UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

PROCESS ENGINEERING LABORATORY 2
(CHE523)
NAME

: ABDUL HADI BIN MOHD FAIZAL DIN CHAN

GROUP

: EH2203A

EXPERIMENT

: DISTILLATION COLUMN

DATE PERFORMED

: 12.10.2015

SEMESTER

:3

PROGRAMME/CODE

: EH220 CHEMICAL ENGINEERING (HONS)

SUBMIT TO

: MADAM NOOR FAZLIANI SHOPARWE

No.
1
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Title
Abstract/Summary
Introduction
Aims
Theory
Apparatus
Methodology/Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
Reference
Appendix
TOTAL MARKS

Remarks :
Checked by :
_______________________
Date :

Allocated Marks (%)

5
5
5
5
5
10
10
10
20
10
5
5
5
100

Marks

ABSTRACT
This experiment is conducted to determine the refractive index of the distillation
column for various temperatures in batch distillation, to observe the degree of forming on
trays for each temperature, to determine the refractive index for unknown concentration
of ethanol/water and to plot the curve relating refractive index and percentage of ethanol. For
experiment one, the experiment is started by setting the power with 0.5kW ,0.75kW , 1.0kW,
1.25kW and lastly 1.50kW.During experiment is progressed, there are five level of degree of
forming that are observed which are gentle, violent, foaming gently over whole tray ,
foaming violently over whole tray and liquid flooding in column. The data of refractive index
for each temperature in valve 8 (V8) and valve 11 (V11) are collected and is put in the
observation table. For the next experiment, to determine the refractive index for unknown
concentration, the mixture of ethanol and water is mixed in appropriate volume that is
calculated. Then, the refractive index is measured using refractometer. From the data, the
graph of refractive index versus percentage of ethanol is plotted.

INTRODUCTION
Distillation columns are one of the main units used for separation processes in
industry. The basic theory behind them is very simple and relies on a mixture being made of
components of different boiling points. As a feed enters the column and some fractions may
vaporise and rise up the tower. The vapour components will condense and leave the column
at different levels as the temperature decreases up the tower. Based on a binary mixture, the
more volatile component (mvc) will come out at the top of the tower, and the less volatile
component (lvc) will leave at the bottom as a liquid. The lvc will have a higher boiling point
so it will be a liquid in the column.
The function of distillation is to separate, by vaporization, a liquid mixture of miscible
and volatile substances into individual components or, in some cases, into groups of
components. The separation of a mixture of alcohol and water into its components; of liquid
air into nitrogen, oxygen, argon; and of crude petroleum into gasoline, kerosene, fuel oil, and
lubricating stock are examples of distillation. Suppose there are two components, A and B.
Both of these components are found in both phases. There are four variables: pressure,
temperature, and concentrations of component A in the liquid and vapor phases (the
concentrations of component B are unity less those concentrations of A). If the pressure is
fixed, only one variable, e.g., liquid-phase concentration, can be changed independently and
temperature and vapor-phase concentration follow. In practice, distillation may be carried out
either of two principal methods. The first method is based on the production of a vapor by
boiling the liquid mixture to be separated and condensing the vapors without allowing any
liquid to return to the still. There is then no reflux, which is called batch distillation. The
second method is based on the return of part of the condensate to the still under such
conditions that this returning liquid is brought into intimate contact with the vapors on their
way to the condenser. Either of these methods may be conducted as a continuous steady-state
distillation process, including single-stage partial vaporization without reflux (flash
distillation) and continuous distillation with reflux (rectification), for systems containing only
two components.

The distillation column experiment is a purification experiment 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 analyzed to
determine the composition of the liquid. We performed a boiling point test on the mixture to
determine the unknown composition of the liquid. The data obtained from the boiling point
test allowed us to determine the composition using an x, y, T data plot for methanol-water.
Two experiments were performed.

Figure 1 : Distillation Column

OBJECTIVES

Operate Vapour Liquid Separation Experiment using a Packed Column Distillation

Process Unit.
Analyse the sample for the Top and Bottom Product by Refractometer to obtain the

Refractive Index (RI) in order to determine their respective composition.

