FACULTY OF CHEMICAL ENGINEERING

PROCESS ENGINEERING LABORATORY II (CPE554)

NAME :
STUDENT ID. :
GROUP : EH2425B
EXPERIMENT TITLE : LAB 4: DISTILLATION COLUMN
DATE PERFORMED : 18TH OCTOBER 2016
DATE OF SUBMISSION : 1ST NOVEMBER 2016
LECTURERS NAME : SIR MUHAMAD FITRI BIN OTHMAN

No Remarks
Title Marks
.
1 Abstract/Summary 5
2 Introduction 5
3 Aims/Objective 5
4 Theory 10
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 10
11 Recommendation 5
12 Reference/Appendix 5
Total marks 100

Checked by: Date:

............
(SIR MUHAMAD FITRI BIN OTHMAN)

CONTENT
 1.0 ABSTRACT 2
2.0 INTRODUCTION 2-3
3.0 OBJECTIVES 3
4.0 THEORY 3-6
5.0 APPARATUS AND MATERIALS 6
6.0 PROCEDURES 7-8
7.0 RESULTS 9-10
8.0 CALCULATIONS 11-13
9.0 DISCUSSIONS 13-14
10.0 CONCLUSIONS 14-15
11.0 RECOMMENDATIONS 15
12.0 REFERENCES 16
13.0 APPENDICES 17

1.0 ABSTRACT

This experiment is conducted to determine the refractive index of the distillation column for
various boil-up rates in batch distillation column, to observe the degree of forming on trays
for each power supply, to determine the refractive index of unknown concentration of
methylcyclohexane (MCH)/toluene and to plot the curve relating refractive index and
percentage of ethanol. 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, 1.25 and 1.50 kW. For each power, the sample was collected until it
reached 90mL and then the procedures were repeated for each increment. The collected
samples were tested for its refractive index using refractometer. 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.

2.0 INTRODUCTION

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Distillation columns are one of the main units used for separation processes in industry.
Distillation is a process of separating the component substances from a liquid 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 may result in essentially complete
separation (nearly pure components), or it may be a partial separation that increases the
concentration of selected components of the mixture. 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.

The basic requirement for the separation of components by distillation is that the composition
of the vapor be different from the composition of the liquid with which it is in equilibrium at
the boiling point of the liquid. Distillation is concerned with solutions where all components
are appreciably volatile, such as ammonia-water or ethanol-water solutions, where both
components will be in the vapor phase. 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 will come out at the top of the tower, and the less volatile
component will leave at the bottom as a liquid. The less volatile component will have a
higher boiling point so it will be a liquid in the column. This experiment will investigate the
pressure drop over the distillation column for various boil-up rates.

3.0 OBJECTIVES

1) To determine the pressure drops and refractive indexes of the distillation column for
various boil-up rates in batch distillation column.
2) To observe the degree of forming on trays for each power supply.
3) To determine the refractive index of unknown concentration of methylcyclohexane
(MCH)/toluene.

2
 4) To plot the curve relating refractive index and percentage of methylcyclohexane.

4.0 THEORY

Distillation is a separation process of 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. Any countercurrent separation device has its own capacity limit. This limit is the
known as flooding point and is a result of high vapor velocity. At high vapor velocities, the
pressure exerted by the vapor from below balances the gravity head of the liquid, as a result
liquid starts building up in the column. This condition is reflected by sudden increase in the
pressure drop.

Figure 4.1: Equipment setup

The equipment will be set up to operate at total reflux meaning all the formed vapor will after
condensation return to the column. The charge of feed mixture can be loaded directly in the

3
reboiler through the filler cap provided without first charging the feed tank. At total reflux
there will be no feed or top product or bottom product. Make up 10 L of a mixture of 50 mol
% methylcyclohexane and 50 mol% toluene required for this mixture are

50 mol 98.19 g/ gmol 50 mol 92.15 g /gmol

of MCH : of toluene
0.774 g/ml 0.867 g /ml

6343.0 ml of MCH :5314.3 ml of toluene

1.19 ml of MCH :1.00 ml of toluene

Thus for 10 L of the mixture consist 5.43 L of methylcyclohexane and 4.57 L of toluene.

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 the top of the
tray. As the velocity of the vapors passing up the column increases, then the overall pressure
drop also increases. The velocity is controlled by varying the boil-up rate which is done by
varying the power input to the reboiler. Under conditions with no liquid present, the sieve
trays will behave like an orifice in that the pressure drop will be proportional to the square of
the 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 indexes measured. The refractometer measures the critical angle of the
liquid under thest and each concentration will show a different critical angle. From this the
refractive index can be found.

