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Pressure Swing Distillation with Aspen HYSYS V8.0

1. Lesson Objectives
Configure distillation columns in Aspen HYSYS Learn to use pressure swing to overcome azeotropic mixture

2. Prerequisites
Aspen HYSYS V8.0 Working knowledge of vapor-liquid equilibrium and distillation

3. Background
Basics on Azeotropic Distillation
An azeotrope occurs when the liquid and vapor mole fractions of each component are the same. On a y -x plot, an azeotrope is shown by a line which passes through the x = y line. Azeotropes present challenges to separation processes and need to be accounted for in process design and operation.

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No further enrichment can occur in either phase when the system reaches the azeotrope constraint because the driving force is eliminated. A mixture will separate towards a pure component and the azeotropic mixture. The component which is purified depends on which side of the crossover the initial mixture is. To purify the minority component, you must first cross the azeotrope. This can be done by adding an entrainer, another chemical which breaks the azeotrope. This creates the need for additional separation and usually material recycle with a purge stream. Alternatively, the composition of the azeotrope is dependent on pressure, which can be exploited to get the mixture across the azeotrope. This is called pressure swing distillation. Ethanol and water form an azeotrope at approximately 95.5mol-% ethanol at 1 atm. This is a low-boiling point (or positive) azeotrope. The boiling point of the mixture is lower than either of the pure components, so the azeotropic mixture exit from the top of the column regardless of which compound is being enriched in the bottoms. 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
A feed of 24,000 kg/h of 20mol-% ethanol and 80 mol-% water must be separated. The required product stream is 99 mol-% ethanol at a flowrate of at least 7,500 kg/h. This separation will be achieved by using pressure swing distillation. We begin by creating a technically feasible design for a two-column separation train. We will report for each column: operating pressure, number of stages, reflux ratio, and the purity and recovery specifications. Also report a stream table with the flowrates and compositions of relevant streams. Material recycle will be necessary to achieve these results. We will use an operating pressure of 0.1 bar for the first column, and an operating pressure of 20 bar for the second column.

Aspen HYSYS Solution

4.01. 4.02. Create a new simulation in Aspen HYSYS V8.0. Create a component list. In the Component Lists folder select Add. Add ethanol and water to the component list.

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4.03.

Define property package. In the Fluid Packages folder select Add. Select NRTL as the property package. Select RK as the Vapour Model . The non-random, two liquid ( NRTL) model works well for very non ideal liquid systems which is important because of the hydrogen bonding present. The Redlich-Kwong equation model works much better at high pressures than the ideal gas assumption in the vapour phase.

4.04.

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

4.05.

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

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4.06.

Double click the column ( T-100). This will open the Distillation Column Input Expert window. Enter the following information and click Next when complete.

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On the second page of the input expert leave the default selections for a Once-through, Regular Hysys reboiler and click Next. On page 3 of the input expert enter Condenser and Reboiler Pressures of 0.1 bar. Click Next when complete.

4.08.

4.09.

On page 4, leave all fields for temperature estimates blank. Click Next to continue. On page 5 of the input expert, again leave all fields blank and click Done to configure the column. We will now define the feed stream. Double click on the Feed stream. In the Worksheet tab enter a Temperature of 65C, a Pressure of 1.2 bar, and a Mass Flow of 24,000 kg/h.

4.10.

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4.11.

Go to the Composition form under the Worksheet tab to define the composition of the feed stream. Enter Mole Fractions of 0.2 for ethanol and 0.8 for water. When complete, the feed stream should be fully defined and will solve.

4.12.

Double click the column ( T-100) to finish specifying the operating conditions. Go to the Specs form under the Design tab. First, we would like to recover 99% of ethanol from the feed stream. To do this we will click the Add button and select Column Component Recovery. Select stream D1 as the Draw, enter a Spec Value of 0.99, and select Ethanol as the Component.

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4.13.

Second, we would like the distillate stream ( D1) to have a mole fraction of 0.90 for ethanol. The azeotrope prevents us from the reaching the desired product purity of 99% with a single column, but we would still want the distillate from the first column to be very pure while losing as little product to the bottoms stream as possible. Click Add and select Column Comp Fraction. Select Stream for Target Type , D1 for Draw, 0.90 for Spec Value , and Ethanol for Component.

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4.14.

Go to the Specs Summary form under the Design tab. Make sure that the only specifications marked as active are Comp Recovery and Comp Fraction. The column will attempt to solve once these specs are active.

4.15.

If the solver fails to converge, we may have to add some parameter estimates. For example, we can provide an estimate for the distillate stream flow rate based on a simple mass balance. We know that the feed contains approximately 200 kgmole/h of ethanol. We also know that we want to recover 99% of ethanol with an ethanol mole fraction of 0.9 in the distillate. We can then provide an estimate of 220 kgmole/hr for the distillate stream. In the Specs Summary grid, enter 220 kgmole/h for Distillate Rate which will serve as an estimate as long as it is not an active specification. Click Run when complete. The column should now converge. Also note that the bottoms stream is over 99% water, which means that we are throwing away very little ethanol. A pure water stream is also desirable because we can now repurpose or dispose of this stream with minimal further processing.

