You are on page 1of 71

Dist-009H Revised: Nov 19, 2012

Separation of Acetone-Water with Aspen HYSYS® V8.0


Liquid-Liquid Extraction with 3-Methylhexane as the Solvent

1. Lesson Objectives
 Learn how to build an extraction and solvent recovery flowsheet.
 Learn how to configure a liquid-liquid extractor and a distillation column.

2. Prerequisites
 Aspen HYSYS V8.0

3. Background
Water has a high latent heat (heat of vaporization) compared to many other components. For the separation of
a water-acetone mixture (50 wt-% each), it may be more energy efficient to use extraction instead of direct
distillation. In this example, we utilize 3-methylhexane as a solvent to remove water via liquid-liquid extraction,
followed by distillation to remove the solvent from acetone.

The examples presented are solely intended to illustrate specific concepts and principles. They may not
reflect an industrial application or real situation.

4. Problem Statement and Aspen HYSYS Solution


Problem Statement

Determine how much energy is required to separate a 50 wt-% acetone 50 wt-% water stream using 3-
methylhexane as a solvent.

Aspen HYSYS Solution

4.01. Start a new simulation in Aspen HYSYS V8.0.

4.02. Create a component list. In the Component Lists folder select Add. Add Acetone, Water, and 3-
methylhexane to the component list.

1
Dist-009H Revised: Nov 19, 2012

4.03. Select property package. In the Fluid Packages folder select Add. Select PRSV as the property package.
For information about the PRSV property package see Aspen HYSYS help.

4.04. Move to the simulation environment by clicking the Simulation button in the bottom left of the screen.

4.05. First we will add a Mixer to the flowsheet from the Model Palette. This mixer will serve to mix together
the recycled solvent stream and the solvent make up stream.

2
Dist-009H Revised: Nov 19, 2012

4.06. Double click the mixer (MIX-100). Create two Inlet streams called Make Up and Solvent-Recycle.
Create an Outlet stream called Solvent.

3
Dist-009H Revised: Nov 19, 2012

4.07. Double click on the Make Up stream. Specify a Temperature of 25°C, a Pressure of 1 bar, and a Molar
Flow of 0. We will later assign this stream a flowrate, but for now it will have zero flow. In the
Composition form enter a Mole Fraction of 1 for 3-methylhexane.

4.08. Double click on the Solvent-Recycle stream. Enter a Temperature of 30°C, a Pressure of 1 bar, and a
Mass Flow of 150 kg/h. In the Composition form enter a Mole Fraction of 1 for 3-methylhexane. These
specifications will serve as an initial guess as to what the actual recycle stream will be.

4
Dist-009H Revised: Nov 19, 2012

4.09. Add a Liquid-Liquid Extractor to the flowsheet from the Model Palette.

4.10. Double click on the extractor (T-100) to open the Liquid-Liquid Extractor Input Expert window. On the
first page enter a Top Stage Inlet called Feed and select Solvent for the Bottom Stage Inlet. Change the
number of stages to 8. Enter an Ovhd Light Liquid stream called Rich-Sol and a Bottoms Heavy Liquid
stream called Water. Click Next when complete.

5
Dist-009H Revised: Nov 19, 2012

4.11. On Page 2 of the Input Expert enter Top and Bottom Stage Pressures of 1 bar. Click Next when
complete.

4.12. On the final page of the Input Expert enter a Top Stage Temperature Estimate of 25°C. Click Done
when complete to configure the column.

6
Dist-009H Revised: Nov 19, 2012

4.13. We must now define the feed stream. Go to the Worksheet tab in the Column: T-100 window. For the
Feed stream enter a Temperature of 25°C, a Pressure of 1 bar, and a Mass Flow of 100 kg/h.

4.14. In the Compositions form under the Worksheet tab enter Mass Fractions of 0.5 for acetone and water
in the Feed stream.

7
Dist-009H Revised: Nov 19, 2012

4.15. Click the Run button at the bottom of the Column: T-100 window to begin column calculations. The
column should converge.

4.16. Check the composition of the Water stream exiting the bottom of the column. You will see that the
mole fraction for water is 1.

8
Dist-009H Revised: Nov 19, 2012

4.17. We will now insert a Distillation Column Sub-Flowsheet from the Model Palette.

4.18. Double click the column (T-101) to open the Distillation Column Input Expert. On Page 1 enter the
following information and click Next when complete.

