EPS Chemical Engineering

Laboratory Experiment Notes

HERIOT - WATT UNIVERSITY/BAKU HIGHER OIL SCHOOL

School of Engineering & Physical Sciences
Chemical Engineering Laboratory
Batch and Continuous Distillation Demonstrator Notes
CONTENTS
Introduction................................................................................................................................................... 1
Objective...................................................................................................................................................... 1
Block Diagram.............................................................................................................................................. 2
Basic Theory................................................................................................................................................. 2
Method......................................................................................................................................................... 3
Operational Notes........................................................................................................................................ 3
SAFETY NOTE............................................................................................................................................. 3
References................................................................................................................................................... 3

Introduction
Distillation is the means by which mixtures of fully miscible mixtures can be separated into their individual
components. As a technique for separation, distillation is a very common operation and particularly
important for the petrochemical industry.
Depending on the feedstock composition and product quality requirements, distillation can be dine in
many different ways. A few of the factors that may be considered include the choice of the type of column
(packed or sieve plate), operating conditions (eg pressure, reflux ratio), the type of tray for each stage, the
tray spacing, sieve hole diameter, packing material and type, column dimensions. The simple binary
distillation column sizing method normally involves finding the number of stages from a x-y diagram, the
temperature of the distillate and bottoms product using a Txy diagram. The operating lines for the bottom
and top of the column depend on the reflux ratio and the condition of the feed.
Columns can operate in two modes; continuous where a feed is supplied and products are extracted
continually, and in batch mode where the top product composition and composition in the boiler changes
over time.
In this experiment, you will look at both batch and continuous distillation of an ethanol/water mixture.
Students will meet distillation for the first time in Separations A when they look at Binary Distillation and
Column Hydraulics. HOWEVER they will only look at CONTINIOUS DISTILLATION in the lecture notes;
batch distillation may be covered but its the continuous distillation that most students in most Universities
will look at first.
The BAD NEWS is that setting up the GUNT rig for continuous distillation is not that easy so the first
experiments done are for Batch.

Aims and Objective

The general aim of this experiment is to gain operating experience of a distillation column in particular the
role that instrumentation has in monitoring the column. You will
Carry out a batch distillation at a set reflux and heating power value and record how the distillate
composition changes with time.
Carry out a continuous distillation at a set feed rate and reflux value, looking into the impact of the
two conditions on the temperature profile in the column.
Perform a theoretical determination of the number of trays and hence compare the operation of
the column to what would be expected.

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Batch is simpler to operate so is done first. Demonstrators should discuss the basic theory of a continuous
binary column with students before the experiment starts you MUST stress the importance of
temperature measurements and that knowing the temperature for a binary system at thermodynamic
equilibrium si a measure of the composition of that mixture. You should then explain with the aid of a T-xy
and x-y diagram what a batch column under continuous reflux looks like and that the top product
composition will change over time.
For both batch and continuous mode, the data logging feature of the software MUST be used to record all
temperature and conditions from the column. Students should be TOLD to take KEY temperature readings
by hand as well in case the data logging fails.

Block Diagram
The flow diagram for this experiment is complex, with certain flow lines not normally used during the
process.

Even though there is a diagram here, students should redraw this one using VISO or PowerPoint. They
should NOT copy the schematic impression from the GUNT manual.
It is best to have 2 diagrams, one for batch and one for continuous. Both diagrams should show the key
vessels (the column, the reflux collector, the reflux drum etc) and instrumentation points. Drawings should
NOT show things like the utility flow lines.