To obtain the time when the Vapour Liquid Separation is nearly finish.

THEORY

Distillation columns are one of the most often used types of separation equipment in
industry.Distillation is one of the most common liquid-liquid separation processes, and can be
carried out in continuous or batch system.Distillation works by the application and removal
of heat to exploit differences in relative volatility. The heat causes components with lower
boiling points to be vaporized, leaving less volatile components as liquids. This makes
separations of close-boiling and azeotropic feeds difficult, so special distillation techniques
have to be used to separate these mixtures.
Distillation can be used to separate binary or multi-component mixtures. Many
variables, such as column pressure, temperature, size, and diameter are determined by the
properties of the feed and the desired products.Distillation is widely used for separation in
industry, most notably in petroleum, natural gas and chemical processing as well as any other
large-scale liquid production.
Distillation columns require packings and trays with low pressure drop and high
performance, especially those for vacuum applications. Pressure drops across trays and
packings are one of the most crucial factors to evaluate the performance of the column
internals. Pressure drop measurements also play an important role in troubleshooting of the
distillation column since the misleading or incorrect measurements are among the top ten
causes of column malfunctions (Kister, 2005). Using bubbler, pressure drop measurements
can also give the results of liquid head inside liquid distributors, liquid holdup on tray decks,
and downcomer backup etc (Cai and Resetarits, 2011).
Various studies show that the column size affects pressure drops across the packed
bed. This effect is packing dependent. For random packings and small columns (less than 0.9
m), the smaller diameter column presents lower bed pressure drops (Cai and Resetarits,
2011). It is believed that this is likely due to the wall effect of columns. Compared to larger
diameter columns, small columns have higher ratio of wall surface area to packing surface
area. This may explain why the pressure drops in small columns seems higher than those in
large columns (Cai and Resetarits, 2011). However, for structured packings, the effect of
column size on pressure drops is opposite. Limited data indicate that pressure drops measured
in smaller column are higher than those from larger columns (Olujic, 1999). This may be
caused by the relatively higher number of bends for vapor flow in a small column.

Adverse vapour flow conditions can cause foaming, entrainment, weeping/dumping

and flooding. Where foaming refers to the expansion of liquid due to passage of vapour or
gas. Although it provides high interfacial liquid-vapour contact, excessive foaming often
leads to liquid buildup on trays. In some cases, foaming may be so bad that the foam mixes
with liquid on the tray above. Whether foaming will occur depends primarily on physical
properties of the liquid mixtures, but is sometimes due to tray designs and condition.
Whatever the cause, separation efficiency is always reduced. Entrainment refers to the liquid
carried by vapour up to the tray above and is again caused by high vapour flow rates. It is
detrimental because tray efficiency is reduced: lower volatile material is carried to a plate
holding liquid of higher volatility. It could also contaminate high purity distillate. Excessive
entrainment can lead to flooding.
The phenomenon of weeping/dumping is caused by low vapour flow. The pressure
exerted by the vapour is insufficient to hold up the liquid on the tray. Therefore, liquid starts
to leak through perforations. Excessive weeping will lead to dumping. That is the liquid on
all trays will crash (dump) through to the base of the column (via a domino effect) and the
column will have to be re-started. Weeping is indicated by a sharp pressure drop in the
column and reduced separation efficiency. Flooding is brought about by excessive vapour
flow, causing liquid to be entrained in the vapour up the column. The increased pressure from
excessive vapour also backs up the liquid in the downcomer, causing an increase in liquid
holdup on the plate above. Depending on the degree of flooding, the maximum capacity of
the column may be severely reduced. Flooding is detected by sharp increases in column
differential pressure and significant decrease in separation efficiency.
The best way to reduce operating costs of existing units is to improve their efficiency
and operation via process optimisation and control. To achieve this improvement, a
throughout understanding of distillation principles and how distillation system are designed is
essential.