9
Dist-009H Revised: Nov 19, 2012

4.19. On Page 2 of the Input Expert leave the default selections for a Once-through, Regular Hysys Reboiler.
Click Next.

4.20. On Page 3 of the Input Expert enter Condenser and Reboiler Pressures of 1 bar. Click Next when
complete.

10
Dist-009H Revised: Nov 19, 2012

4.21. On Page 4 and 5 leave all fields blank. Click Done on the final page to configure the column.

4.22. We must define the design specifications for this column. Go to the Specs Summary form under the
Design tab. Enter 1.2 for Reflux Ratio and make sure that the reflux ratio specification is the only active
design specification.

4.23. We will now add a specification for the mole fraction of acetone in the distillate stream. Go to the Specs
form under the Design tab. Click Add and select Column Component Fraction. Select Stream for Target
Type, Acetone for Draw, enter 0.99 for Spec Value, and select Acetone for Component.

4.24. The Degrees of Freedom for the column should now be 0. Click the Run button to begin column
calculations. The column should solve.

11
Dist-009H Revised: Nov 19, 2012

4.25. We now need to add a cooler to cool the bottoms stream in order to recycle it back to the mixer. Add a
Cooler to the flowsheet from the Model Palette.

12
Dist-009H Revised: Nov 19, 2012

4.26. Double click on the cooler (E-100). Select stream Sol-Rec as the Inlet, and create an Outlet called Lean-
Sol and an Energy stream called Q-Cool.

4.27. In the Worksheet tab enter an outlet Temperature of 30°C and a Pressure of 1 bar. The block should
solve.

13
Dist-009H Revised: Nov 19, 2012

4.28. Now we will add a Spreadsheet to control to flowrate of solvent in the Make Up stream.

4.29. Double click on the spreadsheet (SPRDSHT-1). Go to the Spreadsheet tab and enter the following text in
cells A1 and A2.

14
Dist-009H Revised: Nov 19, 2012

4.30. Right click on cell B1 and select Import Variable. Select Master Comp Molar Flow of 3-methylhexane in
the acetone product stream.

4.31. Click on cell B2 and enter “=B1”. Right click on cell B2 and select Export Formula Result. Select the
Molar Flow of stream Make Up. This will set the Make Up stream flowrate equal to the flowrate of
solvent being lost in the product stream.

15
Dist-009H Revised: Nov 19, 2012

4.32. We will now recycle the bottoms streams from the second column in order to prevent throwing away
acetone product. Add a Recycle block to the flowsheet from the Model Palette.

16
Dist-009H Revised: Nov 19, 2012

4.33. Double click on the recycle block (RCY-1). Select stream Sol-Rec as the Inlet and stream Solvent-Recycle
as the Outlet. The flowsheet should solve.

4.34. We can now try to minimize the amount of solvent that we are recycling. It is possible that there are
many solutions for the amount of solvent recycle, and we wish to find the op timum solution. We can
vary the mass flow of the recycle stream and find where the reboiler duty is at the lowest.

4.35. Go to Case Studies in the navigation pane and click Add. In Case Study 1 click Add and select the Mass
Flow of stream Solvent-Recycle and the Reboiler Duty of column T-101. Enter a Low Bound of 75 kg/h,
a High Bound of 200 kg/h, and a Step Size of 5 kg/h. Click Run.

17
Dist-009H Revised: Nov 19, 2012

4.36. Check results. Go to the Plots tab and you will see that the reboiler duty is the lowest when the solvent
recycle flow is around 75 kg/h. You may try setting the flowrate of Solvent-Recycle even lower, but you
will find that the flowsheet will not converge.

18
Dist-009H Revised: Nov 19, 2012

4.37. Double click on stream Solvent-Recycle and enter a Mass Flow of 75 kg/h. The flowsheet should
converge after a few moments.

4.38. Check results. Double click on column T-101 and go to the Cond./Reboiler form under the Performance
tab. Make note of the Condenser and Reboiler Duty.

4.39. Double click on energy stream Q-Cool and make note of the cooling duty.

19
Dist-009H Revised: Nov 19, 2012

4.40. The total heating duty for this design is 16,270 kcal/h and the total cooling duty is 9,218 kcal/h.

4.41. Save this the HYSYS file as Dist-009H_Extraction.hsc.

5. Conclusions
Based on the simulation results, it would require 16,270 kcal/h of heating and 9,218 kcal/h of cooling to
separate the water –acetone mixture via liquid-liquid extraction. This design is proven to be feasible, however it
may or may not be the optimal design. Another option would be dire ct distillation of water and acetone. Direct
distillation of water and acetone would require less equipment, but it may require more energy.

