CHEN: 302

Module 10: Distillation II

Learning Outcome:
When you complete this module you will be able to ….
Evaluate the operation and efficiency of a continuous distillation tower using a DCS
control system.

Learning Objectives:
Here is what you will be able to do when you complete each objective.
10.1 Start up a distillation tower in manual mode using the DCS control system
and switch to automatic after steady state conditions have been achieved.
10.2 Adjust operating parameters to achieve acceptable product purity using the
DCS control system.
10.3 Analyze samples to determine the percentage of methanol in various
process streams.
10.4 Plot an equilibrium curve for a methanol water mixture at atmospheric
pressure.
10.5 Determine the number of ideal stages required for the product purity
attained during operation by plotting a McCabe –Thiele diagram.
10.6 Calculate overall column efficiency.
10.7 Calculate Murphee tray efficiency for each tray in the column.

Introduction
Distillation I focused on the fundamental purpose and operating conditions in distillation.
Distillation II looks at how column efficiencies can be calculated. It also includes some
more advanced control strategies.

Equilibrium Data
The separation that occurs in any distillation process depends on the properties of the
components that are present in the feed. All of the discussion that follows will focus on a
binary mixture and, in particular, a mixture of methanol and water.
If the liquid and vapor of a binary mixture remain in contact with each other for a
sufficient amount of time, the concentrations of the liquid and the vapor will both be
constant. It can be said that the liquid and vapor are in equilibrium. From the discussion
in the first distillation lab, you should realize that the vapor formed is more concentrated
in the more volatile component. For a methanol water mixture, methanol is the more
volatile component. Equilibrium data expresses the relationship between liquid and vapor
concentrations over a broad range of concentrations and is very useful in determining
how easily the mixture can be separated. If the equilibrium vapor and liquid
concentrations are very similar, the mixture will be difficult to separate. This can be
compensated for by increasing the number of stages or trays in the distillation column.

Equilibrium data for methanol and water is presented in Table 1. Distillation data is also
often presented in graphical form. An example of graphical representation is presented in
Figure 1. The graphical representation of equilibrium data will be useful in the
development of concepts that follow.
 Equilibrium Data for Methanol and Water

120

100

80
Mole % Methanol in Vapor

60

40

20

0
0 20 40 60 80 100 120
Mole % Methanol in Liquid

Figure 1: Equilibrium Data for Methanol and Water

 Table 1: Equilibrium Data for Methanol and Water

BP % by mole methanol Vapor-Liquid Equilibrium

Temp. of Methanol/Water[1]
°C liquid vapor P = 760 mm Hg; T = 64.6°C - 72.0°C
100.00 0.0 0.0 BP % by mole methanol
Temp.
92.2 5.0 29.3 °C liquid vapor
87.5 10.2 43.0 71.4 60.0 83.1
84.3 15.0 52.2 69.6 70.0 87.4
81.5 20.0 59.0 67.8 80.0 91.8
78.0 30.0 67.5 66.9 85.0 93.0
75.4 40.0 73.5 66.1 90.0 96.1
72.6 52.6 79.4 65.4 95.0 98.1
72.4 54.0 80.1 64.6 100.0 100.0

Source: http://en.wikipedia.org/wiki/Methanol_(data_page)

McCabe-Thiele Diagrams
McCabe Thiele diagrams are a graphical method of determining the number of
equilibrium stages required to achieve a defined degree of separation between two
products. An equilibrium stage is defined as one in which the liquid on a tray and the
vapor evolved from that liquid are in equilibrium. If ten equilibrium stages are required,
the actual number of stages will be greater because, in practice, equilibrium between the
liquid and vapor is not reached. The number of equilibrium trays required is less than the
number of stages because the reboiler counts as one equilibrium stage. A total overhead
condenser does not count as a stage.

McCabe-Thiele Diagrams utilize material balances to develop operating equations, which

are then plotted. McCabe-Thiele diagrams are based on a number of assumptions. These
include:

• Heats of vaporization of all components are equal

• When one mole vaporizes, one mole condenses
• There is equal molar flow rate throughout the column
• Heat gain or loss from the column to the surroundings is negligible
• Heat of mixing is negligible
In present day practice, it is unlikely that McCabe-Thiele diagram would be used to
determine the number of trays in an actual design. Computer simulations are the method
of choice. However, McCabe-Theile diagrams are a useful way of illustrating some
operating principles.

The following three lines define the operating conditions within a tower. Derivation of
the equations for these lines is beyond the scope of this lab.

1. Operating line of the rectifying section. This is the section above the feed inlet.
This line passes through the point on the y = x line which corresponds to the
composition of the liquid overhead product. This line has a slope = R/(R +1)
where R stands for the reflux ratio.

2. Operating line that represents the condition of the feed. Also called the q line.
This line passes through the point on the y = x line, which corresponds to the
composition of the feed. The q line has a slope equal to q/(q-1) where q is defined
as follows:

• q = heat to vaporize the feed

heat to vaporize feed at its boiling point

Analysis of this equation shows that if the feed is partially vapor, q is less than 1. If the
feed is liquid below its boiling point, q is greater than 1 and if the feed is liquid at its
boiling point, q is equal to 1.