APPARATUS
1.The Continuous Distillation Column
2.100ml measuring cylinder
3.Automatic digital Refractometer
4.Stop watch
5.Distilled water
6.Methylcyclohexane
7.Toluene
8.Dropper

condense

refux
column

reboiler

Bottom
product
receiver

Figure 2: Distillation Column Apparatus

Figure 3: Automatic digital Refractometer

PROCEDURE
(A) Determination of pressure drop (P) due to the power increments.
1. The distillation column was set up by the instructor. The temperature, heating
boiler element and relative valves was set up by the instructor.
2. Reboiler was filled with the10L of mixture components consists of 50%
methylcyclohexane and 50%of toluene.
3. The temperature selector (T1, T2, T3, T4,T5, T6, T7, and T8) and regulated
switch were switched on. The power of control panel was turned manually.
4. As the reflux form, (methylcyclohexane achieved boiling point) the degree of
forming was observed at the column.
5. Next, the valve V6 and V7 were opened to collect the pressure drop. The reading
of pressure drops over both rectifying (top) and stripping (bottom) section was
taken.
6. Valves V6 and V7 were closed as finished collect the data.
7. As the steady state was obtained, valve 3 was partially opened to take sample and
condensate was drained from the reflux system.
8. 0.090L of sample was collected and the time taken to reach the volume was
measured.
9. Steps 4-8 was repeated with different power of 0.5, 0.75, 1.00, 1.25, 1.50 and 1.75
KWs.
10. Every time changed the power, wait for 10 minutes to achieve steady state.
11. The power of control panel was turned off as the experiment finished.
(B) Measuring refractive index of mixture compositions.
1. Before the experiment was started, the volume of the methylcyclohexane and
toluene must be measured first by using the equation that has been given. The %
of methylcyclohexane must consist of 0%, 25%, 50%, 75% and 100%.
2. After volume of both components was determined, poured the component in
the100ml beaker.
3. The sample of mixture component was measured their refractive index by using
refractometer.

RESULTS
Part A : Determination of pressure drop (P) due to the power increments
Table 1: Pressure drop of distillation column for various boil-up rates and refractive index
Degree of foaming on
Power

Boil

up Pressure drop (cm trays

(kW)

rates

HO)

(L/h)

overall

Top

0.5
0.95
1.00

0.78125
2.5
14.93

61
65
73

1.25

18.62

84

1.50

20.88

78

Refractive
Index

bottom
Gentle localised
Violet localised
Foaming gently over
whole tray
Foaming gently over
whole tray
Liquid flooding in
column

1.44058
1.44254
1.45343
1.46020
1.47764

Part B : Measuring refractive index of mixture compositions

Table 2 : Refractive index of mixture component
concentration

Refractive index

100%

1.49630

75%

1.48010

50%

1.47440

25%

1.45471

0%

1.42346

Pressure drop (cm H2O) vs Boil-up Rate

90
80
70
60
50
Pressure Drop

40
30
20
10
0

10

15

20

25

Boil-up rate

Figure 1 :The curve relating pressure drop as a function of boil-up rate.

Refractive index vs Mole Fraction of MCH

1.52
1.5
1.48
1.46
Refractive index 1.44
1.42
1.4
1.38
0%

20%

40%

60%

80%

100% 120%

Mole fraction of metylcyclohexane

Figure 2 : The graph of refractive index versus mol percent methylcyclohexane in

methylcyclohexane/toluene mixture.

CALCULATIONS
Part B: Measuring refractive index of mixture compositions

concentration (%)