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Basic Theory
The fundamental theory for distillation is that we have a number of stages where we have a liquid stream
and vapour stream meeting together. There is an exchange of heat and some for the vapour condenses
and some of the liquid vaporises. The liquid and vapour streams leaving the stage are in thermodynamic
equilibrium and are sent to the next stage liquid to the stage below and vapour to the stage above.
Adding stages on top of each other creates a column where the composition of the vapour slowly
increases in the more volatile component, and the liquid flowing down the column becomes richer in the
least volatile component. To make sure we have vapour flowing up through the column, we some of the
liquid at the bottom of the column and vaporise it. To create the liquid flowing down the column we take
the vapour and condense it. This means that we have a temperature profile across the column; cold at the
top, hotter at the bottom.
Batch Distillation In batch distillation, a volume of mixture is charged into the boiler which sits below
the column. The heating source for the boiler is turned on and the temperature of the boiler contents will
rise. At a certain point, evaporation of the mixture will start and this vapour travels up through the column.
The vapour then passes into a condenser where cold water utility fluid is used to completely subcool the
vapour. The liquid condensate is then held in a reflux drum and is then sent either back into the column as
reflux, or into the product collection drum (vessel V). The composition of the overhead liquid product from
the condenser will be rich in the more volatile component of the mixture. As more product is taken off the
top of the column, the reboiler will become rich in the less volatile component and so the composition will
change and also the boiling point the temperature in the reboiler will rise. In terms of a x-y diagram, then
the composition of the top product and the bottom product that is inside the reboiler will change over time.
Since the reflux ratio is held constant, then we will end up with a series of operating lines that are parallel
to each other. Eventually there comes a point when the bottoms product is nearly all one phase and the
top product becomes contaminated with the heavier component.
Continuous Distillation In this mode, a feed which is usually liquid is pumped into the feed point in the
column. For the purposes of this experiment the feed is located at the mid point. Product from the reboiler
is continually extracted as is product from the condenser; note there is a portion of the condenser product
that is sent back the column as reflux. The mass lost from the column in the distillate product and the
bottoms product is replaced by the fresh feed into the column. Industrial columns will have two types of
condenser; a partial condenser or a total condenser which will produce a stream that is at its saturation
temperature. In the column in this experiment, the condenser will SUBCOOL the liquid reflux.
For either batch or continuous distillation we normally use a x-y diagram for a binary system. The
graphical representation of the distillation column is known as a McCabe-Thiele diagram. This diagram
has the equilibrium curve and one or more operating lines drawn to represent the top rectification section
and the bottom stripping section. In a batch column, there is no stripping section and we will have 1
operating line.
The relationship between operating line and equilibrium compositions is given by a series for equations
that give us the gradient and intercept of these operating lines.
The equations that describe this relationship are:

x
R
x d
R 1 R 1
The operating line for the top of the column is
L
B
y x xb
V
V
Operating line for the bottom of the column is
The reflux ratio R is defined from L RD
And the overall balance on the column is F D B
y

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Where R is the reflux ratio

L is the flowrate of liquid product down the column in the top section
V is the vapour flowrate in the top section of the column

L,V

are the flowrates of liquid and vapour in the bottom of the column
subscripts d and b refer to the distillate and bottoms product
Composition For this particular column with water and ethanol, the composition of a liquid mixture of
these two can be found be measuring the density of the liquid. There are charts that will give the mass %
composition as a function of density.
Students should not repeat this theory in their report but need to say something about how a distillation
column works. It is far better if they produce a TXY and XY diagram for ethanol/water and put onto this a
sketch of what happens for a batch and continuous column. They should mark off the temperatures they
measure on the T-xy and then read off what the molar compositions will be of the reboiler and condenser.
They should then compare the compositions from the condenser with the measured concentrations from
the density bottle samples.
For BHOS I would also recommend doing a mass balance over the unit so they can CALCULATE the
composition in the reboilier. This is going to be a very rough and inaccurate calculation but it is one they
should be able to do.

