UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

HEAT & MASS TRANSFER LABORATORY
(CHE504)
EXPERIMENT : DISTILLATION COLUMN EXPERIMENT
GROUP : EH2204C
NAME : NUR RAMADAN BT ARIFFIN (2019582215)
NUR AMALINA BT MOHD AZAM (2019582259)
NURSYAQIRA BT RAMLE (2019582319)
NUR SYAHIRAH AMALINA BT ROSLAN (2019167991)
GEBRINA RIZKIA BT MUHAMMAD NURDIN(2019663812)
DATE PERFORMED : 25TH OF OCTOBER 2019
PROGRAMME/CODE : EH220
SUBMIT TO : DR SITI NOOR SUZILA BINTI MAQSOOD ALHAQUE

No. Title Allocated Marks (%) Marks

1 Abstract/Summary 5
2 Introduction 10
3 Aims 5
4 Theory 10
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 5
11 Recommendations 5
12 Reference / Appendix 5
TOTAL MARKS 100

Remarks:

Checked by:

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Date:
 TABLE OF CONTENT

1. ABSTRACT…………………………………………………………….…………………2
2. INTRODUCTION…………………………………………………………………………3
3. OBJECTIVES……………………………………………………..…..…………………..5
4. THEORY……………………………………………………………..……………………6
5. MATERIALS AND APPARATUS……………………………….………………………8
6. METHODOLOGY…………..…………………………………………………………...10
7. RESULTS…………………………………………………………….…………………..13
8. CALCULATIONS……………………………………………………………………….16
9. DISCUSSION……………………………………………………………………………18
10. CONCLUSION……………………………………………………….………………….22
11. RECOMMENDATIONS…………………………………………..…………………….23
12. REFERENCES………………………………………………………..………………….24
13. APPENDICES……………………………………………………………………………25

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 1. ABSTRACT

Distillation is a separation process which involved a mixture of liquid or vapor or

more substance which then will be separated into its desired component fractions through
boiling and condensation. In this experiment, mixture of methylcyclohexane (MCH) and
toluene were used as reactants and fed into the distillation column. This experiment was
conducted to determine pressure drop for various boil-up rates in a batch distillation, to
observe the degree of foaming on trays each time the power increased and the measurement
of Refractive Index. The experiment consists of two parts. The first part is to determine
pressure drop in batch distillation while the second part is to determine unknown
concentration. The power will be vary to study the pressure drop inside the column. The
power was set up to 0.5kW, 0.75kW, 1.00kW, and 1.25kW respectively. Every increment of
power, 100mL of sample was collected after 5 minutes to measure the Refractive Index. It is
observed the degree of foaming was increased with the increment of power. In experiment B,
pure MCH, pure toluene, 25% MCH, 50% MCH and 75% MCH were tested for their
Refractive Index to compare the value with the previous sample from experiment A. It can b e
concluded that this experiment has achieved its objectives which is the boil-up rates has a
correlation with the power used for the distillation column. The greater the heater power, the
higher the boil-up rates will be. The refractive index values also shows an increment when
the power input increase.

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 2. INTRODUCTION

The distillation column experiment is a purification process to separate a binary

mixture of methanol and water. After becoming familiar with the column and its setup,
several experiments were conducted to observe the operation and performance of the column.
The holding reservoir, which contained the methanol-water mixture, was analysed to
determine the composition of the liquid. A boiling point test was performed on the mixture to
determine the unknown composition of the liquid. The data obtained from the boiling point
test will be used to determine the composition using an x, y, T data plot for methanol-water.
Two experiments were performed during the four-week period. A batch distillation was
performed first. The distillation column was monitored until the reboiler started to boil. The
time was recorded and the volume change was monitored in the reboiler. The second
experiment involved a continuous distillation experiment. The column was allowed to reach
steady state. Once steady state was obtained the time was recorded and the compositions of
each tray were determined during a specific time interval. The collection of this data helps to
determine the tray efficiency and plot the separation line on the equilibrium diagram. The
diagram of our system is given on the following page as Figure 1.

Figure 1: Illustration of distillation column.

