Continuous Bubble Cup Distillation

EXPERIMENT 3: CONTINUOUS BUBBLE CAP TRAY

DISTILLATION

INTRODUCTION

The Continuous Bubble Cap Tray Distillation Column is developed primarily for
teaching, training and research purposes. It is used for the separation of mixtures
at atmospheric pressure in a continuous operation. The unit has the following
special features, which are of particular value in training situations:

Direct heat input into the reboiler using steam and to be controlled by
reboiler temperature or pressure differential across the column.
Silver coated and vacuum jacketed bubble cap tray column minimizes
heat loss to the surroundings.
Sampling on each trays and on the bottom and top product to determine
the practical separation behaviour of the particular mixture.

The method of operation of a bubble cap tray distillation column for the
separation of liquid mixtures can be described in the following terms: The vapour
mixture rises from the reboiler, passes over the column trays and is fully
condensed in the condenser. The condensate runs down the column counter-
current to the vapour through the trays back into the reboiler. At each trays, 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 a bubble cap tray distillation column can be evaluated using the
number of theoretical plates required to achieve the same separation as the
actual 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.

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 Cooling
Water V17
V15
Cooling FI
TI
V18
17
Water 02

TI TI FI
16 V16 18 03
W2
KS-01
FI
04 TI
13

Vent V5 TI
sampl
TI 14
12
sampl
TI
11
sampl
TI
10
PdIC sampl
TI
01
09 K1 W3
sampl
W5 TIC
01
TI
08

TI
15

sampl
el. TI
07
FI sampl
01 TI
06 B5
sampl
TI
05
sampl
V4 TI
V6
TI 04
21 sampl
TI
03

TIC
02
TIA
20
V10 PIA
01
LS-
01
B2 B3
W4
B1
W1
B6
V3 PI TI FI
02 19 05
V19
V2 V11 Condensate
V20 CV01 Steam
V9 6 bar
V1 M
P1 B4
HS
1
V13
V12 V7

V14 V8

Figure 1: Process flow diagram for the continuous bubble cap tray distillation unit

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CONTINUOUS BUBBLE CAP TRAY 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. Cooling Water System – Laboratory tap water is used as the cooling media.
Hose connections are such that the cooling water enters the top condenser
(W2), distillate cooler (W3) and bottom product cooler (W4) in parallel. Adjust
each cooling water flow rates using valves V16, V17 and V18 to maximise
cooling and condensation. The temperature of the cooling water leaving the
condenser should not exceed 45°C.

Caution: In order to avoid water hammer, open the cooling water

valves slowly.

2. Heating Control – The heat input or steam flow rate into the reboiler can be
controlled using PID controls by either monitoring the reboiler temperature
(TIC-02) or pressure differential across the column (PdIC-01). Select the
heating control mode to either TIC-02 or PdIC-01 on the control panel, and
adjust the setpoint on the controller. The setpoints can also be adjusted on
the DAS if the control switch is at the Remote position.

3. Pump Settings – The feed flow rate can be adjusted by changing the stroke
and frequency settings on the pump. Adjust the stroke length between 0 and
100 mm by turning the knob on the pump, and set the frequency between 0 to
130 strokes/minute.

Caution: Remember to stop the pump operation before changing any

of the pump settings.

4. Feed Preheater (W5) – The feed temperature entering the distillation column
can be controlled by adjusting the temperature setpoint of TIC-01 on the
control panel.

5. 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.

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

EXPERIMENTAL PROCEDURES

General Start-Up Procedures

1. Ensure all valves are closed except V6, V11 and the ventilation valves.
2. Turn on the power for the control panel.
3. Prepare a 50 to 60 L mixture containing ethanol and filtered water at the
desired composition. Charge the unit as follows:
a) Open valve V3 and V12.
b) Open the quick closure cap on reboiler B1.
c) Pour all the ethanol-water mixture into reboiler B1 and observe the
overflow of liquid into the bottom product vessel B4 and pump P1.
d) Switch on feed pump P1 and adjust the stroke length and frequency.
e) Allow the mixture from vessel B4 to be pumped into the feed vessel B2
through valve V3.
f) Stop the pump as soon as the bottom product vessel B4 is almost empty.
g) Close valves V3 and V12.
4. Set the reflux divider KS-01 to total reflux. This is to prevent any distillate from
escaping when starting up the distillation column.
5. Let the cooling water flow into the condenser (W2) and product coolers (W3 &
W4) by opening valves V15, V16, V17 and V18.
6. Set the heating control mode to TIC-02 and adjust the temperature setpoint to
100°C, which is the boiling point of the heavy key component, water.
7. Drain any condensate in the steam line by opening valve V20.
8. Open the steam inlet valve V19 and let the flow of steam through the control
valve CV01 and coil heat exchanger W1. Allow the liquid in the reboiler to boil.
As the liquid boils, the liquid level in the reboiler will start to drop.
9. Observe the vapor rising from the boiling liquid into the distillation 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.
10. Check that the condenser has sufficient cooling water flow to minimize escape
of vapor into the vent.
11. Let the distillation column run until a stable condition is observed. The stable
condition is reached when all temperature indicators on the column give a
constant reading with an allowable ± 0.2°C fluctuation.

