BATCH PACKED DISTILLATION UNIT

EXPERIMENT 2:

BATCH PACKED DISTILLATION UNIT

INTRODUCTION
The Batch Packed Distillation Unit is developed primarily for teaching, training
and research purposes. It is used for the separation of mixtures at atmospheric
pressure in a batch operation. The unit has the following special features, which
are of particular value in training situations:
Direct heat input into the evaporator using cartridge heaters.
Silver coated and vacuum jacketed column minimizes heat loss to the
surroundings.
Vapour sampling and liquid sampling on the bottom and top to determine
the practical separation behaviour of the particular mixture.
The method of operation of a packed distillation unit for the separation of liquid
mixtures can be described in the following terms: The vapour mixture rises from
the evaporator, passes over the column packings and is fully condensed in the
condenser. The condensate runs down the column counter-current to the vapour
through the packings back into the evaporator. Among the packings, the rising
vapour attempts to achieve equilibrium with the liquid. In the ideal case the rising
vapour should be in equilibrium with the liquid. In actual columns, complete
exchange does not always take place.
The efficiency of batch packed distillation unit can be evaluated using the height
equivalent theoretical plates (HETP), which is defined as the height of the column
divided by the number of theoretical plates required to achieve the same
separation as the packed column. As the purity of a distillate is dependent to a
very large extent on the number of theoretical plates, determination of the
number of theoretical plates in a column is very important.

BATCH PACKED DISTILLATION UNIT

Cooling
Water

TI
05

FI
02

V9

V10

V8

Cooling
Water

TI
06

FI
01

W3
Vent

TI
03

V3

KS 01
TI
02

TI
07

V2

W4
TI
04

K1

PdI
01

B3

V4
V5

V6

PI
01

B2

TI
01
LS01

W1,2

V7

B1
V1

Figure 1: Process flow diagram for batch packed distillation unit

BATCH PACKED DISTILLATION UNIT

GENERAL OPERATING PROCEDURES

It is important that the user read and fully understand all the instructions and
precautions stated in the manufacturer's manuals supplied with the distillation unit
prior to operating. The following procedures will serve as a quick reference for
operating the distillation unit.
1. Valves Positions
valves.

All valves must be initially closed except the vent

2. Cooling Water System Laboratory tap water is used as the cooling media.
Hose connections are such that the cooling water enters both the top
condensor (W3) and product cooler (W4) in parallel. Adjust both the cooling
water flow rate to maximise cooling and condensation. The temperature of the
cooling water leaving the two units should not exceed 45C.
Caution: In order to avoid water hammer, open the cooling water valves
slowly.
3. Heater Power The heater output power is adjustable between 0 and 100%
so that one may vary the flow rate of the vapor and liquid inside the distillation
column. Turn the heater resistance knob located at the control panel between
a value 0 to 10.
4. Reflux Divider The reflux divider controller KS-01 has 3 positions with the
following settings:
Position 0
Total reflux
Position Hand Total distillate offtake
Position Auto Timer controlled reflux
To adjust the reflux ratio, set the reflux timer and distillate timer on the control
panel at KS-01. The reflux timer is represented by the time in seconds on the
display, while the distillate timer is represented by the time in seconds with an
additional blinking light at the lower right corner of the display. The reflux ratio
is equal to the ratio between the total reflux time and the total offtake time.

BATCH PACKED DISTILLATION UNIT

EXPERIMENTAL PROCEDURES
General Start-Up Procedures
1. Ensure all valves are closed except valve V3 and ventilation valve V6.
2. Prepare a 15 L mixture containing ethanol and filtered water at the desired
composition. Open the charge port cap and charge the evaporator B1 with the
ethanol-water mixture. Close the charge port cap.
Note:
water.

You can use any suitable binary system other than ethanol-

3. Turn on the main power on the control panel.

4. Set the reflux divider to total reflux. This is to prevent any distillate from
escaping when starting up the distillation unit.
5. Open the main cooling water valve V10. Let the cooling water flow into the
condensor (W3) and distillate cooler (W4) by opening valves V8 and V9.
Maintain at least a 20 L/min flow at the condensor and 10 L/min flow at the
distillate cooler.
6. Switch on the cartridge heaters W1 & W2 and set the heater power to 100%.
Allow the liquid in the evaporator to boil. As the liquid boils, the liquid level in
the evaporator will start to drop. Adjust the level switch to ensure that the tip
of the level switch is above the cartridge heater.
7. Observe the vapor rising from the boiling liquid into the column. As the vapor
reaches the condenser, it will condense and flow back into the column as
liquid. Mass transfer will take place between this liquid and vapor phase in the
column.
8. If flooding is observed in the column (liquid being held up by the flow of vapor
in the packings), reduce the vapor flow rate by reducing the heaters power.
9. Check that the condensor has sufficient cooling water flow to minimize escape
of vapor into the vent.
10. Leave the distillation unit for approximately 30 - 40 minutes until a stable
condition is observed. The stable condition is reached when all the
temperature indicators on the column give a constant reading with an
allowable 0.2C fluctuation.
General Shut-Down Procedures
1. Set the reflux divider to total reflux.
2. Keep the cooling water running through the condensor (W3) and distillate
cooler (W4).
3. Switch off the cartridge heaters W1 & W2. Monitor the temperature drop in the
evaporator. Wait until it has cooled down to room temperature.
4. Drain all liquid from the evaporator B1 and product vessel B2.
5. Close the cooling water valves V8, V9 and V10.