Experimental Technique
The experiment is designed for 3 users and no more than 5. One user should be responsible for recording
every thing that happens in an electronic logbook and keeping a record of the measurements taken by the
other two. One user should be responsible for taking samples of product from the condenser or product
receivers, then finding the density of the sample. The 3 rd user can be responsible for using the density
measurements and the temperature measurements to work out what can be happening on a T-xy
diagram.
There are two parts to this experiment where the
Part 1 : Batch mode. Operate the column under batch mode with at least 2 different reflux
settings.
Part 2: Continuous Mode. Operate the column
Before the start of each experiment, make sure the cooling water is supplied to the condenser, make sure
the PC is on and the CE600 software is running. You are advised to start the data logging system that will
record all values in the background. You should also take a note of all key temperatures at regular
intervals and samples from key points as necessary.
Sampling You will take samples at regular intervals from key points in the column. These include
a) The feed tank before the experiment starts
b) The liquid product from the condenser that is in vessel V4
c) In continuous mode, take a sample of the product from the reboiler using the add-on valve V20
note: Do not attempt to take samples directly from the reboiler using valve V8 during the
experiment as this mixture will be boiling.
At least 50ml of liquid sample should be taken and put into a 50ml density bottle. Record the mass of
liquid inside the bottle and use a suitable chart to convert the density to a composition. Note that you will
need both a mass% and molar% composition for your analysis.
You should note that this experiment really should be done by students so that they get used to taking
data from a number of different points and in a number of ways e.g
Liquid samples for density can come directly from sample valves or by pipette
Volumes of liquid inside storage tanks should be measured by measuring the depth of liquid then
converting to a volume
Batch Experiments (Part 1):
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1. Transfer 6L or 7L of mixture stored in the two feed tanks marked VI. Open both valves V1 and V2
at the bottom of tank VI, set the pump X speed to 100%.
2. Take samples from tanks VI using a pipette to withdraw a volume into a density bottle
(recommend a 50ml density bottle)
3. Once the level inside the reboiler reaches 7L, switch off the pump and close the two values V1
and V2
4. Set the reflux to 100%
5. Set the heater power to 100% and wait until there is the first signs of bubbling on the 1 st plate
6. Wait a short period of time approximately 10 minutes until the column starts to heat up.
7. As a side note, if the temperature of the top stage increases beyond 82C, the product purity
significantly decreases and the column will become harder to control over time also, with
temperature differences between stages being as little as 1-2C.
8. Reduce the heater power to the desired value recommend 45%.
9. The cooling water flowrate will fluctuate throughout the experiment, so ensure that it is at about
150 to 180 LPM at all times unless a higher flowrate is required.
10. Wait until the column has reached steady state make sure the reflux collector (vessel IV) does
not become too full. Recommend this should be 20 minutes
11. Once at steady state, switch the reflux to the desired value and start taking samples of the product
from the condenser.
12. Due to operational limitations, the reflux inlet to the column will be 22-25C. In event of thermal
runaway where the reflux temperature increases substantially (>35C) then increase the reflux to
100%, the cooling water flowrate to 200 LPH, feed pump power to 90%, and reduce the reboiler
power to 10%. Ensure pressure gauge still reads 1 atm. In the event of overpressure, use the
emergency shutdown button on the main control unit.
13. Make sure your log records the sample weights, the key temperatures (reboiler and condenser).
Recommend you record the volume of condensate collected in the product storage tank (vessel
V)
14. Once the condenser temperature becomes close to 100 deg C, and the composition of the
condensate begins to change to give more water, turn off the experiment by turning the heater
power to 0%, and switching to 100% reflux. See the drain down procedure below for finally
shutting down the experiment.
Note:
The reboiler will gradually loose volume and it is likely that the low level shut down will trip the
heater before the end of the experiment.
You should transfer all samples into the feed tanks try to distribute the samples evenly between
the two feed tanks.