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 This separation of distillation process use heating power from reboiler to separate the
vapor and liquid phase. Heating element installed at the bottom of column to ensure the liquid
mixture evaporates in the whole column. The vapor phase will rise up into the condenser and
the product will be entering into the distillate tank, meanwhile the liquid will go downward as
bottom products. The process will be continuous to ensure high purity of product. There are
two heat exchangers in the distillation column. First is reboiler to heat up the liquid that go
downward and the function of the second exchanger acts as condenser which allow the vapor
will be turn into condensate or in liquid form. Then the reflux tank will be filled with the
condensate that flow from condenser. The electromagnetic controlled in the column by
switching of on and off controlled the reflux ratio. The remaining from the reflux tank then
turned back to the top of the column. The separation behavior of the column can be analyzed
by the sample analyzed for each stage. Therefore, the refractive index of every sample can be
analyzed by refractor meter. The rectification is the mass transfer between the two phases in
equilibrium.

From the distillation column system, there are two principle methods that need to be
followed in order to carry out the experiment which is batch distillation method and
continuous steady state distillation process. Batch distillation process is the process when a
mixture is distilled to separate it into its component fractions before the distillation still is
again charged with more mixture and the process is repeated. Continuous steady state
distillation process is ongoing separation in which a mixture is continuously (without
interruption) fed into the process and separated fractions are removed continuously as output
streams.

In the industries, there are many categories of products that use distillation for
separation such as petroleum refining, petrochemical, coal tar processing, liquor production,
liquified air separation, hydrocarbon solvents production. In generally, the typical aim of
using distillation column is to remove the light component from mixture of heavy
components. Other example of distillation process in industry is distillation within the
pharmaceutical industry which is often used in solvent swap because the reaction of solvent is
usually different to the crystallization solvent or to concentrate a solution before
crystallization.

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 3. OBJECTIVES

1. To determine the pressure drop over the distillation column for various boil-up rate.
2. To determine the mixture compositions by using refractometer.

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 4. THEORY

The unit operation distillation is a method used to separate the components of a liquid
solution, which depends upon the distribution of these various components between a vapour
and liquid phase (Geankoplis, 1993). Distillation is a physical process used to separate
chemicals from a mixture depending on the differences in volatilities of the components that
make up the mixture. In the distillation process, a volatile vapour phase and a liquid phase
that vaporizes are involved (Geankoplis, 1993). Their operation is based on the difference in
boiling temperatures of the liquid mixture components. The boiling point of
methylcyclohexane is 101°C (PubChem, 1997) while toluene is 111°C (PubChem, 2002).
The binary mixture of methylcyclohexane-toluene is used in the experiment to understand the
concept of distillation.

Where:

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/m

Then, the methylcycloheane-toluene mixture is heated at varying boiling-up rate which is

done by varying the power input to the reboiler.

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 In order to determine which component reach equilibrium, the component with the
most volatile will reach the equilibrium and in this case, methylcyclohexane reach
equilibrium. The vapour raised in the boiler flow unit at the bottom of the column. The
velocity of vapour that passes through the column depends on the boil –up rate. Pressure drop
will be detected as the vapour passes through the column on the sieve trays due to the
restriction occurs on the hole.

The pressure drop is expected to increase as the boil –up rate increases. Vapour will
cooled the condenser as it exit the top of unit. The condensate is then restored in reflux drum.
The refractive indexes can be measured for mixtures of known concentration made up of
binary system. Here, the refractometer works using the principle of light refraction though
liquids. The critical angle of the liquid can be measured under the test and different
concentration will yield to different reading of the critical angle.

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5. MATERIALS AND APPARATUS

Figure 2: Continuous Distillation Column (UOP3CC)

Figure 3: Automatic Digital Refractometer RX-5000a

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5.1 MATERIALS

a) 10L of 50 mole percent Methylcyclohexane- 50 mole percent Toluene.

b) Pure methylcyclohexane

c) Pure Toluene

d) 25 mole percent, 50 mole percent and 75 mole percent methylcyclohexane

e) Distilled Water

5.2 APPARATUS

a) Continuous Distillation Column (UOP3CC)

b) 100 mL of measuring cylinder

c) Stopwatch

d) Automatic Digital Refractometer RX-5000a

e) Dropper

f) 250 mL Beaker

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 6. METHODOLOGY

General Start-up Procedure

1. Move the ELCB switch to UP position and the electrical power was switched on to control
the console. The lamp in the reboiler which is LOW LEVEL lamp section of console
illuminated along with the reboiler power, reflux timer, column temperature and process
temperature displays.