4
 Figure 4.2: Cross section of Refractometer.

The volumes of constituents to use were calculated as followed:

For 25 mol % MCH, 75 mol % toluene;

Molecular weight MCH = 98.19 g/gmol

Molecular weight toluene = 92.15 g/gmol

Density of methylcyclohexane = 0.774 g/ml

Density of toluene = 0.867 g/ml

V MCH MCH 100

MW MCH
25=
V MCH MCH V tol tol
+
MW MCH MW tol

100
25=
V tol MW MCH
1+ tol
V MCH MW tol MCH

5
 V tol MW MCH
3= tol
V MCH MW tol MCH

V tol MW tol
=3 MCH
V MCH MW MCH tol

V tol 92.15 0.774

=3
V MCH 98.19 0.867

V tol =2.51V MCH

Thus, for 100 ml of mixture required 28.49 ml MCH and 71.51 ml toluene.

5.0 APPARATUS AND MATERIALS

Distillation column Model UOP3CC, Refractometer, stopwatch, 100 ml measuring cylinder,

dropper, distilled water, methylcyclohexane and toluene.

6.0 PROCEDURES

A. Experiment 1: Determining Column Pressure Drop.

1. The general start-up procedures were performed.

2. All valves on the equipment were ensured to be closed.
3. Valve V10 on the reflux pipe were opened.
4. The boiler was filled with 10 litres of mixture to be distilled.
5. The filler cap on the top of the reboiler was firmly replaced.
6. The power of the control panel was switched on.
7. The temperature selector switch was set to T9, the temperature in the
reboiler.
8. Valve V5 was opened admitting the cooling water to the condenser at a
flow rate on F11 of approximately 3 L/min.
9. The power controller for the reboiler heating element on the control panel was turned
fully anti-clockwise and the switch turning on the power to the heating element was
switched to power on position.
10. Another red lamp will illuminate indicating the heating element was on.

6
11. The power controller was turned until a reading of approximately 0.5kW is obtained on
the digital wattmeter.
12. The boiler was let to heat for 10 minutes for warm up the contents of the reboiler.
13. After 10 minutes, valve V6 and valve V7 were opened. The pressure drop on the
manometer was recorded for top and bottom pressure.
14. The degree of foaming on the trays was observed and recorded in the result table.
15. Valve V3 was opened to collect 90 ml of the sample using measuring cylinder while the
collecting time was recorded using stopwatch. Later on, the boil up rate (L/hour) was
calculated based on the time taken.
16. The collected sample was later on determined the refractive index using Refractometer.
17. Before that, the refractometer must be calibrated first using distilled water before testing
the refractive index of the sample.
18. The experiment was repeated using 0.75, 1.0, 1.25 and 1.5 kW power.
19. The general shut-down procedures were performed.

B. Experiment 2: Determining Mixture Compositions.

1. The refractive index of pure methylcyclohexane and pure toluene were measured.
2. Small quantities of 25 mol %, 50 mol %, and 75 mol % of MCH were made and their
refractive indexes were measured.
3. The volume of constituents to use were calculated as followed:

For 25 mol % MCH, 75 mol % toluene;

Molecular weight MCH = 98.19 g/gmol

Molecular weight toluene = 92.15 g/gmol

Density of methylcyclohexane = 0.774 g/ml

Density of toluene = 0.867 g/ml

V MCH MCH 100

MW MCH
25=
V MCH MCH V tol tol
+
MW MCH MW tol

7
 100
25=
V MW MCH
1+ tol tol
V MCH MW tol MCH

V tol MW MCH
3= tol
V MCH MW tol MCH

V tol MW tol
=3 MCH
V MCH MW MCH tol

V tol 92.15 0.774

=3
V MCH 98.19 0.867

V tol =2.51V MCH

Thus, for 100 ml of mixture required 28.49 ml MCH and 71.51 ml toluene.

