UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

CHEMICAL ENGINEERING LABORATORY II
CHE523

NAME :
GROUP : EH2203 (GROUP 5)
EXPERIMENT : DISTILLATION COLUMN
DATE PERFORMED : 17 JUNE 2014
SEMESTER : 3
PROGRAMME / CODE : CHE523
SUBMIT TO : MADAM AZRINI

No. Title Allocated Marks (%) Marks
1 Abstract/ Summary 5
2 Introduction 5
3 Objectives 5
4 Theory 5
5 Apparatus 5
6 Methodology/ Procedure 10
7 Result 10
8 Calculations 10
9 Discussion 20
10 Conclusion 10
11 Recommendations 5
12 Reference 5
13 Appendix 5
TOTAL MARKS 100


Remarks:
Checked by:
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Date :
TABLE OF CONTENTS

BIL TITTLE PAGE
1 ABSTRACT
2 INTRODUCTION
3 OBJECTIVES
4 THEORY
5 APPARATUS
6 PROCEDURES
7 RESULTS
8 CALCULATIONS
9 DISCUSSION
10 CONCLUSION
11 RECOMMENDATIONS
12 REFERENCE
13 APPENDIX

















INTRODUCTION
The distillation column is a process in which a liquid or vapor mixture of two or more
substances is separated into its component fractions of desired purity, by the application and
removal of heat. 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. The fact about distillation column is the vapor of a boiling
mixture will be richer in the component that have lower boiling point. Therefore, when this vapor
is cooled and condensed, the condensate will contain more volatile components. At the same
time, the original mixture will contain more of the less volatile material. The separation process
requires three things. First, a second phase must be formed so that both liquid and vapor
phases are present and can contact each other on each stage within a separation column.
Secondly, the components have different volatilities so that they will partition between the two
phases to different extent. Lastly, the two phases can be separated by gravity or other
mechanical means. Distillation differs from absorption and stripping in that the second phase is
created by thermal means. 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.



OBJECTIVES
Experiment A: to determine the pressure drop over distillation column for various boil-up rates,
in batch distillation.
Experiment B: use of refractometer for determining mixture composition.

Theory
Distillation is a process of separating two or more miscible liquids by taking advantage of
the boiling point differences between the liquids. In order to understand how the distillation
works, consider the mixture of toluene and methylcyclohexane for this distillation experiment.
Heat is added to the mixture of toluene and methylcyclohexane and eventually the most volatile
component (in this case methylcyclohexane) begins to vaporize. When the methycyclohexane
vaporizes, it takes with it molecules of toluene. The methycyclohexane-toluene vapor mixture is
then condensed and evaporated again, giving a higher mole fraction of methycyclohexane in the
vapor phase and a higher mole fraction of toluene in the liquid phase.
This process of condensation and evaporation continues in stages up the column until the
methycyclohexane rich vapor component is condensed and collected as top product and the
water rich liquid is collected as bottom product. Figure below shows the distillation column used
in the experiment.

In order to understand thoroughly the distillation process, let consider what happen when
heating a liquid. At the boiling point, the molecules of the liquid posses enough kinetic energy to
escape into the vapor phase (evaporation) and some molecule in the vapor phase return to the
liquid phase (condensation).
During the mixing, the vapor will pick up more of component methylcyclohexane from the
liquid while the liquid will be richer with component toluene. As the vapor rises further up,it
becomes richer and richer in component methylcyclohexane but poorer with component
toluene. The feed stream is introduced on some intermediate tray where the liquid has
approximately the same composition as the feed. The part of column above the feed point is
rectifying section while the lower part is stripping section.

APPARATUS
Experiment A: determine the pressure drop over the distillation column for various boil-up rates,
in batch distillation.
1. Distillation column.
2. 100mL of measuring cylinder.
3. Refractormeter.
4. 250mL measuring cylinder graduated.
5. Stop watch.
Experiment B: determining mixture compositions
1. Refractometer.
2. 100mL beaker
3. Burrete
4. Droper.