BATCH PACKED DISTILLATION UNIT

6. Turn off the main power on the control panel.

Preparation of a Refractive Index (RI) vs. Composition Plot
1. Prepare a set of mixtures containing ethanol and water within a specified
range of composition between pure water and pure ethanol. Refer to the
sample table in Appendix A.
2. For each mixture, obtain their refractive index (RI) readings using a
refractometer.
3. Prepare a plot of RI vs. composition for the whole range of mixtures. This will
serve as the calibration curve for further experiments.

Sampling Procedures
Samples can be taken from the distillate and the bottom product for analysis:
1. Distillate sampling:
a)
b)
c)
d)
e)

Open sampling valve V2 to drain the sample line of any remaining liquid.
Place a vial below valve V2.
Set the reflux divider to total distillate for a few seconds.
Collect a 10 mL sample and close sampling valve V2.
Switch the reflux divider back to total reflux.

2. Bottom sampling:
a) Place a vial below valve V1.
b) Open sampling valve V1 and collect a 10 mL sample. Be careful of the hot
liquid while collecting a sample.
c) Close sampling valve V1.
d) Cool the sample by immersing the sample vial in cold water.
Note: Always collect samples in vials with cap to avoid excessive evaporation
of ethanol before analysis.

BATCH PACKED DISTILLATION UNIT

EXPERIMENT 1: Batch Distillation At Total Reflux

OBJECTIVE:

To determine the height equivalent theoretical plates (HETP) at total

reflux.
To determine the effect of liquid and vapor loading on the HETP at total
reflux.

PROCEDURES:
1.

Perform the general start-up procedures (Section 3.1).

2.

Once the distillation unit has reached stable condition, record the top and
bottom temperatures.

3.

Collect samples from the distillate and bottom product (Section 3.4).

4.

Measure the refractive index for both samples and determine their
compositions.

5.

For different liquid and vapor loading, adjust the heater power settings in
W1 and W2. Doing so will decrease the heating duty and hence decrease
the vapor flow in the column. Consequently, the liquid flow will also
decrease.

6.

Change the heater power settings and wait for approximately 15 mins to
allow the distillation unit to achieve stable condition. Then, follow steps 2
to 5.

ANALYSIS & DISCUSSION:

1.

Use the sample table in Appendix B for data collection.

2.

Using the X-Y equilibrium diagram for ethanol-water system, mark the top
and bottom compositions on the diagram and determine the theoretical
number of plates in the distillation unit using the McCabe-Thiele method.
Refer to Appendix D.1 for a step-by-step guide.

3.

Calculate the height equivalent theoretical plates (HETP) by dividing the

effective column height with the number of theoretical plates.

4.

Plot a graph of HETP vs. heating power and observe the relationship.

BATCH PACKED DISTILLATION UNIT

EXPERIMENT 2: Batch Distillation At Constant Reflux

OBJECTIVES:

To operate a batch distillation unit at constant reflux.

To examine the change in top and bottom composition, and the height
equivalent theoretical plates (HETP) over time in a batch distillation.
To carry out mass balance calculations on the distillation unit.

PROCEDURES:
1. Perform the general start-up procedures (Section 3.1). Record the initial
volume and composition of ethanol-water mixture in the reboiler.
2. Set the heater power to 70%.
3. Once the distillation unit has reached stable condition, record the top and
bottom temperature.
4. Collect samples from the distillate and bottom product (Section 3.4). Do not
discard the samples. Instead, return all distillate and bottom samples into
separate containers for mass balance calculations later.
5. Measure the refractive index for both samples and determine their
compositions. This will constitute the composition at the beginning of the
experiment.
6. Set the reflux divider to give a reflux ratio of 1 (e.g. reflux timer 5 sec, distillate
timer 5 sec), and allow the process to run for 10 minutes.
7. Collect samples from the distillate and bottom product (Section 3.4). Measure
the refractive index for both samples and determine their compositions.
8. Measure the distillate flow rate as follows:
a)
b)
c)
d)

Close valve V4 and start the timer.