General Shut-Down Procedures

1. Set the reflux divider KS-01 to total reflux.

2. Keep the cooling water running through the condenser (W2) and product
coolers (W3 & W4).

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

3. Stop the steam input to the coil heat exchanger (W1) by adjusting the setpoint
at TIC-02 to 0°C and PdiC-01 to 0 mbar. Monitor the temperature drop in the
reboiler. Wait until it has cooled to room temperature.
4. Close the cooling water valves V15, V16, V17 and V18.
5. If necessary, drain all liquid from the reboiler B1 and product vessels B3 and
B4. The distillate and bottom product can also be recycled back into the feed
vessel B2 using pump P1 and opening valves V7 and V12.
6. Turn off the power for 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 the mixtures.

Sampling Procedures

Samples can be taken from the trays, distillate and the bottom product for
analysis:

1. Tray sampling:
a) Carefully insert a syringe needle through the gaskets in the sampling port.
b) Collect enough sample in the syringe and withdraw the needle.

2. Distillate sampling:
a) Drain any remaining liquid in the sampling valve V5.
b) Place a vial below valve V5.
c) Set the reflux divider to total distillate for a few seconds.
d) Open valve V5, collect enough sample and close the valve.
e) Switch the reflux divider back to the original setting.

3. Bottom sampling:
a) Drain the stagnated liquid in the sample line above valve V9.
b) Place a vial below valve V9.
c) Open valve V9, collect enough sample and close the valve. Be careful of
the hot liquid while collecting a sample.
d) Cool the sample by immersing the vial in cold water.

Note: Always re-cap the vials quickly after collecting samples to avoid
excessive evaporation of ethanol before analysis.

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

EXPERIMENT 1: Batch Distillation At Total Reflux

OBJECTIVE:
To determine the number of theoretical plates at total reflux.

PROCEDURES:
1. Perform the general start-up procedures as described in Section 3.1.
2. Once the distillation column has reached stable condition, record the trays,
top and bottom temperature.
3. Collect samples from the trays, distillate and bottom product (Section 3.4).
4. Measure the refractive index for all samples and determine their
compositions.

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 trays,
top and bottom compositions on the diagram and determine the number of
theoretical plates in the distillation column using the McCabe-Thiele method.
Refer to Appendix C.1 for a step-by-step guide.
3. Calculate the Murphree efficiency for each tray in the column.
4. Plot the temperature and composition profile for the distillation column.

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

EXPERIMENT 2: Continuous Distillation At Constant Reflux

OBJECTIVE:
 To operate a continuous distillation column at constant reflux.
 To carry out mass balance calculations on the distillation column.
 To examine the effects of reflux ratio and feed conditions on the number of
theoretical plates in a continuous distillation.

PROCEDURES:
1. Perform the general start-up procedures as described in Section 3.1.
2. Set the reflux ratio to 1 (e.g. 10 sec reflux & 10 sec distillate) at the reflux
divider controller (KS-01).
3. Switch on the feed pump P1 and adjust the pump stroke to 80 mm and
frequency to 40 strokes/min in order to obtain a flow rate of approx. 10 L/hr.
4. Once the distillation column has reached stable condition, record the trays,
top and bottom temperature.
5. Collect samples from the trays, distillate and bottom product (Section 3.4).
6. Measure the refractive index for all samples and determine their
compositions.
7. Measure the distillate and bottom product flow rate as follows:
a) Close the valve (V6 or V11) below the measuring vessel (B5 or B6) and
start the timer.
b) Collect the distillate or bottom product in the vessel for a period of time.
c) Record the volume of the liquid collected at that specific period of time to
determine the flow rate.
d) Re-open the valve (V6 or V11).
8. Repeat the experiment (steps 2 to 7) with a different value of reflux ratio.
9. Repeat the experiment (steps 3 to 7) with a different feed temperature by
switching on the feed preheater W5 and set the temperature to 60°C.

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 trays,
top and bottom compositions on the diagram and determine the number of
theoretical plates in the distillation column using the McCabe-Thiele method.
Refer to Appendix C.2 for a step-by-step guide.
3. Calculate the Murphree efficiency for each tray in the column.
4. Plot the temperature and composition profile for the distillation column.
5. Carry out a mass balance calculation on the distillation column and compare
with the experimental results.

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

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 cooling pressure of 2 bar(g) for the top condenser
(W2) and product coolers (W3,W4).
11. Only 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.

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

(Singapore), 1995.