PROCEDURES
Experiment A: determine the pressure drop over the distillation column for various boil-up rates,
in batch distillation.
1. Before starting, al the valves on the equipment are closed. Then, the valve V10 on the
reflux pipe is opened.
2. The boiler is filled with 10 litres of mixtures to be distillated.
3. The filter cap on the top of the reboiler is firmly replaced.
4. Turned on the power supply to the control panel.
5. The temperature selector switch is setup to T9 which is for temperature in boiler. The
cooling water is admitting to condenser by opened the V5 at flow rate on F11 of
approximately 3 litres/min.
6. The power controller are turned on for reboiler heating element dully anti-clockwise and
switch the switch turning on the power to the heating element to power on position.
7. Red lamp is illuminate to indicate the heating element is on.
8. The power controller is turned to clockwise until reading of approximately 0.75W is
obtained on the digital wattmeter.
9. The contents of the reboiler will begin to warm up and observed through the temperature
readout meter.
10. Valves V6 and V7 is opened which connect base and top of distillation column,
respectively, to the manometer.
11. The V6 and V7 are opened.
12. First and 5
th
plates are observed.
13. Vapour is rise up in the column and observed.
14. Vapour enters the condenser and reappears as droplets into the glass walled distilled
receiver vessel.
15. V3 is partially open and drained the condensate. The sample is start to collect and timing
at the same time. Sample is collected approximately 90mL and 100mL.
16. After taking a sample, take reading of pressure drops over both the top and bottom
section. Make sure always open V6 and V7.
17. Measure the sample by using refractometer.
18. After finish read pressure drop, close V6 and V7.
19. Repeat the experiment for power 250 watt until 1.5kW after 10 minutes done taking
pressure drop reading.
Experiment B: determining mixture composition
1. The refractive index (RI) of pure methylcyclohexane and pure toluene is measured.
2. The small quantities of 25 mol %, 50 mol % and 75 mol % methylcyclohexane are
prepared is mixed respectively with 75 mol%, 50 mol% and 25 mol% toluene to measure
their RI.
3. The data are recorded.





















RESULTS
Experiment A: Determining column pressure drop
Power (kW) Boil-up Rate
( litres/hr)
Pressure drop (cm
H
2
O) Top bottom
overall
Degree of
foaming on
trays
Refractive
index
0.50 3.81 70 Gentle 1.43755
0.95 10.80 66 Gentle
localized
1.43794
1.00 14.40 223 Localized 1.43836
1.25 81.00 150 Loading 1.44688
1.50 9.53 128 Flooding 1.45339




Experiment B: Determining mixture compositions
Concentration Refractive index
100% 1.42326
75% 1.43789
50% 1.46129
25% 1.33310
0% 1.49683





Plot the curve relating pressure drop as a function of boil-up rate.


The graph of refractive index versus mol percent methylcyclohexane in
methylcyclohexane/toluene mixture.




0
50
100
150
200
250
3.812 10.8 14.4 81 9.53
P
r
e
s
s
u
r
e

d
r
o
p
,

c
m

H
2
O

Boil-up rate, L/hr
Pressure drop vs boil-up rate
1.25
1.3
1.35
1.4
1.45
1.5
1.55
0 0.25 0.5 0.75 1
R
e
f
r
a
c
t
i
v
e

i
n
d
e
x

Mole fraction of methylcyclohexane
Refractive index vs mole fraction of MCH
SAMPLE OF CALCULATION
For 100 ml of mixture, quantity required:
i) 0% methylcyclohexane : 100% toluene