Collect the distillate in the measuring vessel B3 for a period of time.
Record the volume and time of the distillate to determine the flow rate.
Open valve V4.

9. Repeat steps 7 and 8 for every 10 minutes for at least 1 hour.

10. At the end of the experiment, measure the volume of liquid left in the reboiler
and volume of distillate collected. Remember to include all previous samples.
Also measure the refractive index for the combined distillate and determine its
composition.
ANALYSIS & DISCUSSION:
1. Use the sample table in Appendix C for data collection.
2. Using the X-Y equilibrium diagram for ethanol-water system, mark the top and
bottom compositions for each sampling time on the diagram. Observe the
change of composition over time in the batch distillation column.

BATCH PACKED DISTILLATION UNIT

3. Determine the theoretical number of plates for each sampling time in the
distillation column using the McCabe-Thiele method. Refer to Appendix D.2
for a step-by-step guide.
4. Calculate the height equivalent theoretical plates (HETP) by dividing the
effective column height with the number of theoretical plates.
5. Using the Rayleigh equation, calculate and plot the amount of ethanol left in
the evaporator against time.
6. Carry out a mass balance calculation on the distillation column at the end of
the experiment and compare with the experimental results.
Safety Considerations
1. The unit must be operated under the supervision of an authorized staff who
has been properly trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
3. Feed stock which severely affect PTFE, PFA and borosilicate glass are not to
be used.
4. The system should not be subjected to shock, sudden impact, vibration,
additional load, or permanent external action of aggressive vapours.
5. Always check and rectify any leak.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting
materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric
pressure.
10. Do not exceed the maximum coolant pressure of 2 bar(g) for the top
condenser (W3) and product cooler (W4).
11. Only a properly trained staff shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
12. Before any servicing, shut down the whole operation and let the system to
cool down and be properly ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
14. Leaking couplings should be carefully retightened. Replace any gaskets or
seals if necessary.
REFERENCES
1. McCabe, Smith & Harriott, Unit Operations of Chemical Engineering,
McGraw Hill, (Singapore), 2001.

BATCH PACKED DISTILLATION UNIT

2. Geankoplis C.J., Transport Processes and Unit Operations, Prentice Hall,

(Singapore), 1995.
3. Perry R.H., Perrys Chemical Engineers Handbook, McGraw Hill, (USA),
1997.
APPENDIX A
SAMPLE TABLE FOR PREPARATION OF REFRACTIVE INDEX VS COMPOSITION PLOT
Molar volume of ethanol = ____ mol/L
Molar volume of water

= ____ mol/L

Volume of
ethanol (mL)

Volume of
water (mL)

10

1.0

9.0

2.0

8.0

3.0

7.0

4.0

6.0

5.0

5.0

6.0

4.0

7.0

3.0

8.0

2.0

8.5

1.5

9.0

1.0

9.5
10.0

0.5
0.0

Mole fraction
ethanol

Mole fraction
water

Refractive index
(RI)

BATCH PACKED DISTILLATION UNIT

APPENDIX B
SAMPLE TABLE FOR EXPERIMENT 1: BATCH DISTILLATION AT TOTAL REFLUX

Heater
W1,W2
power
100 %
80 %
60 %
40 %
20 %

Distillate
Temp
(C)

Refract.
index

Bottom product
Mole
fraction

Temp
(C)

Refract.
index

Mole
fraction

HETP
(mm)

BATCH PACKED DISTILLATION UNIT

APPENDIX C
SAMPLE TABLE FOR EXPERIMENT 2: BATCH DISTILLATION AT CONSTANT REFLUX
Heater power = _____ %
Reflux ratio

Time
(min)

= _____
Distillate
Temp
(C)

Refract.
index

Mole
fraction

0
10
20
30
40
50
60

For mass balance calculations:

Initial conditions:
Reboiler volume

= _____ L

Reboiler composition = _____

Final conditions:
Reboiler volume

= _____ L

Reboiler composition = _____

Distillate volume

= _____ L

Distillate composition = _____

Bottom product
Flow rate
(mL/min)

Temp
(C)

Refract.
index

Mole
fraction

BATCH PACKED DISTILLATION UNIT

APPENDIX D.1
MCCABE THIELE CALCULATION FOR BATCH DISTILLATION AT TOTAL REFLUX
1. Start with the X-Y equilibrium diagram and
locate the following points on the X axis:
a) Distillate, D
b) Bottom product, B

B
Bottom

2. For total reflux, the operating line is the

same as the 45 line. Step off the
equilibrium stages from the distillate
point, D until it passes the bottom
product point, B.

Distillate

B
Bottom

Distillate

3. The number of theoretical stages required to achieve the separation obtained from the
distillation column can be calculated from the number of steps drawn on the diagram. In this
case, it is 3.