Continuous Experiments (Part 2)

1. Repeat steps 1 to 8 as in Part 1
2. Make sure valve V9 to the bottoms product collector is closed, open the bottom valve V8 on the
reboiler
3. Wait until the reboiler gets to 5L
4. Set the reflux ratio to its desired value (eg 45%) and set the pump speed to its value (suggest
20% for the first experiment).
5. The level in the reboiler should increase, so slowly open valve V9 to draw off product from the
reboiler. Be careful not to withdraw too much or the level will fall and the low level shutdown
switch will turn off the heater.
6. Continue to take samples from the condenser and from the feedline into the bottoms product
collector. Note down any relevant temperatures and take note of liquid levels in all tanks.
7. If the low level alarm shuts off the heater, close valve V9 and allow the level in the reboiler to
increase. Make sure that you turn on the power to the heater on the main control panel after the
level has reached a safe working valve.
8. If time permits, repeat the experiment with reflux ratio 25% and 35%

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You can see from these instructions that the continuous distillation is more difficult to set up and
potentially there could be quite a few different events that affect the operation of the unit. The students
should examine the recorded data profiles and see if they can match the composition of the samples with
the measured temperatures.

Key Observations to Make

The objective of this experiment is to study distillation, and to be able to look at a T-xy and x-y diagram
and match this with samples taken during the distillation. You also need to comment on the temperature
profiles within the column and comment if the column is behaving as it should be. You should also attempt
to use theory for Binary Distillation (the McCabe-Thiele method) to graphically show what this column is
doing. The column has a number of sieve trays and you should attempt to see if the number of stages is
performing the distillation as it would be expected to do. To that end you need to:
a) Take a specific note of the temperatures in the reboiler and condenser
b) That you take samples on a regular basis and convert these to mole fractions (assuming your T-xy
and xy diagrams are in mole fractions)
c) Other observations you may like to make are
a. The vapour and liquid rates inside the column you will need to record and calculate the
product flowrate and bottoms flowrate from measurements of liquid volume in the
collectors.
b. You may like to note how the pressure drop across the column changes with changes in
heating rate and the link to the vapour generated
c. You may also like to note the cooling water temperature through the condenser and
compare this with the temperature of the liquid reflux.
d. You should also note any numerical accuracy errors with the density measurement
(typically +/- 0.05g)
Specific aims from Part 1 and Part 2 are:
Part 1:
a) Use the given ethanol concentration vs density calibration and convert this into a molar
concentration vs density chart. Use this conversion in analysis of all samples.
b) Plot a graph of time vs ethanol molar concentration in the top product. Comment on the difference
between the different batch operating conditions (ie the reflux ratio)
c) Compare the measured compositions with those expected from the T-xy diagram show this
comparison in a convenient format.
Part 2:
a) For one of the reflux ratio settings, plot the operating line on a x-y diagram for the top section and
draw in the operating line for the bottom section. You will need to assume a suitable q value for
the feed as the feed will come into the column sub cooled. Attempt to draw in the number of
stages that would give you the composition of the distillate and reboiler
b) Investigate the temperature profile in the column by plotting the average plate temperature against
plate number. Determine if which, if any, of the trays are active in the separation or not.
Pure ethanol density 787 g/L
Pure water density 996 g/L
The main output from this experiment will be
1. To show on a Txy and xy diagram the points that correspond to specific times recorded in the
experiment, using the recorded temperatures. It should be possible to track what has happened to
the distillation by marking the points on the dew point and bubble point lines
2. They should show the difference in composition of the collected condensate samples and what
the temperature is indicating. Ethanol-water is a common separation to do and so there should be
data available on the web and in other places.
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Laboratory Experiment Notes

3. They should try looking at the number of stages in the column. Suggest that they try plotting each
plate out on the T-xy diagram then translating that to the x-y diagram.
4. If it is possible, they should show the batch distillation as a series of operating lines. They may
know the boil up rate from the condensate flowrate and reflux ratio.

