone required will be
90.34 kg/h (85*0.482*0.688/0.312). A slightly greater flow will be used
(95 kg/h {210 lb/hr}) to ensure separation of the Benzene/Cyclohexane
azeotrope.
Adding the Azeotropic Distillation Column

1.
Insert a Distillation Column with the following data:
In This Cell...
Enter...
Connections
Column Name
T-100
No. of Stages
28
Condenser Energy Stream
Q-Cond
Inlet Streams
Azeo Feed, Stage 6

Acetone, Stage 21
Condenser Type
Total
Overhead Liquid
Azeo Liq
Bottoms Liquid Outlet
Benzene
Reboiler Energy Stream
Q Reb
Pressures
Delta P
Condenser
95 kPa (13.75 psia)
Reboiler
101.3 kPa (14.7 psia)
Temp. Estimates
Condenser
55C (130F)
Reboiler
80C (175F)
Specifications
Because we expect an
azeotrope to be present in this
column, we must check the
Azeotropic box on the Solver
page.
Benzene Recovery in Reboiler
0.998
Acetone Recovery in Cond
0.998
Reflux Ratio (Estimate)
10.0
Azeo Liq Draw (Estimate)
130 kg/h (285 lb/hr)
2.
On the Parameters tab, Solver page, check the Azeotropic box

and supply a Fixed Damping Factor of 0.5.
3.
Run the column.
10
The Liquid-Liquid Extractor

Liquid-liquid extraction is used as an alternative to distillation in
situations where distillation is either ineffective or very difficult. These
situations can be found in all process industries. The extraction of
penicillin from fermentation broth and the extraction of aromatics
from lube oil fractions are two industrial examples. Extraction based on
chemical differences is sometimes preferable to distillation, which is
separation based on relative volatilities. Some examples of situations
when extraction is preferred are listed below:
Excessive amounts of heat are required for distillation - relative

volatility of the components is near one
Separation via distillation is limited due to the formation of
azeotropes
The high temperatures of distillation cannot be withstood by the
components, even under vacuum conditions
There are only small amounts of solute in the feed solution
The components to be separated are extremely different in
nature
Extraction involves the separation of a solute from a feed solution by
mixing in a solvent in which the solute is preferentially soluble. In
addition, the solvent must be insoluble, or have a limited solubility in
the feed solution. The extraction operation, on a stage by stage basis,
can therefore be discussed in terms of two processes:
The mixing of a feed solution, a solvent, and any external feeds

The separation of the two immiscible liquid phases which result
from the mixing
HYSYS models the liquid-liquid extraction process using countercurrent flow in a column similar to the absorber template.
10
Property Package
The Liquid-Liquid Extractor cannot be used with the following property
packages:
Use only property packages

that support 2 liquid phases.
Wilson
Antoine
BraunK10
Esso Tabular
Steam
Amine
Chao-Seader
Grayson-Streed
Sour PR
Sour SRK
Activity Models are recommended for most applications.
Overhead Estimate
You will not be required to provide an estimate for the Overhead
Product Flow. The Extractor will generate an estimate from a mole
weighted TP-Flash of the combined tower feeds.
Column Sizing Utility

The column sizing utility in HYSYS is designed for columns with vapour
and liquid traffic; therefore, it is not applicable to the Extractor unit
operation.
Stage Efficiencies
The HYSYS Extraction algorithm models the Extractor as a staged
tower, allowing you to specify either ideal stages or actual stages with
efficiencies.
Side Draw
If you require a Side Draw on the Extractor, you can choose to draw
either the Light or Heavy phase from a stage. HYSYS will perform a
three phase flash on the entire contents of the stage to produce the
conditions and composition of the specified draw.
11
11
12
The purpose of the Liquid-Liquid Extractor is to determine the required

solvent flow (in this case water) which will cause a mixture to phase
split, forming two liquid phases. A rough estimation of the solvent flow
can be obtained by using a Mixer, and then examining the phase
separation while varying the solvent flow. However, because the
extractor is divided into stages, the flow determined can only be used as
an estimate. Use a flow of 200 kg/h (440 lb/hr) of Water.
1.
Enter the following data for the stream Water:
In This Cell...
Enter...
Conditions
Stream Name
Water
Temperature
25C (77F)
Pressure
101.3 kPa (14.7 psia)
Mass Flow
200 kg/h (440 lb/hr)
Mass Fraction H20
1.0
12
2.
Add the Liquid-Liquid Extractor with the following data:
In this cell...
Enter...
Connections
The Temperature Estimates for