6. Copyright
Copyright © 2012 by Aspen Technology, Inc. (“AspenTech”). All rights reserved. This work may not be
reproduced or distributed in any form or by any means without the prior written consent of
AspenTech. ASPENTECH MAKES NO WARRANTY OR REPRESENTATION, EITHER EXPRESSED OR IMPLIED, WITH
RESPECT TO THIS WORK and assumes no liability for any errors or omissions. In no event will AspenTech be
liable to you for damages, including any loss of profits, lost savings, or other incidental or consequential
damages arising out of the use of the information contained in, or the digital files supplied with or for use wit h,
this work. This work and its contents are provided for educational purposes only.

AspenTech®, aspenONE®, and the Aspen leaf logo, are trademarks of Aspen Technology, Inc.. Brands and
product names mentioned in this documentation are trademarks or service marks of their respective companies.

20
RX-008H Revised: Nov 6, 2012

Simple Combustion Reactor with Aspen HYSYS® V8.0

1. Lesson Objectives
 Use conversion reactor block
 Determine air flow rate needed for a clean burn
 Determine heat available from a fuel stream

2. Prerequisites
 Aspen HYSYS V8.0
 Understanding of enthalpy of combustion

3. Background
Natural gas, which is primarily methane, is distributed in underground pipes. The pressure in these pipes varies
depending on where in the pipe it is: the closer to the pumping station, the higher the pressure. An industrial
customer can expect to get natural gas at around 60 psig, and is typically charged per cubic foot of natural gas
used. Methane burns in the following reaction:

CH4 + 2 O2  CO2 + 2 H2O

The examples presented are solely intended to illustrate specific concepts and principles. They may not
reflect an industrial application or real situation.

4. Problem Statement and Aspen HYSYS Solution


Problem
Determine how much energy is available from a 5 ft 3/h (0.472 kg/h) fuel stream that consists of only methane at
60 psig. The air feed should be approximated with 80 mol-% nitrogen and 20 mol-% oxygen. There should be
10% excess oxygen in the air stream so the fuel-air mixture is not too rich. Assume the exhaust is 182 °C. Report
the air flow rate in mol/h and ft 3 /h (at 1 atm) in addition to the available heat in kW.

Mole Balance
Two moles of oxygen are required to combust each mole of methane. Oxygen is one fifth of the moles in air.
Therefore there will need to be ten moles of air for each mole of methane for a stoichiome tric mixture. A 10%
excess requires a 10% increase in the relative amount of air, or 11 moles of air for each mole of methane.

1
RX-008H Revised: Nov 6, 2012

Aspen HYSYS Solution


4.01. Start Aspen HYSYS V8.0. Select New to create a new simulation.

4.02. Create a component list. In the navigation pane find Component Lists and select Add to create a new
HYSYS component list. Add Oxygen, Nitrogen, Methane, Carbon Dioxide, and Water to the component
list.

4.03. Add a fluid package. Go to Fluid Packages and select Add. Select Peng-Robinson as the property
package.

4.04. Define reaction. Go to Reactions and click New to create a new reaction set. In the form for the newly
created reaction set, click Add Reaction and select Hysys, Conversion.

2
RX-008H Revised: Nov 6, 2012

4.05. Double click Rxn-1 to open the Conversion Reaction: Rnx-1 window. Enter the following information.
Notice that the Reaction Heat is automatically calculated to be -8.0e+05 kJ/kgmole.

4.06. Attach reaction to fluid package. In the Reaction Set 1 form, click the Add to FP button. Select Basis-1.

3
RX-008H Revised: Nov 6, 2012

4.07. At this point, you are ready to move to the simulation environment. To do so, click the Simulation
button at the bottom left of the screen.

4.08. On the main flowsheet create a material stream using the Model Palette. Select the icon for material
stream and place it onto the flowsheet.

4
RX-008H Revised: Nov 6, 2012

4.09. Double click the stream to open the stream property window. Change the stream name to Methane,
and enter a Temperature of 25°C, a Pressure of 515 kPa, and a Mass Flow of 0.472 kg/h.

4.10. Go to the Composition form and enter a Mole Fraction of 1 for Methane. You will notice that after
entering the stream composition, the status bar will turn green and say OK. This indicates that stream is
fully defined and solved for all parameters.