V
mch
+ V
tol
= 100ml
0

+ V
tol
= 100ml
V
mch
= 0
V
tol
= 100 mL

ii) 25% methylcyclohexane : 75% toluene

V
mch
+ V
tol
= 100ml
V
mch
+ 2.51 V
mch
= 100ml
V
mch
= (100/3.51)
V
mch
= 28.49 mL
V
tol
= 71.51 ml

iii) 50% methylcyclohexane : 50% toluene

V
mch
+ V
tol
= 100ml
V
mch
+ 0.838 V
mch
= 100ml
V
mch
= (100/1.838)
V
mch
= 54.4mL
V
tol
= 45.6 mL




iv) 75 %methylcyclohexane : 25% toluene

V
mch
+ V
tol
= 100ml
V
mch
+ 0.280 V
mch
= 100ml
V
mch
= (100/1.280)
V
mch
= 78.125mL
V
tol
= 21.875 mL


v) 100% methylcyclohexane : 0% toluene

V
mch
+ V
tol
= 100ml
V
mch
+ 0 = 100ml
V
mch
= (100/1)
V
mch
= 100mL
V
tol
= 0 mL













Discussion
Based on the results of the experiment conducted, the more power input to heat the
higher the boil up rate of the mixture. Gradually the degree of foaming on trays changed from
gentle to flooding when the heat increased. This shows the mixture of methylcyclohexane are
diffused in the distillation column and separated in the Rasching ring. The process was speed
up rapidly when the heat increased per time and the mixture collected and to compare with
refractive index. The foaming on trays mostly localized and flooding where the mixture
completely separated in contact of fluid and the Rasching ring help to increase the separation
process by the surface area of fluid contact each other and diffuse more easily. But when the
process too flooding, it reflux and the remaining collected for the other batch.
The most suitable power required for this process based on the results obtained, the 1
kW power is suitable for separating the methylcyclohexane in the distillation process. 1 kW
power produces 14.4 L/hr of boil up rate and the pressure drop of 223. In addition the foaming
state was localized where the most required process for distillation column to determine the
pressure drop (top to bottom) and steady process. With this state, the process easy to handle
and most crucial was pressure drop. The pressure drop obtained was high and it reached the
equilibrium where the separation needed is in steady state. The localized foaming was not too
aggressive and the methylcyclohexane not reflux.
For the refractive index, the concentration of 50% methylcyclohexane and 50% toluene
shows the 1.46129 index where the separation was at optimum. The volume needed for the
refractive index from distillation column was almost suitable for the whole process required.







Conclusion
From the experiment, we can conclude that the objective of the experiment is achieved.
What we can see from the result, the pressure drop in the distillation column is not the function
of the power that has supplied. At power of 0.50kW, the pressure drop recorded was 70cm H
2
O.
At 0.95 kW the pressure drop was drop to 66cm H
2
O. However by increasing the power to 1kW
the pressure drop increase to 223 cm H
2
O. From the observation, the degree of foaming is
changing with the increasing power. It changes from gentle-gentle localized-localized-loading
and flooding. From the experiment, from the compare of RI value, the more power the distillation
process consumed, the more high molar composition of methylcyclohexane that collected as the
product.


Recommendations
There are several recommendations must be performed to decrease the percentage of the error
in order to increase the accuracy of the Reynolds number such as;
1. The general start-up procedures need to be performed before starting each of the
experiment. This is to ensure all the components of the unit are in good conditions and
working smoothly. It will affect the reading of the experiment and reduce the
performance of the unit if the components are not in satisfied conditions.
2. To get more accurate reading, the experiment must be repeated at least 3 times by
calculating the average reading. This will reduce the deviation from the theoretical data.
3. Make sure that our eye is the same level as the meniscus of water when we take the
reading to avoid parallax error.





REFFERENCE
1. UiTM Chemical Engineering Lab Manual 2014, Distillation Column
2. Unit Operations Of Chemical Engineering 7
th
Edition, Warren L. McCabe, Julian C.
Smith, Peter Harriott
3. Green, D.W., ed. Perrys Chemical Engineering Handbook. Sixth Edition. McGraw-Hill
Book Company, New York. 1984.
4. http://www.nt.ntnu.no/users/preisig/Repository/TKP_4110_Felles_Lab/experiment%20de
scriptions/DistInstruct.pdf







APPENDIX