100%

100
vol.tol
MWMCH
tol
1

MWtoluene
MWtol
MCH

100
vol.tol
MWMCH
tol
1

MWtoluene
MWtol
MCH

a)
Volume of methylcyclohexane = 0 ml
Volume toluene = 100 ml

75%

100
vol.tol
MWMCH
tol
1

MWtoluene
MWtol
MCH

b)
Volume toluene = 78.19 ml
Volume MCH = 21.81 ml

50%

100
vol.tol
MWMCH
tol
1

MWtoluene
MWtol
MCH

c)
Volume toluene = 45.59 ml
Volume MCH = 54.41 ml

25%

100
vol.tol
MWMCH
tol
1

MWtoluene
MWtol
MCH

d)
Volume toluene = 45.59 ml

Volume MCH = 54.41 ml

0%

100
vol.tol
MWMCH
tol
1

MWtoluene
MWtol
MCH

e)
Volume toluene = 45.59 ml
Volume MCH = 54.41 ml

DISCUSSION

Distillation is one of common methods of purification and identification of organic

liquids. It is a physical process used to separate chemicals from a mixture by a difference in how
easily they vaporize. Their operation is based on the difference in boiling temperatures of the
liquid mixture components, and on recycling counter-current gas liquid flow.
In this experiment the objectives is achieved which are to determine the refractive index
of the distillation column for various temperature, to observe the degree of forming on trays for
each temperature, to determine the refractive index for unknown concentration of ethanol/water
and to plot the curve relating refractive index and percentages of MCH.
This experiment can be divided into two stages. First is distillation column with finding
refractive index using refractometer. Second is non distillation mixing of MCH and water.
For experiment 1, MCH becomes the upper product or distillate because it has lower
boiling point than water thus more volatile . From this experiment also the 3 levels of vapour
flow condition in the distillation column can be observe during the distillation process which is
gently, flooding and foaming. Gentle flow refers to the flow of vapour which in steady condition
and no sudden abrupt rise occurs. Flooding refers by excessive vapour flow, causing liquid to
been trained in the vapour up the column. However, foaming refers to the expansion of liquid
due to passage of vapour or gas.
The graph of refractive index versus percentage of MCH is plotted. From the graph it can
be used to find the percentage of MCH in an unknown concentration and also can used to find
the theoretical stages of distillation column. Therefore, it found that there are 2 stages plus
reboiler.
There are several precaution steps that need to be alert during the experiment which are
use glove to hold the measuring cylinder during taking the volume of ethanol, avoid direct
contact with distillation column because it is hot, clean the refractometer surface using distilled
water before use that apparatus, after the finish the experiment, and collect back the sample of
mixture because it can be reused.

CONCLUSION
In distillation column experiment, from observation in experiment 1, the degree of
forming can be determined. The degree of forming at 0.5kW is gentle, at 0.95kW is gentle
localize, at 1.00kW is localized, at 1.25kW is Loading and lastly at 1.50K is flooding in column..
However, in experiment 2, the graph is plotted. Then according the graph that is plotted, the
theoretical stages can be determined which is 2 stages plus the reboiler.

RECOMMENDATION
In this experiment, there are several errors that are accidentally occurs which affected
the results obtained. Firstly, the eye position should be perpendicular to the meniscus and the
scale when reading the pressure differences. This error is also called parallax error.
Secondly, the duration of time before the data for each flowrate is taken must be
accurate which is in 10 minutes. Students can be accidentally missed the time and take the
data before or after the 10 minutes. This can slightly affect the results.
Beside that, the valve must be partially opened and not fully opened when the example
is going to be taken. This can cause the time taken to be much faster and eventully effect the
results if the valve is fully opened.
Finally, the instrument will remove and refill the water automatically when the
temperature during the process approaches the limit temperature for this distillation column.
This is the safety system for this instrument so that the toluene is not overly heated. This
safety system can affect the results because the toluene will take time to achieve the stability
again. Thus, the data will slightly difference from the theory.

Reference
1. Azyyati Binti Johari, Mass Transfer Chapter 2 Power Point Slide Note,
UNIKLMICET, 2014, Page 954)
2. Braz. J. Chem. Eng. vol.26 no.3 So Paulo July/Sept. 2009
3. http://www.uolab.lsu.edu/packed_distillation_column.htm
4. http://lorien.ncl.ac.uk/ming/distil/distiltyp.htm

APPENDIX

Figure 4 : The temperature control meter for the distillation column

Figure 2 : The trays of the distillation

column

Figure 3 : The pressure drop scale