5
RX-008H Revised: Nov 6, 2012

4.11. Create a second material stream to be the air stream that is required for combustion. Double click on
the new material stream and enter the following information. Bold blue font indicates a user-entered
value. From the solved Methane stream, we know there are 0.02942 kgmole/hr of Methane. We
would like there to be 11 moles of air for each mole of methane, therefore we will enter a molar
flowrate of 0.324 kgmole/hr for the air stream. Enter a Mole Fraction of 0.2 for Oxygen and mole
fraction of 0.8 for Nitrogen. The stream should then solve.

6
RX-008H Revised: Nov 6, 2012

4.12. The flowsheet should now look like the following.

7
RX-008H Revised: Nov 6, 2012

4.13. We will now place a valve in order to reduce the pressure of the methane stream to ambient pressure.
Select a Control Valve from the Model Palette and place it onto the flowsheet.

4.14. Double click the valve to open the valve property window. In the Connections page select Methane as
the Inlet stream and create an Outlet called Methane-LP.

8
RX-008H Revised: Nov 6, 2012

4.15. Specify valve outlet pressure. Go to the Worksheet tab and enter a Pressure of 101.3 kPa for the
Methane-LP stream. The valve should solve.

9
RX-008H Revised: Nov 6, 2012

4.16. Insert reactor. Press F12 to open the UnitOps window. Select the Reactors radio button and add a
Conversion Reactor to the flowsheet.

4.17. In the Conversion Reactor property window select streams Air and Methane-LP as Inlet streams.
Create a Vapour Outlet stream called VAP-Out and a Liquid Outlet called LIQ-Out.

10
RX-008H Revised: Nov 6, 2012

4.18. Go to the Reactions tab. Select Set-1 for Reaction Set. The reactor should solve and the status should
turn green and say OK.

11
RX-008H Revised: Nov 6, 2012

4.19. The flowsheet should now look like the following.

4.20. To check results go to Worksheet tab of the Conversion Reactor. You can see that the stream VAP-Out
is leaving the reactor at an extremely high temperature. This is due to the high heat of reaction. To
calculate exactly how much energy is released from this reaction simply take the heat of reaction found
in the Reactions tab and multiply it by the methane molar flowrate. In this case, burning 5 ft 3 /h of
methane releases 6.5 kW.

12
RX-008H Revised: Nov 6, 2012

5. Conclusions
5 ft3 /h of methane produces 6.5 kW of heat. To run a quality, lean mixture there must be 280 ft 3 /h of air (that is
20 mol-% oxygen) which is 0.324 kgmole/h. The conversion reactor block is useful for quick simulations with
well understood reactions. Reactions with slow kinetics, or complex systems with series or parallel reactions are
outside the scope of this reactor model.

This simulation could also be created using a Gibbs reactor block. The Gibbs reactor is unique in that it can
function without a defined reaction set. This reactor block will minimize the Gibbs free energy of the reacting
system to calculate the product composition. This reactor block is useful when the exact reactions or kinetics
are unknown, and the reaction reaches equilibrium very quickly. It may be a useful exercise to repeat this
module using a Gibbs reactor and compare results.

6. Copyright
Copyright © 2012 by Aspen Technology, Inc. (“AspenTech”). All rights reserved. This work may not be
reproduced or distributed in any form or by any means without the prior written consent of
AspenTech. ASPENTECH MAKES NO WARRANTY OR REPRESENTATION, EITHER EXPRESSED OR IMPLIED, WITH
RESPECT TO THIS WORK and assumes no liability for any errors or omissions. In no event will AspenTech be
liable to you for damages, including any loss of profits, lost savings, or other incidental or consequential
damages arising out of the use of the information contained in, or the digital files supplied with or for use with,
this work. This work and its contents are provided for educational purposes only.

AspenTech®, aspenONE®, and the Aspen leaf logo, are trademarks of Aspen Technology, Inc.. Brands and
product names mentioned in this documentation are trademarks or service marks of their respective companies.

13
Design-001H Revised: Nov 7, 2012

Ammonia Synthesis with Aspen HYSYS® V8.0


Part 1 Open Loop Simulation of Ammonia Synthesis

1. Lesson Objectives
 Become comfortable and familiar with the Aspen HYSYS graphical user interface
 Explore Aspen HYSYS flowsheet handling techniques
 Understand the basic input required to run an Aspen HYSYS simulation
 Determination of Physical Properties method for Ammonia Synthesis
 Apply acquired skill to build an open loop Ammonia Synthesis process simulation
 Enter the minimum input required for an simplified Ammonia Synthesis model
 Examine the open loop simulation results

2. Prerequisites
 Aspen HYSYS V8.0

3. Background
Ammonia is one of the most highly produced chemicals in the world and is mostly used in fertilizers. In 1913
Fritz Haber and Carl Bosch developed a process for the manufacture of ammonia on an industrial scale (Haber-
Bosch process). This process is known for extremely high pressures which are required to maintain a reasonable
equilibrium constant. Today, this process produces 500 million tons of nitrogen fertilizer per year and is
responsible for sustaining one-third of the Earth’s population.

