ABSTRACT

Distillation column is used to determine pressure drop for various boil-up rates in
batch distillation. The degree of foaming on trays for each power increment also can be
determined. In order to study the pressure drop of the column, the power was set to 0.5 kW
and then 0.75, 1.00, and lastly 1.25 kW. For each power, the sample was collected until it
reached 90mL and then the procedures were repeated for each increment. The samples
collected were tested for its Refractive Index. It is observed that degree of foaming increases
when the power was increased. The degree of foaming at 0.5 kW was gentle as opposed to
the others, where the foaming starts to become vigorous. Finally, the refractive index for pure
MCH and toluene was determined in order to match the mixture obtained from the sample.

INTRODUCTION
Distillation is a process of separating a mixture into two or more products that have
different boiling points, by partial vaporization of a liquid mixture and/or by partial
condensation of a gas mixture thereby rendering liquid phase richer in less volatile (with
higher boiling point) component and the vapor phase is richer in more volatile (with lower
boiling point) component. Distillation probably accounts for 90% of all separation processes
in the chemical industry, and is also a significant user of energy due to the necessary heating
involved. This process is conducted by using the Distillation Column apparatus.
The column is consisted of bubble cap trays, reboiler, product and feed tank, reflux
splitter, and condenser. Each bubble cap allows vapor to pass upward from the tray below
and condense while allowing liquid to pass back. Two heat exchangers are located above the
column. The second exchanger acts as a condenser. It condenses the vapor leaving the first
exchanger using cooling water. The condensate flows into the reflux tank. Then it can be
refluxed back to the top of the column or directed to the product tank.

Figure 2.1: Schematic Diagram of Distillation Column

There are two principal methods to carry out distillation process. The first one is
producing a vapor by boiling the liquid mixture to be separated and condensing the vapors
without allowing any liquid to return to the still. That means, there is no reflux, and this
process is called batch distillation. The second method is part of the condensate returns to the
still under such conditions that this returning liquid is brought into close contact with the
vapors on their way to the condenser. For systems containing only two components,
distillation can be conducted by using either of these methods as a continuous steady-state
distillation process, including single-stage partial vaporization without reflux (flash
distillation) and continuous distillation with reflux (rectification).
Examples of distillation process in the industry are: separation of a mixture of liquid
air into nitrogen, oxygen, argon; the distillation of crude fermentation broths into alcoholic
spirits; and the fractionation of crude oil into useful products, such as gasoline and heating
oil. In the organic lab, distillation is used to purify solvents and liquid reaction products.

OBJECTIVES
The purposes of this experiment are:
1. To determine the pressure drop of the distillation column for various boil-up rates in
batch distillation.
2. To plot the curve relating the pressure drop and the boil-up rates.
3. To observe the degree of foaming on trays for each power increment.
4. To determine the refractive index for unknown concentration of
methylcyoclohexane/toluene from the distillation column for each power increment.

THEORY
The total pressure drop across each tray is the sum of that caused by the restriction of
the holes in the sieve tray, and that caused by passing through the liquid (foam) on top of the
tray.
As the velocity of the vapours passing up the column increases then so does the
overall pressure drop. The velocity is controlled by varying the boil-up rate which is done by
varying the power input to the boiler. Under condition with no liquid present, the sieve tray
will behave like an orifice in that pressure drop will be proportional to the square of velocity.
Due to the fact that there is a liquid head however, this square relationship does not become
apparent until the head of liquid has been overcome and foaming is taking place. In a graph
of pressure drop vs boil-up rate (log/log), at low boil-up rates the pressure drop will remain
fairly constant until foaming occurs when the pressure drop would be expected to rise sharply
for unit increases in boil-up- rate.
For the system methylcyclohexane/toluene, mixture of known concentration can be
made up and their refractive index measured. The refractometer measure the critical angle of
the liquid under test and each concentration will show a different critical angle. From this, the
Refractive Index can be found.

APPARATUS

b
g
f

c
d
e

Figure 5.1: Distillation Column Apparatus

1. Distillation Column
a. Condenser
b. Electromagnet (reflux control)
c. Reboiler
d. Cooler
e. Bottom
f. Distillate
g. Feed
2. Refractometer
3. Refractor
4. 1- 250ml Measuring Cylinder graduated in mls
5. 1- 1000ml Beaker graduated in mls
6. Stopwatch / timing device

MATERIALS
1. Methlcyclohexane
2. Toluene

PROCEDURE
6.1 General Start-Up Procedures
1. It is made sure that all valves are closed.
2. The power for the control panel is turned on.
3. A 30-40 L mixture containing methylcyclohexane and toluene at the desired
composition is prepared. The unit is charged as follows:
i)

The charge port cap at the reboiler B1 is opened, and the reboiler is filled up to
the level of the internal overflow height.

ii)

The remaining methylcyclohexane-toluene mixture is poured into the feed

vessel B2 through the feed charge port.

