ABSTRACT

In this experiment, we carry out the process of distillation to separate a liquid mixture consisting
of two solvents, methylcyclohexane (MCH) and toluene. The experiment includes determining
various boil-up rates and pressure drops in batch distillation, as well as the degree of foaming in
the tray after each power increment. A refractometer is then used to obtain the reading of the
refractive indices. Starting at 0.5kW, the power is increased up until 1.5kW with 0.25kW
increments, while collecting 100mL samples for every increment in order to find the refractive
indices. The degree of foaming was observed whether the tray was foaming gently, violently, or
flooding. In conclusion, the experiment proved a success as we deduced that the boil-up rate
depends on the power of the heater used. The boil-up rates will increase along with the heater
power used and similarly, the refractive index will also increase as the power input increases.

INTRODUCTION

The word ‘Distillation’ is often used in the chemical industry around the world but first
what is distillation? Distillation is a process where it requires liquid to convert into vapor then the
vapor condensed back into liquid form. This distillation process is often used in industries such as
water purification.

On the other hand, a distillation column is known as a tube that is used for distillation of a
liquid mixture so that it can be separated into its own components. This distillation column
contains several important parts such as trays or plates and condensers. This distillation column
comes along with the series of stacked plates where the liquid mixture enters the column and
flows on the plates while the vapor flows up and passes through the liquid via the holes in the
plates. The refractive index is being measured from every experiment that has been carried out to
determine the purity of the liquid component.

This distillation column allows for condensation and vaporization to happen before the
vapor can reach the condenser so that the more volatile liquid can be concentrated.

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 Furthermore, this distillation column has a series of stacked plates where its
function is to allow liquid holdup. This situation can let the vapor that flows up to encounter the
liquid for the vapor-liquid mass transfer. Example types of trays that can be used in distillation
columns are sieve trays, valve trays and bubble-cap trays.

Bubble cap trays Valve trays

In addition, foaming can occur in this distillation column when the power starts to rise due
to the high velocity of the vapor passing through the liquid or in other word the rate of
evaporation is way higher. Foaming in the distillation column can cause the efficiency of the
column drops and the column may flood.

Meanwhile in this distillation column experiment, refractive index is used for

identification purposes where this refractive index acts as the measurement of purity in the liquid
that has been examined. This refractive index can be measured using a refractometer.

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 OBJECTIVES

1. To determine the pressure drop of the distillation column at different boil-up rates.
2. To observe the degree of foaming on trays for every power level.
3. To determine the refractive index for every power increment for unknown concentration
of methylcyclohexane/toluene from the distillation column.

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 THEORY

Distillation is a process whereby components of a liquid mixture are separated through boiling
and condensation. The components in the liquid mixture can be separated as different substances
have different boiling points and different vapor pressures. Briefly, distillation consists of mainly
two processes, boiling and condensation. The liquid mixture is volatilized, often by heating, until
it reaches the boiling point of one of the components, where it will start changing into vapor.
When the vapor comes in contact with a solid surface, it will turn back into liquid, giving a
purified component in liquid form. A simple apparatus set up can be prepared to demonstrate the
process of distillation. The set up consists of a flask, distillation head, condenser, and sample
collector as in Figure 1. To monitor the temperature of the mixture, a thermometer is included in
the set up. The simplest process that applies the concept of distillation is the purification of water,
where water is distilled to extract pure water from other impurities.

According to (Pubchem, 1997), the boiling point of toluene and methylcyclohexane are 111°C
and 101°C respectively. The binary mixture of methylcyclohexane-toluene is used in this
experiment to further demonstrate the concept of distillation.

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 VMCH = Volume of Methylcyclohexane, mL

VTol = Volume of Toluene, mL

MWMCH = Molecular Weight of Methylcyclohexane, 98.189g/mol (PubChem, 1997)

MWTol = Molecular Weight of Toluene, 92.141g/mol (PubChem, 2002)

ρMCH = Density of Methylcyclohexane, 770 kg/m3

ρTol = Density of Toluene, 867 kg/m3

The power input of the reboiler is set at 0.5W increments to heat up the methylcyclohexane-toluene
mixture at various boil-up rates.

The most volatile component, which is methylcyclohexane in this case, will vaporize first until
equilibrium is achieved. This vapor rises in the boiler before flowing into the unit at the bottom of
the column. depending on the boil-up rate, the velocity of the vapor passing through the column
varies. As the vapor passes straight upward through the liquid on the sieve trays (Tham M. T.,
1997), restriction occurs on the holes of the trays causing pressure drop.

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The total pressure drop across the tray is the sum of that caused by the restriction of the holes in
the sieve tray, and also that caused by passing through the liquid (foam) on top of the tray. The
pressure drop should increase as the boil-up rate increases. as the vapor exits from the column, a
condenser will cool it down, and form a condensate (liquid) which will be stored in the reflux
drum (Figure 2).

To measure the refractive indices, the refractometer is used. It works using the principle of light
refraction through liquids (ProSciTech, 2014). The critical angle of the liquid is measured, where
different concentrations will present different readings. The readings are observed and recorded.