Ammonia is produced by reacting nitrogen from air with hydrogen. Hydrogen is usually obtained from steam
reformation of methane, and nitrogen is obtained from deoxygenated air. The chemical reaction is shown
below:

Our goal is to produce a simulation for the production of ammonia using Aspen HYSYS. We will create a very
simplified version of this process in order to learn the basics of how to create a flowsheet in the Aspen HYSYS
V8.0 user interface. A diagram for this process is shown below.

1
Design-001H Revised: Nov 7, 2012

Knowledge Base: Physical Properties for Ammonia Process


Equation-of-state models provide an accurate description of the thermodynamic properties of the high-
temperature, high-pressure conditions encountered in ammonia plants. The Peng-Robinson equation of state
was chosen for this application.

The examples presented are solely intended to illustrate specific concepts and principles. They may not
reflect an industrial application or real situation.

2
Design-001H Revised: Nov 7, 2012

4. Aspen HYSYS Solution


Build a Process Simulation for Ammonia Synthesis

4.01. Start Aspen HYSYS V8.0. Select New on the Start Page to create a new simulation.

4.02. Create a component list. In the Component Lists folder, select Add. Add the following components to
the component list.

4.03. Create a fluid package. In the Fluid Packages folder, select Add. Select the Peng-Robinson property
package.

4.04. Define reactions. Go to the Reactions folder, and click Add. This will create a new reaction set called
Set-1. In Set-1, select Add Reaction and select Hysys, Conversion. This will create a new reaction called
Rxn-1.

3
Design-001H Revised: Nov 7, 2012

4.05. Double click on Rxn-1 to open the Rxn-1 window. Enter the following information. Close this window
when complete.

4.06. In Set-1, we must now attach the reaction set to a fluid package. Click the Add to FP button and select
Basis-1. The reaction set should now be ready.

4
Design-001H Revised: Nov 7, 2012

4.07. Go to the simulation environment. Click on the Simulation button in the bottom left of the screen. Then
find the Flowsheet Main tab. The Flowsheet Main is the main simulation flowsheet where you will
create a simulation.

4.08. From the Model Palette, add a Compressor to the main flowsheet.

5
Design-001H Revised: Nov 7, 2012

4.09. Double click the compressor (K-100) to open the property window. Create an Inlet stream called
SynGas, an Outlet stream called S2, and an Energy stream called Q-Comp1.

6
Design-001H Revised: Nov 7, 2012

4.10. We must define our SynGas feed stream. In K-100, go to the Worksheet tab. For the stream SynGas,
enter a Temperature of 280°C, a Pressure of 25.5 bar_g, and a Molar Flow of 7000 kgmole/h. In the
Composition form enter the following mole fractions. Stream SynGas should now solve.

4.11. Specify the compressor outlet pressure. In the Worksheet tab of K-100, enter a Pressure of 274 bar_g
for stream S2. The compressor should now solve.

7
Design-001H Revised: Nov 7, 2012

4.12. The flowsheet should look like the following.

4.13. Next, we will add a mixer. Add a Mixer to the flowsheet from the Model Palette.

8
Design-001H Revised: Nov 7, 2012

4.14. Double click on the mixer (MIX-100) to open the mixer window. Select stream S2 as the Inlet and create
an Outlet stream called S3. The mixer should solve. We will eventually use this mixer to connect a
recycle stream to the process.

9
Design-001H Revised: Nov 7, 2012

4.15. Next, add a heater to the flowsheet.

4.16. Double click on the heater (E-100) to open the heater window. Select S3 as the Inlet stream, create an
Outlet stream called S4, and create an Energy stream called Q-Heater. In the Parameters form in the
Design tab, enter a Delta P of 0. In the Worksheet tab, specify an outlet Temperature of 775 K
(481.9°C). Note that this heater is currently acting as a cooler, but once we connect the recycle stream
this block will in fact add heat and raise the temperature of the stream.

10
Design-001H Revised: Nov 7, 2012

4.17. Next, we will add a reactor to the flowsheet. This process uses plug flow reactors to accomplish
synthesis reaction, but for this simplified simulation we will use a conversion reactor. To use a plug flow
reactor, we would need to have detailed kinetics describing the reaction. Press F12 to open the UnitOps
window. Select the Reactors radio button and select Conversion Reactor. Click Add.