2. Make sure all the valves (V1 to V15) were in closed position

3. The laboratory cold water supply turned on and the control flow valve (V5) opened to give
maximum flow into the condenser via flow meter (F11). The leaks were checked.

4. The manometer tub filled until an equal level is visible approximately halfway up the
scale. The V6 and V7 closed.

5. The reboiler heater power was switched on at the console and the power adjusted to the
heater 1.50Kw. The water in the reboiler begins to heat up and observed by the selecting (T9)
on the process temperature digital display.

6. Valve V6 and V7 were opened and the pressure difference in the manometer observed and
V6 and V7 were closed

Experiment A

1. The experiment started when the power of control panel was turned on. All the valves were
closed except valve 10 on the reflux pipe and the boiler filled with 10 litres of mixture to be
distilled.

2. The temperature selector switch was set to T9 which is the temperature in the reboiler.

3. Valve V5 was opened and admitted the cooling water to the condenser approximate 3
litre/min.

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4. When the control panel has been turned on the power controller, the reboiler heating
element that fully anticlockwise was switched by the turning on power heating element to
‘power’ on position.

5. The reading of power approximately 0.5kW was set on the power controller and then the
content of the reboiler was warmed up which observed on the temperature readout meter for
10 minutes heating.

6. After 10 minutes valve V6 and V7 were opened so that the pressure drops obtained on the
manometer for top and bottom. The overall pressure drop was recorded.

7. On the top of the column, the cool distillate was returned and cascade down the trays and
formed a liquid level on the trays while the bubbling vapour passed through the liquid on
those trays. The degree of forming was observed and recorded.

8. The sample of 100ml was collected through valve V3 (opened valve) using measuring
cylinder, meanwhile the collecting time of the sample was recorded and the boil-up rate
(L/hr) was calculated based on the time taken.

9. The refractive index (RI) of the collected sample was obtained by test using
Refractometer. The refractometer was being calibrated by zeroing the instrument using
distilled water before RI testing.

10. The higher power of 0.75KW, 0.10KW and 1.25KW used for the repeated experiment.

General Shut Down

1. The heater power, feed pump motor and reflux valve at the console was switched off.

2. The equipment was disconnected from electrical supply when the equipment not used.

3. All the water from the system was drained using the drain valves V2, V3, V4, V11 and by
breaking the pipe connections of the bottoms product cooler and feed pump.

Experiment B

1. The volume of constituent was calculated.

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2. R.I. measured with the makeup of small quantities of 25 mole percent, 50 mole percent, 75
mole percent and 100 mole percent methyl cyclohexane.

3. The refractive index (R.I) of pure methyl cyclohexane and pure toluene was measured.

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 7. RESULTS

Experiment A: Determining Column Pressure Drop

Power Boil- up Pressure Drop Degree of foaming on

Time, t (s) R.I. (nD)
(kW) Rate (L/hr) (cm H20) trays

Foaming gently on the

0.5 144.77 2.4867 59 1.43871
tray

Foaming vigorously on
0.75 44.13 8.1577 63 1.33231
the tray

Foaming vigorously on
1 6.36 56.6038 253 1.33012
the tray

Foaming vigorously on
1.25 5.43 66.2983 229 1.45499
the tray

Foaming vigorously on
1.5 7.58 47.4934 185 1.45715
the tray

Table 1: Pressure Drop

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 Pressure Drop againt Boil-up Rate
300

Pressure Drop, cm H2O 250

200

150

100

50

0
0 10 20 30 40 50 60 70
Boil-up Rate, L/hr

Figure 4: Graph of Pressure Drop against Boil-Up Rate

Experiment B: Determining Mixture Composition

Concentration of Volume (mL)

Theoretical R.I.
Methylcyclohexane (%)
(nD)
[MCH] Toluene MCH

0 100 0 1.49774

25 71.54 28.46 1.33121

50 45.58 54.41 1.33218

75 21.82 78.17 1.33278

100 0 100 1.42366

Table 2: Refractive Index

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 Refractive Index against Mole Fraction of MCH
1.52
1.5
1.48
Refractive Index, nD

1.46
1.44
1.42
1.4
1.38
1.36
1.34
1.32
1.3
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole fraction od MCH, mol