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4.16.

We are now ready to construct the second column, which will operate on the other side of the azeotrope at a pressure of 20 bar. We first need to insert a pump to increase the pressure of the distillate stream leaving the first column. Add a pump to the flowsheet from the Model Palette .

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Double click the pump ( P-100). Select stream D1 as the Inlet, create an Outlet stream called Feed2, and create an Energy stream called Q-Pump.

4.18.

In the Worksheet tab, enter a Pressure of 20 bar (operating pressure of the second column) for stream Feed2. The pump should solve.

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Next we will insert the second Distillation Column Sub-Flowsheet to the flowsheet, after the pump.

4.20.

Double click the second column ( T-101). This will open the Distillation Column Input Expert. On the first page, enter the following information and click Next when complete.

4.21.

On page 2 of the input expert, leave the default selections for a Once-through, Regular Hysys reboiler. Click Next. On page 3 of the input expert, enter Condenser and Reboiler Pressures of 20 bar. Click Next when complete.

4.22.

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4.23.

On page 4 leave all fields for temperature estimates blank. Click Next. On the final page, also leave all fields blank. Click Done to configure the column. We must now enter the operating specifications for the column. In the column window for T-101 go to the Specs form under the Design tab. Add a column specification for the mole fraction of ethanol in the bottoms stream. Click Add and select Column Component Fraction. Select Stream for Target Type , Ethanol for Draw, 0.99 for Spec Value , and Ethanol for Component.

4.24.

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4.25.

We will now add a specification for the mole recovery of ethanol in the bottoms stream. In the Specs Summary form under the Design tab, double click the specification for Btms Prod Rate . We know that approximately 203 kgmole/h of ethanol are entering the process in the original feed stream. Since we are recovering 99% of the ethanol in the first column, we expect the final product stream to have a flowrate of approximately 200 kgmole/h.

4.26.

In the Specs Summary form, make sure that the only active specifications are Btms Prod Rate and Comp Fraction. The column will attempt to solve, but you should find that it will not be able to converge. This is because we need to add a recycle stream to the flowsheet.

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Double click on the first column ( T-100) and add a second Inlet Stream called Recycle . This stream will enter on the same stage as the Feed stream (stage 25).

4.28.

We will define the recycle stream with a guess of what the actual recycle stream will consist of. We will use this dummy recycle stream to allow both columns to converge, and then we will add a recycle block to find the actual recycle stream conditions. Double click the Recycle stream on the flowsheet. In the Worksheet tab enter a Vapour Fraction of 0, a Pressure of 1.2 bar, and a Molar Flow of 400 kgmole/h. In the Composition form enter Mole Fractions of 0.9 for ethanol, and 0.1 for water. Again, these values are just guesses that will be used to converge both columns. The actual value s for the recycle stream will be determined later through the use of a recycle block. Make sure that you specify Recycle in its own window, rather than in the Worksheet tab of Column T-100, as this will cause a consistency error due to overspecification when you try to complete the recycle loop.

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4.29.

Once the recycle stream is fully specified, double click on each column and click Run to converge the columns. Both columns should now successfully converge.

4.30.

Now we can close the recycle loop to determine the actual values for the Recycle stream. First we must lower the pressure of stream D2 through the use of a valve. Add a Valve to the flowsheet from the Model Palette .

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4.31.

Double click on the valve ( VLV-100). Select stream D2 as the Inlet and create an Outlet called Rec.

4.32.

Go to the Worksheet tab and specify an outlet Pressure of 1.2 bar. The valve should solve.

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4.33.

We will now add a Recycle block to the flowsheet from the Model Palette .

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4.34.

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

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4.35.

Go to the Worksheet tab to view recycle convergence results. The two streams should be equal to each other within a certain tolerance.

4.36.

If you are not satisfied with the recycle convergence, go to the Parameters tab and lower the sensitivities. For example if we change the sensitivity value to 1 for Flow and Composition we get the following results.

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4.37.

The flowsheet is now complete. Further analysis can be performed to optimize the column size, feed location, and energy requirements, but that analysis is not covere d in this lesson.

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5. Conclusions
The azeotrope in the ethanol-water system presents a barrier to separation, but pressure swing distillation can be used to purify ethanol. A technically feasible design for purifying ethanol to 99mol-% with pressure swing distillation can be constructed using Aspen HYSYS. A column with 30 equilibrium stages and operating at 0.1 bar with a reflux ratio of 6.9 increases the ethanol composition to 90mol-%. A second column with 75 equilibrium stages and operating at 20 bar with a reflux ratio of 10.8 increases the purity to 99mol-%.

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.

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