4. The reflux divider KFS-101 is set to total reflux. This is to prevent any distillate from
escaping when starting up the distillation column.
5. The cooling water is let to flow into the condenser W2 and product coolers W3
and W4 by opening valves V13, V14 and V15.
6. The tip of the level switch is made sure to be located below the reboiler
equator, which is at the liquid inlet from the cartridge heaters.
7. The cartridge heaters at W1 are switched on. The liquid in the reboiler is allowed to
boil.
8. The vapor rising from the boiling liquid into the distillation column is observed.
When the vapor reached the condenser, it condensed and flowed back into the column
as liquid. Mass transfer took place between this liquid and vapor phase in the column.
9. The condenser is checked if it had sufficient cooling water flow to minimize
escape of vapor into the vent.
10. The distillation column is 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 fluctuation of 0.2C.

6.2 General Shut-Down Procedures

1. The reflux divider KFS-101 is set to total reflux.
2. The cooling water is kept running through the condenser W2 and product
coolers W3 and W4.
3. The cartridge heaters W1 are switched off. The temperature drop in the
reboiler is monitored until it cooled down to less than 50C.
4. The cooling water valves V13, V14 and V15 are closed.
5. All liquid from the reboiler B1 and product vessels B3 and B4 are drained by
opening valves V6, V9 and V12. The liquid in the pipelines are also drained by
opening valves V5, V8, V10 and V11. The liquid can be re-mixed and recycled
for future use.
6. The power for the control panel is turned off.

6.3 Experiment A: Determining Column Pressure Drop in Batch Distillation

1. The general start-up procedures as in Section 6.1 are performed.
2. The power is set to 0.5 kW.
3. The distillation column is let to reach stable condition after 15 minutes.
4. Valves V6 and V7 are opened. The pressure drop of the distillation column is
recorded.
5. Valves V6 and V7 are closed.
6. To measure for the boil-up rate, valve V3 is opened, the time is started as sample is
collected by using a 100 mL measuring cylinder.
7. The time is stopped after 90 mL of sample is collected, valve V3 is closed.
8. About 5 drops of the sample is taken to measure for the refractive index in Section
6.4, while the balance is put into the conical flask provided.
9. The degree of foaming on the trays is observed.
10. All steps above are repeated with power of 0.75, 1.0, 1.25, and 1.5 kW.
11. Graph of pressure drop against boil-up rate is plotted.

6.4 Experiment B: Determining Unknown Concentration

a) Finding Refractive Index using Refractometer

1.

The refractive index value is taken by using automatic digital refractometer for
each power sample of product at each power increment.

2.

The refractometer is run:

i. The surface is cleaned using distilled water.
ii. The power is switched on.
iii. ZERO setting is pressed (SWL key).
iv. Start key is pressed after placing the sample. The refractive index value is then
recorded.
v. It is cleaned and the power is switched off.

b) Non-distillation Mixing of Methylcyclohexane and Toluene

1. 10 mL of solution is assumed equal to 10 mol%.
2. 0 mol% methylcyclohexane is mixed with 100 mol% toluene using conical flask.
3. The solution is carefully stirred.
4. Steps 2 and 3 are repeated with :
i.

25 mol% methylcyclohexane + 75 mol% toluene

ii.

50 mol% methylcyclohexane + 50 mol% toluene

iii.

75 mol% methylcyclohexane + 25 mol% toluene

iv.

100 mol% methylcyclohexane + 0 mol% toluene

5. The refractive index reading for each mixture is obtained using the refractometer.
6. Graph of refractive index against percentage concentration of methylcyclohexane
is plotted to determine the unknown concentration.