BATCH PACKED DISTILLATION UNIT

APPENDIX D.2
MCCABE THIELE CALCULATION FOR BATCH DISTILLATION AT CONSTANT REFLUX
1. Start with the X-Y equilibrium diagram
and locate the following points on the X
axis for every sampling time:
a) Distillate, D
b) Bottom product, B
(2 sets will be shown together here for
comparison)

D1
D2

B1
B2

2. The column above the reboiler

constitutes an enriching section. It
can be analysed the same way as in
a continuous distillation. The
enriching section operating line is:
xD
R
yn 1
xn
R 1
R 1
R is the reflux ratio.
Mark the Y axis intercept for the
x
operating line at D . Then extend
R 1
the operating line to the distillate
point, D. Repeat for each value of
distillate. For constant reflux ratio,
the operating lines should be
parallel.

D1
D2
x D1
R 1
x D2
R 1

B1
B2

BATCH PACKED DISTILLATION UNIT

3. By using the equilibrium curve, step off

the theoretical equilibrium stages from
each value of distillate to the
corresponding bottom product.
(D1 to B1, solid line)
(D2 to B2, dotted line)

4. Compare between the number of

theoretical stages at each sampling
time and each bottom composition.

D1
D2

B1
B2

5. Use the Rayleigh equation to find the amount of ethanol left in the reboiler at time t 1.
n0
n1

dn
n

dx

x0
x1

ln

n0
n1

n0

n1
exp

x0

dx

x1

y x

t0 = initial condition
t1 = final condition
x = bottom composition
y = top composition
n = total number of moles of ethanol in the reboiler
a) Calculate the values of

1
for every value of x.
y-x

1
against x.
y-x
c) For a change of composition between x1 and x0, find the area below the graph from x1
x0 dx
to x0. That will be the integration value of
.
x1 y
x

b) Plot a graph of

BATCH PACKED DISTILLATION UNIT

APPENDIX E
PHYSICAL PROPERTIES OF COMPONENTS
E.1

Properties of Pure Components

Property

Ethanol

Water

CH3CH2OH

H2O

Molecular weight (g/mol)

46.07

18.02

Specific gravity (20/4)

0.789

1.000

Normal melting point (C)

112.0

0.0

Normal boiling point (C)

78.4

100.0

Critical temperature (K)

514

647.13

Critical pressure (atm)

62.2

217.7

Formula

BATCH PACKED DISTILLATION UNIT

E.2

Equilibrium Data for Ethanol-Water System at 1 atm

Mole fraction ethanol

Temperature
(C)

Liquid phase

Vapor phase

100

0.0000

0.0000

95.5

0.0190

0.1700

89.0

0.0721

0.3891

86.7

0.0996

0.4375

85.3

0.1238

0.4704

84.1

0.1661

0.5089

82.7

0.2337

0.5445

82.3

0.2608

0.5580

81.5

0.3273

0.5826

80.7

0.3965

0.6122

79.8

0.5079

0.6564

79.7

0.5198

0.6599

79.3

0.5732

0.6841

78.7

0.6763

0.7385

78.4

0.7472

0.7815

78.2

0.8943

0.8943

(Source: Perrys Chemical Engineers Handbook, Table 13-1, pg. 13-12)

X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm

1.0000

0.9000

0.8000

Vapor mol fraction

0.7000

0.6000

0.5000

0.4000

0.3000

0.2000

0.1000

0.0000
0.0000

0.1000

0.2000

0.3000

0.4000

0.5000
Liquid mol fraction

0.6000

0.7000

0.8000

0.9000

1.0000

Batch Packed Distillation

E.3

Density of Ethanol-Water Mixture as a Function of Temperature and Composition

Ethanol
composition
(wt%)

20C

25C

30C

0.99823

0.99708

0.99568

0.98938

0.98817

0.98670

10

0.98187

0.98043

0.97875

15

0.97514

0.97334

0.97133

20

0.96864

0.96639

0.96395

25

0.96168

0.95895

0.95607

30

0.95382

0.95067

0.94741

35

0.94494

0.94146

0.93790

40

0.93518

0.93148

0.92770

45

0.92472

0.92085

0.91692

50

0.91384

0.90985

0.90580

55

0.90258

0.89850

0.89437

60

0.89113

0.88699

0.88278

65

0.87948

0.87527

0.87100

70

0.86766

0.86340

0.85908

75

0.85564

0.85134

0.84698

80

0.84344

0.83911

0.83473

85

0.83095

0.82660

0.82220

90

0.81797

0.81362

0.80922

95

0.80424

0.79991

0.79555

100

0.78934

0.78506

0.78075

Density (kg/m3)

(Source: Perrys Chemical Engineers Handbook, Table 2-110, pg. 2-112)

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