3. Operating line of the stripping section. This is the section below the feed. This
operating line passes through the point on the y = x line, which corresponds to the
composition of the bottom product. It also passes through the point where the q
line and the operating line for the rectifying section intersect.
Steps Involved in Preparing a McCabe Thiele Diagram

1. Plot the equilibrium data for the components being distilled. The equilibrium data
must be at the operating pressure of the column.

2. On this same plot draw in a line which represents y = x.

3. Plot the operating line of the rectifying section.

4. Plot the q line.

5. Plot the operating line of the stripping section.

6. Step off the number of theoretical stages.

The following example illustrates the preparation of a McCabe-Thiele diagram.

Assume that a binary mixture consists of two components: A and B, with A being the
more volatile component. The equilibrium data for A and B is shown below. Also assume
that it is desired to distill a feed mixture where A is 33% to produce a top product that is
90% A and 10% B on a molar basis. The bottom product is 10% A and 90% B. A reflux
ratio of 4 will be used and the feed enters as a liquid at its boiling point.

Step 1 The equilibrium data is shown.

Step 2 The y = x line is also shown.

Step 3 The operating line of the rectifying section passes through y = x = 0.9 and
has a slope of 4/(4+1) = 0.8.

Step 4 Since the feed is liquid at its boiling point, q = 1 and the slope of the q line
is ∞, which means the q line is vertical. Remember it also passes through y
= x = 0.33.

Step 5 The operating line for the stripping section passes through y = x = 0.1. It
also passes through the intersection of the q line and the operating line for
the enriching section.

Step 6 Step off the equilibrium stages. Each stage consists of a vertical line
between the operating line and the equilibrium data followed by a
horizontal line from the equilibrium data back to the operating line. The
combination of the two lines represents a stage.
 McCabe Thiele Diagram

0.9
Mole Per Cent A in Vapor

0.8
XD=0.9
0.7

0.6

0.5 Enriching Line

0.4
q line
0.3

0.2
Stripping Line
0.1 XB= 0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole Per Cent A in Liquid

Figure 2: McCabe Thiele Diagram

The separation, which is represented in Figure 2 requires about 3.6 equilibrium stages.

Column Efficiency

Column efficiency can be calculated as the overall column efficiency or by looking at the
efficiency of individual trays.

In calculating the overall column efficiency, the theoretical number of equilibrium stages
is determined using a McCabe-Thiele diagram. Since the reboiler counts as one
equilibrium stage, the number of equilibrium trays is one less than the equilibrium stages.
In the example shown above, 3.6 equilibrium stages are required. If the reboiler counts as
one stage, then 2.6 equilibrium or theoretical trays are required.

Overall Column efficiency = number of theoretical trays

actual number of trays
For the separation shown in Figure 2, if 5 actual trays are used, then:

Overall Column Efficiency = (3.6 – 1 )/5

= 52%
Murphree Tray Efficiency

Murphree Tray Efficiency is a method of calculating the efficiency of individual trays. As

vapor passes upward in the column, it is enriched with the most volatile component.
Murphree tray efficiencies compare the actual change in vapor composition to the
maximum possible change in composition. If you determine the mole fraction of the
volatile component in a sample of vapor flowing to the tray and a sample of vapor
flowing from the tray, the difference between these two values represents the change in
composition that is actually occurring. The maximum change in composition would occur
if the vapor leaving the tray was in equilibrium with the liquid on the tray.

In the lab, the trays in the column are numbered from bottom up with tray 10 being the
tray at the top of the tower. Two sample lines are connected to each tray. The liquid
sample line is connected to a hole in the tray that faces upward. The vapor sample line is
connected to a hole in the tray that faces the bottom of the tray. As a result of this
configuration, when you take a sample of liquid from tray 3, for example, you are
sampling from the liquid layer on top of tray 3. When you take a vapor sample from tray
3, you are getting the vapor leaving tray 2 and arriving at tray 3. The vapor leaving tray 3
is what you get when you sample tray 4. Keep this in mind when you are analyzing the
equation for Murphree tray efficiency.

For the lab column:

Murphree Tray Efficiency = actual change in vapor composition

Equilibrium change in vapor composition

= yn+1 - yn
y*n - yn

y = the vapor fraction of the most volatile component

y* n = the vapor fraction of the most volatile component if the vapor was in equilibrium
with the liquid on tray n

To determine y*n you must take a sample of the liquid on tray n and then determine the
composition of the vapor in equilibrium with this liquid by reading Figure 1.

Note: The vapor arriving at tray 1 is the vapor leaving the reboiler and the vapor leaving
tray 10 becomes the distillate.
Experimental Procedure

Startup procedure

For distillation II, the column will be operated from the DCS operator console. To do
this, the stand alone local control panel must be set to computer and all of the individual
controllers must be set computer and not on manual.