RESULTS

Experiment A: determining column pressure drop

Power (kW)

Boil-up rate

Pressure drop

(mL/s)

(cm H2O) (Top

Bottom Overall)

Degree of forming
on tray

Refractive
Index
(R.I)

0.50

0.692

64

Gentle

1.43950

0.75

2.8125

67

Flooding

1.43958

1.00

2.922

189

Flooding

1.44374

1.25

3.913

147

Flooding

1.45317

1.50

6.429

143

Stable

1.46168

pressure drop (cmH2O)

Pressure drop vs boil-up rate

200
180
160
140
120
100
80
60
40
20
0

y = 13.487x + 76.769
R = 0.264

boil-up rate (mL/s)

Experiment B: determining mixture compositions

Concentration

Refractive Index
(R.I)

100% MCH

1.42312

100% toluene

1.49676

25% MCH

1.47276

50% MCH

1.45245

75% MCH

1.42743

SAMPLE CALCULATION

For 25 mol percent methylcyclohexane and 75 mol percent toluene

Molecular weight methylcyclohexane = 98.19
Molecular weight toluene = 92.15

Density of methylcyclohexane = 0.774 g/ml

Density toluene = 0.867 g/ml

25 =
Thus,
25 =

3=

=3x

=3x

=
Thus for 100 ml of mixture, quantities required will be:

Methylcyclohexane =

x 100

= 71.4286 ml

Toluene =

x 100

= 28.5714 ml

DISCUSSIONS

From the graph plotted, as the power increases, the from 0.50 kW to 1.50 kW, the
boil-up rate increases from 0.692 ml/s to 6.429 ml/s. for pressure drop, at the initial of the
experiment, the pressure is increases at boil-up rate of 0.692 until 2.922 ml/s, but then the
pressure drop from 189 cm H2O to 147 cmH2O and 143 cmH2O. The degree of forming on
trays was gentle at first but then it was flooding at the middle of the experiments and then
become stable again at the end of the experiment.
At the initial of the experiments, the pressure drop is not really occur, because the
heat generated from the power that is used to boil up the solutions is not so high. Therefore,
the pressure was needed to boil-up the solutions so that the required distillate can be
collected. But, when the power was set up at higher value, the boil-up rate getting higher and
the pressure start to drop as the boil- up rate reached its needed rate. At this point, the
pressure start to drop drastically as the distillate was collected.

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At first, the degree of forming on tray was gentle, this is because, the solutions still
not reached its boiling point and the boil-up rate was quite low during this time, but then, in
the middle of the experiment, the solutions on the tray start to flooding, this is because, the
power is continuous increases and the boil-up rate was getting higher and at the end of the
experiment, the degree of forming on tray getting stable again.
Every time the distillate collected, its refractive index (RI) was tested using
refrectometers to test the mixture compositions. The value for the mixture can be compared
with experiment B. In experiment B, the RI of pure MCH, pure toluene, 25 % MCH, 50 %
MCH and 75 % MCH was tested. From the result, it can be clearly seen that, the higher the
percentage of MCH, the lower the refractive index. This is because; the density of toluene is
higher than MCH. From experiment B, we know that the higher the boil-up rate, the higher
the percentage of toluene being distillate.

CONCLUSION
From the experiment, the objective was to determine the pressure drop over the distillation
column for various boil-up rates in batch distillation. From the data collected, graph of
pressure drop versus boil-up rate was plotted and the RI also calculated to determine the
mixture compositions. In conclusion, the experiment was a success because the pressure drop
was successfully determined with various boil-up rates. Therefore, the objective was
successfully determined.

RECOMMENDATIONS
These are some recommendations that should be done while carrying out this experiment:
1) Avoid direct contact with the distillation column because it is hot.
2) Always re-cap the vials quickly after collecting samples to avoid excessive
evaporation of ethanol before analysis.
3) While measuring the volume of methylcyclohexane, use a glove to hold the
measuring cylinder.
4) Before using the refractometer, make sure to clean the surface first using distilled
water.
5) Collect the unused samples of mixture in a conical flask so that it can be reused.
6) For next experiment, the procedures should be repeated another two times, so that
we can compare the results and the values that we get are accurate.

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REFERENCES

There are a few sources used as references in the making of this report:
1) Geankoplis, C.J. (2003). Transport Processes and Separation Process Principles
(includes Unit Operations): 4th Edition. Pearson Education International.
2) Treybal, R.E. (1980). Mass Transfer Operations: 3rd Edition. McGraw-Hill, New
York.
3) McCabe & Smith, J. (1976). Unit Operations of Chemical Engineering. McGrawHill, New York.
4) OShea, S.M. (2007). Distillation Analysis. Retrieved December 2, 2012, from
http://www.wpi.edu/Pubs/E-project/Available/E-project-081607132906/unrestricted/MQPDDB2371Final.pdf
5) Tham, M.T. (2009). Distillation. Retrieved December 2, 2012, from
http://lorien.ncl.ac.uk/ming/distil/distil0.htm

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APPENDIX

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