7.0 RESULTS

A. Experiment 1: Determining Column Pressure Drop.

Power Boil-Up Rate Pressure Drop (cm H2O) Degree of Foaming Refractive
(kW) (L/h) Top Bottom Overall on Trays Index

0.5 4.0602 167 93 74 Gently localised 1.43396

0.75 8.4595 171 92 79 Violent localised 1.43707

Foaming gently over

1.0 23.1400 203 70 133 1.45068
whole tray

Foaming gently over

1.25 28.1700 220 40 180 1.45345
whole tray

1.5 36.8601 235 30 205 Foaming violently 1.45263

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 over whole tray
Table 7.1

Pressure drop vs Boil Up Rate

250

200

150

Pressure Drop (cmH2O)

100

50

0
0 5 10 15 20 25 30 35 40

Boil Up Rate (L/h)

Graph 7.1

B. Experiment 2: Determining Mixture Compositions.

Volume (mL)
Concentration of MCH Refractive
(%) Index
Toluene Methylcyclohexane

100% 0 100 1.42383

75% 21.875 78.125 1.43716

50% 45.59 54.41 1.45526

25% 71.51 28.49 1.47402

0% 100 0 1.49612

Table 7.2

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Graph of Refractive Index vs Mole Fraction MCH

1.52
1.5
1.48
1.46
Refractive Index 1.44

1.42
1.4
1.38
0.00 0.20 0.40 0.60 0.80 1.00 1.20

Mole Fraction Methylcyclohexane

Graph 7.2

8.0 CALCULATIONS

Molecular weight methylcyclohexane = 98.19 g/gmol

Molecular weight toluene = 92.15 g/gmol

Density methylcyclohexane = 0.774 g/mL

Density toluene = 0.867 g/mL

V MCH MCH 100

MW MCH
25=
V MCH MCH V tol tol
+
MW MCH MW tol

100
25=
V tol MW MCH
1+ tol
V MCH MW tol MCH

10
 V tol MW MCH
3= tol
V MCH MW tol MCH

V tol MW tol
=3 MCH
V MCH MW MCH tol

V tol 92.15 0.774

=3
V MCH 98.19 0.867

V tol =2.51V MCH

For 100 mL of mixture, quantity required :-

i. 0% methylcyclohexane : 100% toluene

VMCH + Vtol = 100mL

0 + Vtol = 100mL
VMCH = 0 mL
Vtol = 100mL

ii. 25% methylcyclohexane : 75% toluene

VMCH + Vtol = 100mL

VMCH + 2.51VMCH = 100mL

VMCH = (100/3.51) mL

VMCH = 28.49 mL

Vtol = 71.51 mL

iii. 50% methylcyclohexane : 50% toluene

VMCH + Vtol = 100mL

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 VMCH + 0.838VMCH = 100mL

VMCH = (100/1.838) mL

VMCH = 54.41 mL

Vtol = 45.59 mL

iv. 75% methylcyclohexane : 25% toluene

VMCH + Vtol = 100mL

VMCH + 0.28VMCH = 100mL

VMCH = (100/1.28) mL

VMCH = 78.125 mL

Vtol = 21.875 mL

v. 100% methylcyclohexane : 0% toluene

VMCH + Vtol = 100mL

VMCH + 0 = 100mL

VMCH = (100/1) mL

VMCH = 100 mL

Vtol = 0 mL

9.0 DISCUSSIONS

A fractionating column or fractionation column is an essential item used in distillation of

liquid mixtures which is to separate the mixture into its component parts, or fractions, based
on the differences in volatilities. Continuous distillation, a form of distillation, is an ongoing
separation in which a mixture is continuously (without interruption) fed into the process and

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separated fractions are removed continuously as output streams. Distillation is the separation
or partial separation of a liquid feed mixture into components or fractions by selective boiling
(or evaporation) and condensation

The aims of the experiment A, to determine the pressure drop inside the distillation column
and Experiment B to determine the refractive index of MCH for the calibration curve. In the
distillation column, the inlet feed has already contained a mixture of toluene and methyl
cyclohexane. The mixture will be run through a column of trays. There are two outlet streams
which are the rectifying (top) and the stripping (bottom). The distillates which are the high
volatile component (HVC) and low volatile component (LVC) can be determined from their
boiling point. Methylcyclohexane has a low boiling point which is 101C, while toluene has a
boiling point higher than the methylcyclohexane which is 111C. Thus, methylcyclohexane is
the one whom will be vaporized first and then released up to the rectifying column. In order
to determine the pressure drop over the distillation column for various boil-up rates in batch
distillation, the graph 7.1 had been plotted. The graph of pressure drops against boil-up rates
shown that both the pressure drops and boil-up rates values increased as the power of boiler
heater was increased from 0.50 kW to 1.50 kW.

Moreover, the degree of foaming on trays recorded changing its pattern with different power
supply through our observation. At 0.5 kW, we observed that the degree of foaming on trays
was gently localised. Meanwhile at 0.75 kW, the pattern was started to show a violent
localized, later on, at 1.00kW, it was started to foam gently over the tray same as at the power
1.25kW. Lastly, at 1.50kW, foaming violently over whole tray. Thus, it shown that, the degree
of foaming on the trays will increase as the power supply increase.