Figure 5: Graph of Refractive Index against Mole Fraction MCH

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 8. CALCULATION

Experiment A: Determining Column Pressure Drop

Example calculation for 0.5 kW

164-105

=59 cm H2 O

Experiment B: Determining Mixture Composition

Molecular weight of methylcyclohexane, MCH = 98.19 g/mol

Molecular weight of toluene = 92.15 g/mol

Density of methylcyclohexane = 0.774 g/m3

Density of toluene = 0.867 g/m3

Sample calculation using 75% MCH and 25% Toluene

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Therefore,

Volume of MCH + volume of toluene = 100mL

1 Volume of toluene + 0.2792 volume MCH =100mL

1.2792 Volum MCH = 100mL

Volume MCH = 78.1739 mL

Volume toluene =21.8261 mL

Experimental R.I. (nD) Theoretical R.I. (nD) Error (%)

1.4387 1.4977 -3.9413

1.3323 1.3312 0.0826

1.3301 1.3322 -0.1546

1.4550 1.3328 9.1696

1.4572 1.4237 2.3524

Table 3: Percentage Error

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 9. DISCUSSION

According to John Brennan, distillation is a process that separates the liquid mixtures
by their boiling points. There are 4 types of distillation: simple distillation, fractional
distillation, vacuum distillation and azeotropic distillation (Brennan, 2018). In this
experiment, the type of distillation used is the fractional distillation. The fractional distillation
consists of the cycles. The vapor formed undergoes the reflux. During the reflux stage, the
condensed vapor from the top part of the distillation is condensed and the portion of them
returns to the top of the column to help with the distillation. The distillations separate the
liquid mixture based on their volatility. Volatility refers to the ability of the substance
vaporizes or transform from liquid to gas. High volatility means the liquid is easy to vaporize
first than the others.

From the 1st part of the experiment, the aim is to study the pressure drop across the
distillation column with different boil-up rates.

Pressure Drop againt Boil-up Rate

300
Pressure Drop, cm H2O

250

200

150

100

50

0
0 10 20 30 40 50 60 70
Boil-up Rate, L/hr

Figure 6: Graph of Pressure Drop against Boil-Up Rate

The figure above shows the graph of pressure drop against the boil-up rate. The
graph shows the increase in boil-up rate makes the pressure drop increases. According to Art
Montemayor, in the distillation column, the fixed trays, down comers and etc. represents a

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frictional force that acts against the liquid and vapor flows (2013). The resistance in this case
is measured as the pressure drop. The liquid flows are normally very small in comparison to
the vapor flows and thus the resistance confronted by the vapor (pressure drop) is very
significant when the vapor flow rate is increased beyond its design value. As the heat
increases, the vapor flow generates more pressure drop due to more resistance from excess
vapor trying to ascend through a fixed path.

Other than that, increasing the boil-up rates makes the degree of foaming on the trays
goes from ‘foaming gently’ to ‘foaming vigorously’. Foaming is the expansion of liquid due
to passage of the vapor or gas (M.T.Tham, 2016). The higher power input increases the flow
of the gas and causing the foaming more. Excessive foaming leads to liquid build-up on the
trays and might mixed with the liquid. Aside from that, the foaming provides high inter-facial
liquid-vapor contact that helps in more separation process. Next, increasing the power input
makes the refractive index. Refractive index shows how fast the light travels through the
light. It is also known as the ratio of the speed of radiation, in this case, light, in one medium
to t another medium. The higher refractive index means more separation occurs.

For the 2nd part of the experiment, the refractive indices from the distillation column
is compared to the refractive indices from the direct mixing of the Methyl cyclohexane
(MCH) with different mole fractions with pure toluene.

Refractive Index (dist column) Refractive index (Theoretical)

1.43871 1.49774
1.33231 1.33121
1.33012 1.33218
1.45499 1.33278
1.45715 1.42366

Table 4: Refractive Index of experimental and theoretical value

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 The refractive Indices of Both Part of Experiment.
1.55

1.5
Refractive Index
1.45

1.4

1.35

1.3

1.25

1.2
1 2 3 4 5
RI (Distillation) 1.43871 1.33231 1.33012 1.45499 1.45715
RI (Theoretical) 1.49774 1.33121 1.33218 1.33278 1.42366

Figure 7: Graph of Refractive Index for Experimental and Theoretical

The table and graph above shows the different RI measurements. Both RI
measurements show the same trends. They decrease sharply, experience constant and finally
increases back. Comparing both experiments, Theoretical result reaches the highest RI
number at the beginning of the experiment and the slightly lower from the distillation RI
towards the end of the experiment.