11
Design-001H Revised: Nov 7, 2012

4.18. After clicking Add, the conversion reactor window will open. Select an Inlet stream of S4 and create a
Vapour Outlet stream of S5V, a Liquid Outlet stream of S5L, and an Energy stream called Q-Reac.

4.19. In the conversion reactor window (CRV-100), go to the Reactions tab. Select Set-1 for Reaction Set. In
the Worksheet tab enter an outlet Temperature of 481.9°C for stream S5L. This value will copy over to
S5V. The reactor should then solve. Notice that the contents of the reactor are entirely vapor;
therefore the liquid outlet stream has a flowrate of zero.

12
Design-001H Revised: Nov 7, 2012

4.20. The flowsheet should now look like the following.

4.21. We will now add a cooler to cool the vapor stream leaving the reactor.

13
Design-001H Revised: Nov 7, 2012

4.22. Double click the cooler (E-101) to open the cooler window. Select stream S5V as the Inlet stream,
create an Outlet stream called S6, and create an Energy stream called Q-Cooler.

14
Design-001H Revised: Nov 7, 2012

4.23. In the Parameters form under the Design tab, enter a Delta P of 100 bar. We want to lower the
pressure in order to allow an easier separation of ammonia. In the Worksheet tab, specify an outlet
stream Temperature of 300 K (26.85°C). The cooler should solve.

15
Design-001H Revised: Nov 7, 2012

4.24. Add a separator block to the flowsheet.

4.25. Double click on the separator (V-100). Select an Inlet stream of S6, create a Vapour Outlet called S7,
and create a Liquid Outlet called NH3. The separator should solve.

16
Design-001H Revised: Nov 7, 2012

4.26. The flowsheet should now look like the following.

4.27. Review simulation results. Double click stream NH3. In the Conditions form under the Worksheet tab
you can view the stream flowrate and conditions. In the Composition form you can view the stream
composition. Here you can see that the mole fraction of ammonia is equal to 0.9754.

17
Design-001H Revised: Nov 7, 2012

4.28. After completing this simulation, you should save the file as a .hsc file. It is also good practice to save
periodically as you create a simulation so you do not risk losing any work. The open loop simulation is
now ready to add a recycle stream, which we will then call a closed loop simulation. See module Design-
002H for the closed loop design.

5. Copyright

Copyright © 2012 by Aspen Technology, Inc. (“AspenTech”). All rights reserved. This work may not be
reproduced or distributed in any form or by any means without the prior written consent of
AspenTech. ASPENTECH MAKES NO WARRANTY OR REPRESENTATION, EITHER EXPRESSED OR IMPLIED, WITH
RESPECT TO THIS WORK and assumes no liability for any errors or omissions. In no event will AspenTech be
liable to you for damages, including any loss of profits, lost savings, or other incidental or consequential
damages arising out of the use of the information contained in, or the digital files supplied with or for use with,
this work. This work and its contents are provided for educational purposes only.

AspenTech®, aspenONE®, and the Aspen leaf logo, are trademarks of Aspen Technology, Inc.. Brands and
product names mentioned in this documentation are trademarks or service marks of their respective companies.

18
Dist-012H Revised: Nov 19, 2012

Extractive Distillation for Heptane-Toluene Separation using


Aspen HYSYS® V8.0

1. Lesson Objectives
 Essentials of extractive distillation
 How to compare design alternatives

2. Prerequisites
 Aspen HYSYS V8.0
 Introduction to distillation

3. Background
When the two components in a binary mixture have very close normal boiling points, their relative volatility is
likely to be small if they do not form an azeotrope. For such cases, it may be more efficient to use extractive
distillation with a solvent than normal distillation. In extractive distillation, a less volatile solvent is used to
increase the relative volatilities of the original mixtures, allowing for easier separation. In this example, phenol
is used as the solvent for the separation of n-heptane and toluene.

The examples presented are solely intended to illustrate specific concepts and principles. They may not
reflect an industrial application or real situation.

4. Problem Statement and Aspen HYSYS Solution


Problem Statement

Determine whether conventional distillation or extractive distillation with phenol as a solvent is a more efficient
method to separate n-heptane and toluene.

Aspen HYSYS Solution

4.01. We will build models to simulate the separation of n-heptane and toluene. One model has a single
distillation column and the other uses the extractive distillation approach with two columns. First we
will build a simulation for a single distillation column. Start a new simulation using in Aspen HYSYS V8.0.