Stages 2-19 can be supplied on
the Parameters tab, Profiles
page of the column property
view.
Column Name
T-101
No. of Stages
20
Top Stage Inlet
Water
Bottom Stage Inlet
Azeo Liq
Ovhd Light Liquid
CycloC6
Bottoms Heavy Liquid
Rich Solv
Pressures
Top Stage
101.3 kPa (14.7 psia)
Bottom Stage
101.3 kPa (14.7 psia)
Temperature Estimates
Top Stage
25C (77F)
Stages 2-18
25C (77F)
Stage 19
28C (82F)
Stage 20
33C (91F)
3.
On the Parameters tab, Profiles page, supply an estimate of

48 kg/h (105 lb/hr) for the overhead light liquid.
13
13
14
4.
Go to the Basis Environment and select LLE Basis as the Fluid

Package for the Liquid-Liquid Extractor. Return to the Simulation
Environment.
5.
Run the column.
14
Adding the Solvent Recovery Tower

The Solvent Recovery tower, which separates the Acetone from the
Water, presents a difficult separation at atmospheric pressure. To keep
the number of stages reasonable, an overhead pressure of 53 kPa will be
used. (Once again the data was obtained from HYSYS Conceptual
Design Application).
1.
Add the Solvent Recovery Tower as a Distillation Column with

the following data:
In This Cell...
Enter...
Connections
Column Name
T-102
No. of Stages
20
Inlet Streams
RichSolv, Stage 17
Condenser Type
Total
Overhead Liq
AcetRich
Bottoms Liquid Outlet
H2O Rich
Condenser Energy Stream
RecCond Q
Reboiler Energy Stream
RecReb Q
Pressures
Condenser Pressure
53 kPa (7.75 psia)
Reboiler Pressure
56 kPa (8 psia)
Temperature Estimates
Condenser
35C (95F)
Reboiler
80C (175F)
Specifications
Reflux Ratio
Acetone Recovery (Cond)
0.9998
2.
Supply a Damping Factor of 0.8.
3.
Run the column.
15
15
16
Solvent Recycles
Finally, the two products from the Solvent Recovery tower have to be
recycled to the previous two towers. Because of the temperature and
pressure of the Solvent Recovery tower, each recycle stream will require
a Pump and a Cooler/Heater operation to return the stream to the
necessary tower conditions.
Add a Pump
Add a Pump to the stream H2O Rich with the following information:
In This Cell...
Enter...
Connections
Name
P-100
Inlet
H2O Rich
Outlet
H2O Atm
Energy
Q 100
Parameters
Adiabatic Efficiency
75%
The pressure of stream H2O Atm is 101.3 kPa (14.7 psia).
16
Add a Cooler
Add a Cooler downstream of P-100 with the following information:
In This Cell...
Enter...
Connections
Name
E-100
Inlet
H2O Atm
Energy
Q102
Outlet
H2O Cool
Parameters
Delta P
0 kPa
The temperature of stream H2O Cool is 25C (77F).
17
17
18
Add the Second Pump

Add another Pump from the T-102 product with the following
information:
In This Cell...
Enter...
Connections
Name
P-101
Inlet
Acet Rich
Outlet
Acet Atm
Energy
Q 101
Parameters
Adiabatic Efficiency
75%
The pressure of Acet Atm is 101.3 kPa (14.7 psia).
Add a Heater
Add a Heater operation downstream of Acet Atm with the following
information:
In This Cell...
Enter...
Connections
Name
E-101
Inlet
Acet Atm
Energy
Q 103
Outlet
Acet Warm
Parameters
Delta P
0 kPa
The temperature of Acet Warm is 55C (130F).
18
Adding the Recycles

Make-up streams are necessary to compensate for the losses of Acetone
and Water in the process product streams. To calculate the exact
amount that is lost in the products, Balance operations are used. These
are not real operations but only mathematical ways of obtaining the
make-up values.
A Mole Balance operation will be used to create two streams (Rec Acet
and Rec Water) with the same flowrates and compositions as the tower
product streams Benzene and CycloC6, respectively.
These streams are then sent to a Component Splitter and split into two
streams: one containing the product and the other containing traces of
the lost solvent.
The streams containing the lost solvents are the make-up streams
which will be mixed with the recycled streams from the solvent
Recovery Tower.
19
19
20
Add the Balance Operations

Add two Balance operations with the following data:
In This Cell...
Enter...
Connections
Name
BAL-1
Inlet Streams
Benzene
Outlet Streams
Rec Acet
1.
2.
On the Parameters tab, specify the Balance Type as Mole.

Specify the Temperature and Pressure of Rec Acet to be 55C
(130F) and 101.3 kPa (14.7 psia).
3.
Add the second balance operation with the following

information.
In This Cell...
Enter...
Connections
Name
BAL-2
Inlet Streams
CycloC6
Outlet Streams
Rec H2O
1.
2.
On the Parameters tab, specify the Balance Type as Mole.