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 Refractive Index against Mole Fraction of MCH
1.52

Refractive Index, Theoretical

1.5
1.48
1.46
1.44
1.42
1.4
1.38
1.36
1.34
1.32
1.3
0 0.2 0.4 0.6 0.8 1
Mole fraction od MCH, mol

Figure 8: Graph of Refractive Index against Mole Fraction of MCH

The graph shows the 2 nd part of the experiment. The RI measurement is at 1.49774
when the mixture contains no MCH but pure toluene only. The RI dropped to 1.33121 once
the toluene and MCH are mixed. The more MCH introduced, the reading of RI increased
slowly and finally the RI reading is high again when only MCH is used. This shows the
mixture of MCH and Toluene reduces the RI readings. Both pure MCH and Toluene gives
the high RI reading. According to Narendra et.al, during mixing excess volume is the
measurement of molecular interaction in liquid mixtures. The structural property of liquid
and liquid mixtures can be integrated through refractive indices employing mole fractions.
That is why the RI reading of mixture and pure liquids are different. This is because regions
of space where London dispersion forces act centered in the dissimilar molecules composing
the mixture (Reis, et.al, 2010).

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 10. CONCLUSION

The experiment is conducted by using the distillation column in a laboratory sized.

The main objectives of the experiment are to determine the pressure drop across the
distillation column for various boil-up rates and to determine the mixture compositions by
using the refractometer. The pressure drops gained in this experiment shows increment as the
power supply are increased. The power supply increased makes the boil-up rate increases and
consequently increases the pressure drop. Next, the mixture compositions are determined by
determining the reading of the refractive index of the mixture. The RI readings give different
values of pure substances and mixtures. From the 1st part, it shows that an increase in power
supply and boil-up rate, makes the reading of refractive index increases slightly. As a
conclusion, both of the objectives are achieved as the result gained and the theory is on the
same term.

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 11. RECOMMENDATIONS

There are several recommendations that should be followed while conducting this
experiment in order to get more accurate data. Firstly, after sample being collected,
immediately close the vial. This is to prevent unnecessary evaporation of methylcyclohexane.
Secondly, it is recommended to use glove while collecting the sample as the sample is still
hot. In addition, students should be aware with the changes of degree of foaming inside the
column. This can be observed from time to time based on the interval time. Next, before
using the refractometer, it is advisable to clean the surface of refractometer using distilled
water. This step should be done every single before measuring the refractive index of the
samples. In addition, for the following experiment which to determine the composition of
mixture, after measuring the refractive index of the sample, make sure to put the mixture
back into the inlet for reuse. Lastly, the most important thing is, the students must be
prepared by going through the lab manual before entering the lab to conduct the experiment.
This is to ensure that the experiment can be run smoothly without any interruption.

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 12. REFERENCE

Brennan, J. (2018, March 13). Types of Distillation. Retrieved from Sciencing:

https://sciencing.com/types-distillation-6924000.html
Dr. Kiran Patil, T. B. (2009, september). Distillation Operations: Methods, Operational and
Design Issues. Retrieved from Research Gate:
https://www.researchgate.net/publication/263352060_Distillation_Operations_Metho
ds_Operational_and_Design_Issues
Gillespie, C. (2018, May 15). What is the Difference Between Reflux & Distillation?
Retrieved from Scincing: https://sciencing.com/difference-between-reflux-distillation-
5953384.html
Helmenstine, A. M. (2019, July 3). What Is a Volatile Substance in Chemistry? Retrieved
from Thought.Co: https://www.thoughtco.com/definition-of-volatile-604685
Isabel Lampreia. Angela Santos, M. L. (2010). Refractive Index of Liquid Mixtures: Theory
andExperiment. Retrieved from Chemphyschem:
https://www.academia.edu/21780316/Refractive_Index_of_Liquid_Mixtures_Theory
_and_Experiment
M.T.Tham. (2016). Distillation, an introduction. Retrieved from FACTORS AFFECTING
DISTILLATION COLUMN OPERATION:
https://www.rccostello.com/distil/distilop.htm
Montemayor, A. (2013). Cheresources. Retrieved from Distillation Column Pressure Drop:
https://www.cheresources.com/invision/topic/17592-distillation-column-pressure-
drop/

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13. APPENDICES

Figure 9: Table of raw data from experiment A and B

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