SAFETY NOTE
This experiment involves several hazardous operations and a potentially flammable chemical. You need to
take care when operating this experiment and avoid:
1. Clean up any spillages that occurred during the sample collecting, measuring, or feed vessel refill,
using blue roll.
2. That you take samples of liquid that has been cooled and is not at its boiling point
3. That you do not overfill the reboiler, nor allow any of the other collection vessels to overfill
4. That you make sure there is sufficient cooling water supplied to the condenser

Specific PPE Requirements

PPE
Head
Eye
Hand

N/A
Goggles
Glove

Comments
Does not involve working at height
Eye protection must be used in case of any release of vapour.
Samples will vary in composition condenser samples are likely to
be mainly ethanol. You should wear gloves in case of spillage.

Ear Protection
Clothing
Foot Protection

Not required
Standard
N/A

Lab coat for handling extensive spillages

References
1. Coulson & Richardson, Chemical Engineering Design, vol. 6, chapter on distillation.
2. Coulson & Richardson, Chemical Engineering Design, vol. 2, section on batch distillation
3. Smith & McCabe, Unit Operations
4. Perrys Chemical Engineers Handbook

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DEMONSTARTOR NOTES FURTHER COMMENTS

1. Objective
As in the notes above, this is a complex experiment that only gives a limited number of points, but
a lot of data from the data logging tool. The main focus is as mentioned above to:
To show on a Txy and xy diagram the points that correspond to specific times recorded in the
experiment, using the recorded temperatures. It should be possible to track what has
happened to the distillation by marking the points on the dew point and bubble point lines
They should show the difference in composition of the collected condensate samples and
what the temperature is indicating. Ethanol-water is a common separation to do and so there
should be data available on the web and in other places.
They should try looking at the number of stages in the column. Suggest that they try plotting
each plate out on the T-xy diagram then translating that to the x-y diagram.
If it is possible, they should show the batch distillation as a series of operating lines. They may
know the boil up rate from the condensate flowrate and reflux ratio.

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2. Data files
There are several files to look at; the raw data files extracted from the CE600 data recoding
software converted to asci format, the log files in spreadsheet format recording key values and
notes taken during the experiment.
In practice, there is a lot going on in this experiment normally the temperatures from the column
especially the condenser and reboiler will not match with the measured composition of samples.
This is no error here the fact that samples are taken and then used to give a molar composition
means there is probably a larger error in the composition via density than there is composition via
temperatures.
3. Analysis
The students will need guidance on the data files and what the data is likely to show. You are
advised to look over the time series plots first as a way to understand what was happening during
the experiment. There area few noted issues:
a) The batch experiment tends to go better than the continuous in terms of stability. Once the
heater power and reflux are started, the column tends to maintain a steady operation until the
top product becomes mainly water. There is an oscillation in the heater control circuit that puts
the top temperature into oscillation.
b) The continuous run may show more of an irregular temperature profile as it is more difficult to
set up the column in continuous mode.
c) The data files may contain depths of liquids inside the collection vessels students should
realise that this is a simple way to record the volume inside these chambers. On the
spreadsheet somewhere, there may be conversions that someone has calculated out and
other sheets where there are none.
d) The final analysis will depend on how the data recorded is used. While it would be good to
show the number of theoretical trays, the students may have problems with the McCabeThiele plot. There is nothing wrong in this, because this experiment is brand new and we are
still finding out more about how the unit works.
4. What to look for in marking
In marking, we would look for:
a) A good interpretation of the data files and what can be happening. There may be fluctuation in
say heating power, cooling water flowrate that can be picked out as playing their part in
adjusting the measured compositions.
b) The students MUST be able to use a Txy diagram. They are ot provided with the ethanolwater diagram for the experiment but should be able to find one or at least generate one.
c) We should look for an understanding of what is happening in the column that we have
saturated vapour and liquid streams and that temperature gives us composition.
d) The only calculations are to convert the ethanol composition data from mass % to mole%.
Students need to look up boiling point data

Marking should reflect the level of detail included into the reports
Grade
Marking Comments
E to D
D to C
C to B
B to A
A (70 to 80)
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A (80-100)

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