4.02. Create a component list. In the Component Lists folder select Add. Add n-Heptane and Toluene to the
component list.

1
Dist-012H Revised: Nov 19, 2012

4.03. Select property package. In the Fluid Packages folder select Add. Select NRTL as the property package
and select RK as the Vapour Model.

4.04. Go to the simulation environment by clicking the Simulation button in the bottom left of the screen.

2
Dist-012H Revised: Nov 19, 2012

4.05. Place a Distillation Column Sub-Flowsheet on the main flowsheet from the Model Palette.

4.06. Double click on the column (T-100) to open the Distillation Column Input Expert. On Page 1 enter the
following information and click Next when complete.

3
Dist-012H Revised: Nov 19, 2012

4.07. On Page 2 of the Input Expert leave the default selections for a Once-through, Regular Hysys reboiler.
Click Next.

4.08. On Page 3 of the Input Expert enter Condenser and Reboiler Pressures of 1 bar. Click Next when
complete.

4
Dist-012H Revised: Nov 19, 2012

4.09. On Page 4 and 5 of the Input Expert leave all fields empty. Click Done on the final page to configure the
column.

4.10. In the Column: T-100 window go to the Worksheet tab to specify the feed stream. For the Feed stream
enter a Vapour Fraction of 0.5, a Pressure of 1 bar, and a Molar Flow of 100 kgmole/h.

4.11. In the Composition form under the Worksheet tab enter Mole Fractions of 0.5 for both components.
This stream should solve.

4.12. Now we must define the column design specifications. Go to the Specs Summary form under the
Design tab. Uncheck the Active boxes so that there are no active specifications.

5
Dist-012H Revised: Nov 19, 2012

4.13. Go to the Specs form under the Design tab. We want to add a specification for the mole purity of both
product streams. Click Add and select Column Component Fraction. Select Stream for Target Type,
Heptane for Draw, enter 0.99 for Spec Value, and select n-Heptane for Component.

4.14. Add a similar specification for the mole fraction of toluene in the bottoms product stream.

6
Dist-012H Revised: Nov 19, 2012

4.15. After entering both design specifications the Degrees of Freedom should now be 0. Click Run to begin
calculations. The column should converge.

4.16. Go to the Cond./Reboiler form under the Performance tab. Make a note of both the Condenser and
Reboiler duties. The Condenser Duty is 5.390e+006 kcal/h and the Reboiler Duty is 5.388e+006 kcal/h.

7
Dist-012H Revised: Nov 19, 2012

4.17. Save this file as Dist-012H-Single_Column.hsc.

4.18. We will now create a second simulation, this time using extractive distillation. Create a new file in
Aspen HYSYS V8.0.

4.19. Create a component list. In the Component Lists folder select Add. Add n-Heptane, Toluene, and
Phenol to the component list.

4.20. Select property package. In the Fluid Packages folder select Add. Select NRTL as the property package
and select RK as the Vapour Model.

8
Dist-012H Revised: Nov 19, 2012

4.21. Go to the simulation environment by clicking the Simulation button in the bottom left of the screen.

4.22. Add a Distillation Column Sub-Flowsheet to the main flowsheet from the Model Palette.

9
Dist-012H Revised: Nov 19, 2012

4.23. Double click on the column (T-100) to open the Distillation Column Input Expert. Enter the following
information on Page 1 and click Next when complete.

10
Dist-012H Revised: Nov 19, 2012

4.24. On Page 2 of the Input Expert leave the default selections for a Once-through, Regular Hysys reboiler.
Click Next when complete.

4.25. On Page 3 of the Input Expert enter Condenser and Reboiler Pressures of 1 bar. Click Next when
complete.

4.26. On Page 4 and 5 leave all fields empty. Click Done on the final page to configure the column.

4.27. First we must define the feed streams. In the Column: T-100 window go to the Worksheet tab. For the
Feed stream enter a Vapour Fraction of 0.5, a Pressure of 1 bar, and a Molar Flow of 100 kgmole/h.
For the Solvent stream enter a Temperature of 181°C, a Pressure of 1 bar, and a Molar Flow of 60
kgmole/h.

11
Dist-012H Revised: Nov 19, 2012

4.28. In the Composition form under the Worksheet tab enter Mole Fractions of 0.5 for n-Heptane and
Toluene in the Feed stream, and a Mole Fraction of 1 for Phenol in the Solvent stream. Both streams
should solve.