APPENDIX A

SAMPLE TABLE FOR PREPARATION OF REFRACTIVE INDEX VS COMPOSITION PLOT

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

Molar volume of ethanol = _____ mol/L

Molar volume of water = _____ mol/L

Volume of Volume of Mole fraction Mole fraction Refractive index

ethanol (mL) water (mL) ethanol water (RI)

0 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 0.5
10.0 0.0

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

APPENDIX B

SAMPLE TABLE FOR EXPERIMENTS 1 & 2

Reflux ratio = _____

Feed flow rate = _____ mL/min
Feed composition = _____
Feed temperature = _____ °C

Temperature
Tray Refractive index Mole fraction
(°C)

Distillate
1
2
3
4
5
6
7
8
9
10
Bottom

Distillate flow rate = _____ mL/min

Bottom product flow rate = _____ mL/min

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

APPENDIX C.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 D
b) Bottom product, B
c) Individual tray compositions, N1-4
(only 4 will be shown here for clarity)

B
Bottom N4 N3 N2 N1 Distillate

2. For total reflux, the operating line is the

same as the 45° line. Using the tray
compositions, step off the actual D
equilibrium stages from the distillate
point, D until it reaches the bottom
product point, B (solid line).

Then, by using the equilibrium curve,

step off the theoretical equilibrium
stages (dotted line).

B
Bottom N4 N3 N2 N1 Distillate

3. The number of actual stages are shown by the number of steps drawn on the diagram, which is
the same as the number of trays found on the distillation column. An extra step is observed due
to the extra equilibrium stage in the reboiler.

yn yn 1
4. Murphree tray efficiency =
y n* yn 1 yn*
yn

yn+1

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

APPENDIX C.2

MCCABE THIELE CALCULATION FOR CONTINUOUS DISTILLATION AT CONSTANT REFLUX

1. Start with the X-Y equilibrium diagram and

locate the following points on the X axis:
a) Feed, F D
b) Distillate, D
c) Bottom product, B
d) Individual tray compositions, N1-4
(only 4 will be shown here for clarity)

B
Bottom N4 N3 F N2 N1 Distillate

2. The locus for the feed q-line is:

q xF
y x D
q 1 q 1
where q is defined as ratio between the
amount of heat needed to vaporize 1 mol
of feed at entering conditions to the
molar latent heat of vaporization of the
feed.

The value for q can be found as follows:

H V HF
q
H V HL B
in which HV is the feed enthalpy at dew
Bottom N4 N3 F N2 N1 Distillate
point, HL is the feed enthalpy at bubble
point and HF is the feed enthalpy at
entering conditions.

Draw the q-line orginating from the feed

point, F.

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

3. The enriching section operating line is:

R xD
yn 1 xn D
R 1 R 1

Mark the Y axis intercept for the

x
operating line at D . Then extend the
R 1
operating line to the distillate point, D. xD
R 1

B
Bottom N4 N3 F N2 N1 Distillate

4. The stripping section operating line can

be drawn by connecting the bottom
product point, B to the intersection of the D
q-line and the enriching section operating
line.

B
Bottom N4 N3 F N2 N1 Distillate

5. Using the tray compositions, step off

the actual equilibrium stages from the
distillate point, D until it reaches the D
bottom product point, B (solid line).

Then, by using the equilibrium curve,

step off the theoretical equilibrium stages
(dotted line).

B
Bottom N4 N3 F N2 N1 Distillate

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CONTINUOUS BUBBLE CAP TRAY DISTILLATION UNIT

6. The number of actual stages are shown by the number of steps drawn on the diagram, which is
the same as the number of trays found on the distillation column. An extra step is observed due
to the extra equilibrium stage in the reboiler.

yn yn 1
7. Murphree tray efficiency =
y n* yn 1 yn*
yn

yn+1

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APPENDIX D

PHYSICAL PROPERTIES OF COMPONENTS

D.1 Properties of Pure Components

Property Ethanol Water

Formula 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

Liquid heat capacity (J/mol.K) 112.4 (25°C) 75.38 (25°C)

65.21 (25°C)
Vapour heat capacity (J/mol.K)
73.15 (78°C) 34.02 (100°C)

Latent heat of vaporisation (J/mol) 42,100 (25°C) 44,045 (25°C)

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D.2 Equilibrium Data for Ethanol-Water System at 1 atm

Temperature Mole fraction ethanol

(°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: Perry’s Chemical Engineers’ Handbook, Table 13-1, pg. 13-12)

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

1.0000

0.9000

0.8000

0.7000
Vapor mol fraction

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 0.6000 0.7000 0.8000 0.9000 1.0000
Liquid mol fraction

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Continuous Bubble Cap Distillation

D.3 Density of Ethanol-Water Mixture as a Function of Temperature and Composition

Ethanol Density (kg/m3)

composition
(wt%) 20°C 25°C 30°C
0 0.99823 0.99708 0.99568
5 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

(Source: Perry’s Chemical Engineers’ Handbook, Table 2-110, pg. 2-112)

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Continuous Bubble Cap Distillation

D.4 Enthalpy of Ethanol-Water Mixture as a Function of Composition

Ethanol Enthalpy (kJ/kg)

composition
(wt%) Liquid Vapour
0 418.9 2675.0
10 371.7 2517.0
30 314.0 2193.0
50 285.9 1870.0
70 258.4 1544.0
90 224.7 1223.0
100 207.0 1064.0

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