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 APPARATUS AND MATERIALS

APPARATUS

● Automatic digital refractometer

● Continuous distillation column
● Stopwatch
● 100ml measuring cylinder
● Dropper

MATERIALS

● Distilled water
● 10L (50 mole % methylcyclohexane - 50 mole % toluene)
● Pure methylcyclohexane
● Pure toluene
● 25 mole %, 50 mole % and 75 mole % of methylcyclohexane

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 METHODOLOGY

GENERAL START UP

1. The ELCB switch was moved to the UP position to turn on the electrical power to the
control console. The LOW LEVEL lamp in the reboiler, or the reboiler power, reflux
timer, column temperature and process temperature displays are all illuminated.
2. The valves (V1 to V15) were in a closed position.
3. The cold-water supply in the laboratory was turned on and the control flow valve (V5)
was opened to allow maximum flow into the condenser via flowmeter (F11). The leaks
were examined.
4. The manometer tub was filled until it reached an equal level nearly halfway up the scales.
The V6 and V7 were closed,
5. The power to the reboiler heater was turned on at the console and the power was adjusted
to 1.50 kW. The water in the reboiler begins to heat up which can be seen on the process
temperature digital by selecting (T9).
6. The pressure difference in the manometer was measured when valves V6 and V7 were
opened. The V6 and V7 closed down.

EXPERIMENT A

1. The experiment began when the power of the control panel was switched on. All the
valves closed except valve 10 on the reflux tube and the boiler loaded with 10 liters of
distilled mixture.
2. The temperature selector switch was adjusted to T9, the temperature in the boiler.
3. Valve V5 was opened allowing about 3 liters of cooling water to enter the condenser each
minute.
4. When the power controller on the control panel was turned on, the reboiler heating
element that was completely anticlockwise was shifted to the 'power' on position by
turning on the power heating element.
5. The power controller was adjusted to a reading of about 0.5kW, and the contents of the
reboiler were warmed up for 10 minutes, as measured by the temperature readout meters.
6. After 10 minutes, valves V6 and V7 were simultaneously opened, resulting in pressure

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 drops on the manometer for the top and bottom. The pressure drop was recorded.
7. The cold distillate was returned to the top of the column and cascaded down the trays,
forming a liquid level on the trays as the bubble vapor passed through the liquid. The
degree of foamation was measured and recorded.
8. A 100ml sample was collected using a measuring cylinder through valve V3 (opened
valve), while the sample collected, time was recorded and the boil-up rate (L/hr) was
calculated based on the time taken.
9. Refractometer was used to determine the refractive index (RI) of the collected sample.
Before RI testing, the refractometer was adjusted by zeroing the instrument with distilled
water.
10. The experiment was repeated using power of 0.75kW, 1.00 kW, 1.25 kW and 1.50 kW.

EXPERIMENT B

1. The volume of each mixture was calculated.

2. R.I. was calculated using small amounts of methylcyclohexane at 25 mole %, 50 mole %,
75 mole % and 100 mole %.
3. Pure Methyl Cyclohexane and Pure Toluene were tested for the Refractive Index (R.I.).

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 RESULTS

Experiment A

Power Boil-up Rate Pressure Drop Degree of Refractive

(kW) (litres/hr) Foaming on Index
(cm H2O) Top Trays
Bottom Overall

0.50 2.9508 63 Gentle 1.43706

0.75 7.9017 72 Gentle 1.43986

1.00 52.1739 203 Violently 1.45046

1.25 67.5422 152 Violently 1.45224

1.50 42.5532 138 Flooding 1.45234

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 Figure 1: Graph of Pressure Drop Vs Boil-up Rate

Experiment B

Concentration of Volume (mL) Refractive Index (R.I)

Methylcyclohexane (%)

Methylcyclohexane Toluene 1st 2nd Average

0 0.00 100 1.49600 1.49640 1.49620

25 28.49 71.51 1.47537 1.47479 1.47508

50 54.41 45.59 1.45531 1.45474 1.45503

75 78.19 21.81 1.43642 1.43778 1.43710

100 100 0.00 1.42320 1.42320 1.42325

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 Figure 2: Graph of Refractive Index Vs Mole Fraction of Methylcyclohexane

CALCULATIONS

Experiment A

Power (kW) Boil-up Rate Times (s)

(liters/hr)

0.50 2.9508 122

0.75 7.9017 45.56

1.00 52.1739 6.9

1.25 67.5422 5.33

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 1.50 42.5532 8.46

a) Power: 0.5 kW

b) Power: 0.75kW

c) Power: 1.00kW

d) Power: 1.25kW

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e) Power: 1.50kW

Experiment B

Molecular Weight Methylcyclohexane (MCH) : 98.19 g/mol

Molecular Weight Toluene (tol) : 92.15 g/mol

Density MCH: 0.774 g/mL

Density Tol: 0.867 g/mL

1. 0% Methylcyclohexane: 100%Toluene

Because of the mixture solution is contain 100% Toluene, we can neglect the volume
Methylcyclohexane