The refractive indexes were also obtained using the refractometer for all of the different
power intensities. The refractive indexes are shown the increasing pattern from the power of
0.5kW to 1.25kW, but it slightly decreased at power of 1.5kW. This happened maybe due to
some technically problem during sampling.

Furthermore, the mixture compositions also can determined by using refractometer. In order
to prevent error while reading the value of refractive index by using refractometer, blank
calibration is applied first with distilled water. As a result, random error due to contaminated

13
at sample reading can be avoid. In the determination of the compositions of mixture of
methylcyclohexane/toluene using refractometer, not only the compositions were collected but
also the refractive index. From the graph Refractive index vs. mole fraction of
methylcyclohexane (MCH) plotted, we can see that the refractive index values drops as the
mole fraction methylcyclohexane increased. It clearly shows the decreasing linearly from 0
mole fraction of MCH until it reached 1.00.

10.0 CONCLUSIONS

In conclusion, the objectives of this experiment are to determine the pressure drops and
refractive index of the distillation column for various boil-up rates in batch distillation
column, to observe the degree of forming on trays for each power supply, to determine the
refractive index of unknown concentration of methylcyclohexane (MCH)/toluene and to plot
the curve relating refractive index and percentage of methylcyclohexane.

The greater the heater powers are used, the higher the boil-up rate. As the boil-up rate is
increasing, the time consume to collect the sample is decreasing. Simultaneously, when the
temperature of the mixture is increasing, the pressure drop will be increasing. The
relationship between pressure drop and boil-up rate is shown on the graph plotted which
shown the pressure drop increased as the power increased. As for the degree of foaming on
trays, the degree of foaming was increased as the power supply increased. Also, the refractive
index values are also recorded at all power intensities.

In Experiment B, graph 7.2 had shown the relationship between the mixture composition or
mole fraction of the methylcyclohexane with their refractive index. From the graphs of
Refractive index vs. mole fraction of MCH, the relationship is determined in which the
refractive index values decreased as mole fraction of MCH is increased until it reached 100
mol % MCH. In brief, all the objectives of the distillation column experiment are achieved
and the experiment is successfully done.

11.0 RECOMMENDATIONS

1) Before starting the experiment A, make sure that all the valves on the equipment are
fully closed.

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 2) Repeat the important steps several times to obtain accurate date and reduce some
errors.
3) Error should be avoided such as the overflowed of the sample from the column into
the manometer arms which affected the values of pressure drops significantly and
totally violates the theory
4) Make sure that our eye is the same level as the meniscus of water when we take the
reading to avoid parallax error.
5) Be careful with the hot liquid while collecting the sample to avoid inflammation to the
skin.
6) Do a blank calibration before read exact refractive index to prevent error while
reading the refractive index value.
7) Always wear gloves during conducting this experiment to avoid any contact of
chemical with bare hand. Toluene and methylcyclohexane are flammable, irritating
and toxic. If possible use a fume hood.

12.0 REFERENCES
1) Christie J. G. (2014). Transport Processes & Separation Process Principles (Includes
Unit Operations), 4th Edition. Pearson Education Limited, United Kingdom.
2) Laboratory manual, (n.d). Laboratory manual: Distillation column. Faculty of
Chemical Engineering and Bioprocess. UiTM Shah Alam.
3) McCabe, W. L. and J. C. Smith (1976). Unit Operations of Chemical Engineering
(3rd Edition.). McGraw-Hill, USA.
4) Bravo, Jose L. and James K. Fair. (Jan, 1990). "Distillation Columns." Chemical
Engineering Progress. Retrieved from
http://www.srsengineering.com/our-products/distillation-columns/how-columns-work/
5) Sujata N., Betsy S. at. al. (n.d.). Encyclopedia of Chemical Engineering Equipment;
Distillation Column. Retrieved from
http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/DistillationColu
mns/DistillationColumns.html
6) Process Engineering Guide: Laboratory Distillation (n.d.). GBH Enterprises, Ltd.
Retrieved from
http://www.slideshare.net/GerardBHawkins/laboratory-distillation

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13.0 APPENDICES

Figure 13.1: Distillation Column Figure 13.2: Sample is taken using

measuring cylinder

Figure 13.3: Continuous Distillation Figure 13.4: Reading values

Column Model UOP3CC

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Figure 13.5: Automatic Digital
Refractometer
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