General Operating Procedures:

• All of the pumps in this lab are centrifugal pumps. It is correct operating
procedure to start the pumps with the control valves in the line closed.

• Once the pump is running, gradually open the control valves and monitor the flow
rates to confirm flow.

• If a pump is running and no flow occurs when the control valve is opened, shut
off the pump and troubleshoot the process by tracing the process flow lines.

• Start with the controls on manual and switch to automatic as appropriate.

• Throughout the lab, watch closely for signs of flooding in the tower. Flooding
may be caused by excessive steam flow rate, excessive feed flow rate or excessive
reflux.

Startup sequence

1. Turn on the power for the control panel and instrument air supply.

2. Close overhead accumulator drain valve, located near the bottom of accumulator.

3. Blow down steam lines.

4. Ensure level in reboiler is above 50%. If the reboiler level is below 50%, consult
the instructor before proceeding.

5. Turn on the cooling water flow through the overhead condenser, sampling cooler /
condenser and bottom product cooler. Set the flow rate at 15 USgpm. Flow of cooling
water must be established before the steam flow is initiated.

6. Open the block valve in the steam supply line and then open the flow control
valve in the steam supply line to a valve opening of approximately 95%. You will have a
short wait while the reboiler is heating. Use this time to trace the process flow lines for
the column.
7. When the fluid in the reboiler begins to boil and vapor begins to rise upward into
the tower, start to add a small amount of feed. If the tower begins to flood, reduce the
steam flow rate.

8. When the glass accumulator fills to the point that the low accumulator level alarm
cancels, start the reflux and visually check for flow at top of column. Continue to
monitor for flooding.

9. Since the top product flow has not been started, the accumulator level should be
rising. If it is not, you must either cut the reflux or increase the steam until the
accumulator level begins to rise. Once the accumulator level starts to rise, start the
flow of top product. Place the accumulator level control on automatic with a set
point of about 50%.

10. Since bottom product flow has not been started, the reboiler level should be
rising. The reboiler level should be maintained between 60 to 70%. If the reboiler
level is at or above the desired amount, start the bottom product. Set the reboiler
level control on automatic to maintain the reboiler level at the desired amount.

11. The reflux can be placed on ratio control. Consult your instructor for details on
how and why this should be done.

12. The feed flow control can be switched to automatic if desired.

13. Leave the steam flow control on manual. In this particular lab, this helps to
maintain a constant steam flow rate.

14. Adjust the operating parameters to achieve steady state operation and a reasonable
separation of the components. Review Distillation I to see which parameters can
be adjusted.

Data Collection

Obtain samples of feed, top product, bottom product and determine the percentage of
methanol to see whether a reasonable separation is being attained. When reasonable
operation has been achieved, do the following:

1. Obtain samples of liquid and vapor from each tray, and analyze them for %
methanol. At the same time record the temperature on each tray.

2. Record the flow rate of feed solution, bottom product, top product and reflux.

3. Repeat the analysis of feed, top product and bottom product for final purities.

4. If you are operating on ratio control, record the reflux ratio.

Shutdown Procedure

1. Shut off steam to the reboiler by first closing the hand valve and then closing the
control valve via the DCS.

2. Close all control valves via DCS and shut down all pumps, making sure that all
valves are closed before shutting off the pump.

3. Open the drain valve on the bottom of the accumulator. This allows the contents
of the accumulator to drain into the feed tank. Leave this drain valve open.

4. Turn off instrument air.

5. Shut off the flow of cooling water to the sample condenser.

6. Allow 5-10 minutes for the cooling water to cool the process and then turn off the
cooling water to the overhead condenser.

7. Before leaving, turn off power to the control panel.

8. Do one final inspection to ensure that shutdown is complete. Listen carefully to

determine if anything is still running.
 Report
Marks Complete and hand in the following:

3 1. Table of raw data collected.

5 2. In the raw data, all of the sample concentrations report percentage of methanol on
a mass basis. Convert all of these analyses to mole percent methanol. Show one
sample calculation completely and then summarize the rest of the results in a
table.

5 3. Using the data presented in Table 1, draw a graph of mole fraction of methanol in
liquid (x) versus mole fraction of methanol in vapor for equilibrium conditions.
On the same graph, plot mole fraction methanol in the liquid versus mole fraction
methanol in the vapor using you actual experimental data.

Note: For the real experimental data, for any x and y data points, x will be the
composition of the liquid from tray n and y will be the vapor leaving tray n, which is
actually recorded as the vapor for tray n+1.

The reboiler liquid is the same as bottom product while the vapor from the reboiler rises
to the bottom of tray 1 and is collected from tray 1.

The vapor leaving tray 10 has the same composition as the top product.

5 4. Draw a McCabe-Thiele Diagram to determine how many theoretical trays are

required to achieve the top and bottom product purity that you achieved.

• Use the data in (Table 1) to plot to the equilibrium curve.

• Use you actual experimental data for all other points
• You may assume that q = 1

5. Calculate the overall column efficiency. Remember the actual number of trays is 10.
2
6. Calculate Murphree plate efficiency for each plate in the column.
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