4.29. We must now define our design specifications for the column. Go to the Specs Summary sheet under
the Design tab. We want to specify a distillate product rate of 50 kgmole/h with a mole fraction of 0.99
n-Heptane. Enter 50 kgmole/h in the field for Vent Rate and uncheck the active box for Reflux Ratio.

12
Dist-012H Revised: Nov 19, 2012

4.30. Go to the Specs form under the Design tab. Here we will add a specification for the mole fraction of
heptane in the distillate stream. Click Add and select Column Component Fraction. Select Stream for
Target Type, Heptane for Draw, enter 0.99 for Spec Value, and select n-Heptane for Component.

4.31. The Degrees of Freedom for the column should now be 0. Click Run to begin calculations. The column
should solve.

4.32. We must now add a second column to separate the solvent from the toluene in the Rich-Solvent
stream. Insert a second Distillation Column Sub-Flowsheet from the Model Palette.

13
Dist-012H Revised: Nov 19, 2012

4.33. Double click on the second column (T-101) to open the Distillation Column Input Expert. On Page 1
enter the following information and click Next when complete.

4.34. On Page 2 of the Input Expert leave the default selections for Once-through, Regular Hysys reboiler.
Click Next.

4.35. On Page 3 of the Input Expert enter Condenser and Reboiler Pressures of 1 bar. Click Next when
complete.

14
Dist-012H Revised: Nov 19, 2012

4.36. On Page 4 and 5 of the Input Expert leave all fields blank and click Done on the final page to configure
the column.

4.37. We must define the design specifications for this second column. Go to the Spec Summary form under
the Design tab. Uncheck the active boxes so that there are no active specifications.

4.38. Go to the Specs form under the Design tab. Here we will create two specifications for the mole
fractions of toluene and phenol in the product streams. Click Add and select Column Component
Fraction. Select Stream for Target Type, Toluene for Draw, enter 0.99 for Spec Value, and select
Toluene for Component.

15
Dist-012H Revised: Nov 19, 2012

4.39. Add a similar specification for the mole fraction of phenol in the bottoms product stream. Enter .99999
for Spec Value.

4.40. The Degrees of Freedom for the column should now be 0. Click Run to begin calculations. The column
should converge.

16
Dist-012H Revised: Nov 19, 2012

4.41. We will now recycle the Lean-Solvent stream back to the first column. Add a Recycle block to the
flowsheet from the Model Palette.

17
Dist-012H Revised: Nov 19, 2012

4.42. Double click on the recycle block (RCY-1). Select stream Lean-Solvent as the Inlet and stream Solvent as
the Outlet. The recycle block should solve.

4.43. Check results. Double click on the first column (T-100) and go to the Cond./Reboiler form under the
Performance tab. Make note of the Condenser and Reboiler Duties.

18
Dist-012H Revised: Nov 19, 2012

4.44. Double click the second column (T-101) and go to the Cond./Reboiler form under the Performance tab.
Make a note of the Condenser and Reboiler Duties.

4.45. The following table will summarize the energy requirements from the case with 1 column versus the
case using extractive distillation.

Single Column Distillation Extractive Distillation


Total Heating Duty (kcal/h) 5,388,000 1,803,000
Total Cooling Duty (kcal/h) 5,390,000 1,410,000

5. Conclusions
For the separation of n-heptane and toluene, extractive distillation has a significant advantage in total energy
requirements. Adding phenol as a solvent increased the relative volatilities of n-heptane and toluene in the
mixture and allowed for a much easier separation. However, extractive distillation required more equipment in
this case. Therefore a further analysis on capital versus operational costs would have to be performed in order
to make a decision as to which design is the better option.

19
Dist-012H Revised: Nov 19, 2012

6. Copyright
Copyright © 2012 by Aspen Technology, Inc. (“AspenTech”). All rights reserved. This work may not be
reproduced or distributed in any form or by any means without the prior written consent of
AspenTech. ASPENTECH MAKES NO WARRANTY OR REPRESENTATION, EITHER EXPRESSED OR IMPLIED, WITH
RESPECT TO THIS WORK and assumes no liability for any errors or omissions. In no event will AspenTech be
liable to you for damages, including any loss of profits, lost savings, or other incidental or consequential
damages arising out of the use of the information contained in, or the digital files supplied with or for use with,
this work. This work and its contents are provided for educational purposes only.

AspenTech®, aspenONE®, and the Aspen leaf logo, are trademarks of Aspen Technology, Inc.. Brands and
product names mentioned in this documentation are trademarks or service marks of their respective companies.

20

You might also like