Specify the Temperature and Pressure of Rec H2O to be 25C
(77F)and 101.3 kPa (14.7 psia).
20
Add the Component Splitters

Add two Component Splitters with the following information:
In This Cell...
Enter...
Connections
Name
X-100
Inlets
Rec H2O
Overhead Outlet
H2O Make-up
Bottoms Outlet
Frac CycloC6
Parameters
Overhead Pressure
101.3 kPa (14.7 psia)
Bottoms Pressure
101.3 kPa (14.7 psia)
Splits
Benzene
CycloC6
Acetone
1.0
H2O
1.0
Specify the temperature of one of the product streams to be 25C

(77F). The temperature in the other stream will be calculated from the
energy balance around the operation.
21
21
22
In This Cell...
Enter...
Connections
Name
X-101
Inlets
Rec Acet
Overhead Outlet
Acet Make-up
Bottoms Outlet
Frac Benzene
Parameters
Overhead Pressure
101.3 kPa (14.7 psia)
Bottoms Pressure
101.3 kPa (14.7 psia)
Splits
Benzene
CycloC6
Acetone
1.0
H2O
1.0
Specify the temperature of the product streams to be 55C (130F).
22
Add the Mixer Operations

Add two Mixer operations with the following information:
In This Cell...
Enter...
Connections
Name
Inlets
MIX-100
Acet Warm
Acet Make-up
Outlet
Acet to Rec
Connections
Name
MIX-101
Inlets
H2O Cool
H2O Make-up
Outlet
H2O to Rec
23
23
24
Add the Recycles

The input for the recycles is shown below. Note that because of the
nature of the process, the Flow Tolerance is set to 1 and the
Composition Tolerance is set to 1. The Recycles are installed as
Simultaneous. Put the case in Hold mode before adding the recycles.
In This Cell...
Enter...
Connections
Name
RCY-1
Inlet
H2O to Rec
Outlet
Water
Parameters
Vapour Fraction
10.0
Temperature
10.0
Pressure
10.0
Flow
1.0
Enthalpy
10.0
Composition
1.0
Connections
Name
RCY-2
Inlet
Acet to Rec
Outlet
Acetone
Parameters
Vapour Fraction
10.0
Temperature
10.0
Pressure
10.0
Flow
1.0
Enthalpy
10.0
Composition
1.0
24
Press the Go button to begin calculations.

Having completed the recycles and converged the whole flowsheet,
operations can be opened again in order to be examined.
Save your case!
25
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Azeo Distillation with LL Extractor

Azeo Distillation with LL

2000 AEA Technology plc - All Rights Reserved.

Azeo Distillation with LL Extractor

The problem could be solved with a single set of interaction

Import Fluid Packages

Azeo Distillation with LL Extractor

Azeotropic Distillation Column

Solvent Recovery Tower

Azeo Distillation with LL Extractor

Building the Simulation

The binary coefficients for the Cyclohexane/Water pair are not

Ensure that VLE Basis is the

Azeo Distillation with LL Extractor

Adding the Feed Stream

Enter the following stream Azeo Feed as follows:

101.3 kPa (14.7 psia)

85 kg/h (190 lb/hr)

Composition - Mass Frac

Enter the stream Acetone as follows:

101.3 kPa (14.7 psia)

95 kg/h (215 lb/hr)

Enter a mass fraction of 1.0 for Acetone.

Azeo Distillation with LL Extractor

The Binary extension is

The flow of Acetone required to separate this azeotrope and produce a

Azeo Distillation with LL Extractor

Calculation for Required Acetone Flow

Azeo Distillation with LL Extractor

Adding the Azeotropic Distillation Column

Insert a Distillation Column with the following data:

Condenser Energy Stream

Azeo Feed, Stage 6

Bottoms Liquid Outlet

Reboiler Energy Stream

95 kPa (13.75 psia)

101.3 kPa (14.7 psia)

Benzene Recovery in Reboiler

Acetone Recovery in Cond

Reflux Ratio (Estimate)

Azeo Liq Draw (Estimate)

130 kg/h (285 lb/hr)

On the Parameters tab, Solver page, check the Azeotropic box

Run the column.

Azeo Distillation with LL Extractor

The Liquid-Liquid Extractor

Excessive amounts of heat are required for distillation - relative

The mixing of a feed solution, a solvent, and any external feeds

Azeo Distillation with LL Extractor

Use only property packages

Activity Models are recommended for most applications.

Column Sizing Utility

Azeo Distillation with LL Extractor

The purpose of the Liquid-Liquid Extractor is to determine the required

Enter the following data for the stream Water:

101.3 kPa (14.7 psia)

200 kg/h (440 lb/hr)

Mass Fraction H20

Azeo Distillation with LL Extractor

Add the Liquid-Liquid Extractor with the following data:

The Temperature Estimates for

Top Stage Inlet

Bottom Stage Inlet