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2. 25% Methylcyclohexane: 75%Toluene

3. 50% Methylcyclohexane: 50%Toluene

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4. 75% Methylcyclohexane: 25%Toluene

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 5. 100% Methylcyclohexane: 0%Toluene

Because of the mixture solution is contain 100% Methylcyclohexane, we can neglect the volume
Toluene

DISCUSSION

For this experiment, at each stage of the process, a sequence of flash-vaporizations are arranged
in such a way that the vapor and liquid product are countercurrent to each other. Theoretically, the
degree of separation was based on the volatility of the two components involved where the most
volatile component will be boiled towards the top of the column as a vapor thus separating it with
the least volatile component. The product collected at the bottom part of the distillation column in
the form of a liquid will be considered as the least volatile component.

Generally, our experiment was divided into two which are experiment A and experiment B.
Experiment A's main goal is to figure out how much pressure drops over the distillation column
at different boil-up rates. The degree of foaming as one of the parameters also needs to be
observed for each of the power supply increases. A mixture of toluene and methylcyclohexane
were boiled up in the distillation column at power supply of 0.5KW, 0.75KW, 1.00KW, 1.25KW
and 1.50KW. As the result obtained, a graph of pressure drop versus boil up rate is plotted.

At first, the graph shows a moderate increase at the first two points which will then surge rapidly
before returning to a slight dip. The pressure drop should be increased as the boil up taken
increases. The error might have occurred when the pressure drop values were taken. To assure
data accuracy, the value shown on the manometer should be allowed to stabilize first before the
value was taken.

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Different power supplies also affect the degree of foaming inside the distillation column and the
refractive index of the system. At 0.5KW and 0.75KW, the same degree of foaming was observed
to be ‘gentle’. The degree of foaming started to foaming ‘violently’ over the trays as the power
supply increased to be 1.00KW and 1.25KW before ‘flooding’ occurred at 1.50KW. From that,
we can conclude that as the power supply increases, the upward flow of the vapor also increases.

On the other hand, the refractive index of the system was also being taken from the condensate
mixture using a refractometer which will then be compared with the refractive index obtained in
experiment B. For experiment B, we need to find out the refractive index of various
concentrations of methylcyclohexane also by using a refractometer. Based on the result obtained,
a graph of refractive index versus mole fraction of Methylcyclohexane is plotted. From that, we
can see that the graph undergoes a constant drop along the experiment conducted.

After comparing the calibration curve from experiment B with the value of the refractive index
from experiment A, a major observation can be seen where we can conclude that the condensate
mixture collected in experiment A having a refractive index value ranging from 1.43 to 1.45 is a
methylcyclohexane. This is due to the value obtained being much closer to the value of RI for
50% - 100% of methylcyclohexane/toluene concentration. Therefore, it is proved that the top
product of the distillation column will be methylcyclohexane as it is more volatile and has lower
boiling point compared to toluene.

CONCLUSION

In summary, all the objectives were successfully achieved. From the results, it shown that
the boil-up rate has been calculated by using data and formula given which is 2.9508 L/hr, 7.9017
L/hr, 52.1739 L/hr, 67.5422 L/hr and 42.5532 l/hr from 0.5, 0.75, 1.00, 1.25 and 1.5kW of power
rising. Plus the pressure drops are 63, 72, 203, 152 and 138 cmH2O and the degree of foaming
whether it is violently or flooding is observed. The refractive index is 1.49620, 1.47508, 1.45503,
1.43710 and 1.42325. From the pressure drop against boil-up rate graph, we can see that when
pressure drop increases, the boil-up rate also increases until it reaches flooding. Beside, foaming
occurs when the components form a stable foam. Thus efficiency of the column drops and the
column may flood.

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 RECOMMENDATION

While conducting the experiment, students should wear appropriate PPE. Due to the high
temperature and possibly harmful nature of the distillation column experiment, proper PPE is
strongly advised. To find the precise finding and avoid error, eyes should be placed perpendicular
to the scale while reading the pressure drop. In order to improve accuracy, the sample should be
examined many times. For the best results, proper measuring apparatus should be used for
measuring the quantity of toluene or methylcyclohexane to make the baseline.

REFERENCES

1. Tonya Yirka, April 25, 2017. What Causes Foaming in a Distillation Column? Retrieved
from https://sciencing.com/causes-foaming-distillation-column-8697646.html
2. M.T.Tam (2016). Distillation Column Internals. Retrieved from
https://www.rccostello.com/distil/distilint.htm
3. 13 January, 2022. Microsoft Word - 2219_EXP5_Simple_Distillation__. Retrieved from
https://web.mst.edu/~tbone/Subjects/TBone/chem226/distproc.pdf
4. Tham, M. T. (October, 1997). Basic Distillation Equipment and Operation. Retrieved 28
March, 2018, from COSTELLO: https://www.rccostello.com/distil/distileqp.htm
5. UiTM Faculty of Chemical Engineering Laboratory Manual: Heat & Mass Transfer
Laboratory (CHE504), page 10

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APPENDIX

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