EKB 2131 Chemical Engineering Lab - III

Bachelor of Chemical Engineering (Hons)

LAB REPORT

EKB 2131 - CHEMICAL ENGINEERING LAB - III

EXPERIMENT TITLE PACKED BED DISTILLATION COLUMN

NAME OF CANDIDATE
SHAMINI SATHIVEL
WITH REG NO.
SESSION DATE 22th OCTORBER 2015, Thursday
DATE OF SUBMISSION 29TH OCTORBER 2015, Thursday

NAMES OF GROUP MEMBERS

No REG No.
NAME
.
1 1000013 Sangidha Jegathesan
2 1000045 Sasi Varnan
3

MARKING SIGNATURES

MARKS
DETAILS TOTAL
AWARDED
Participation
and Attitude (Name of Faculty Supervising)
TABLE OF CONTENTS
Mr.Arasu Uttaran
Lab Report

CHEM. ENGG. LAB-IV INCHARGE

Total (Dr. TVN. Padmesh/Arasu Uttran)

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EKB 2131 Chemical Engineering Lab - III

S. NO. DESCRIPTION PAGE NO.

Abstract 3

1 Introduction 3

2 Materials and Methods 5

3 Results and Discussions 7

4 Conclusions and Recommendations 8

5 References 9

Appendix 9

ABSTRACT
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The experiment was carried out to study the process of packed bed distillation column. The
experiment was conducted under total reflux condition. The moles fraction of methanol in feed,
residue and distillate was determined by the graph of R.I vs. x corresponding to refractive indexes
respectively. The mole fraction of methanol in feed, F was determined to be 0.37 moles. The mole
fraction of methanol of residue B was determined to be 0.25 moles. The mole fraction of methanol
of distillate D was to be 0.057. The error that was calculated is 2.61. The value of minimum plates,
Nm that was calculated is 0.84.

1. INTRODUCTION

1.1. Distillation

Distillation is defined as a process in which a liquid or vapour mixture of two or more substances
having different vapour pressures is separated into its component fractions of desired purity, by the
application of heat [1]. When the vapours of the boiling mixture is cooled and condensed, the
condensate will contain more volatile components (low boiling point). As distillation progresses, the
original mixture will contain more of less volatile material (high boiling point). Depending on the
concentrations of the components present, the liquid mixture will have different boiling point
characteristics. Distillation occurs because of vapour pressures of the components in the liquid
mixture. If relative volatility is very close to 1, they have similar vapour pressures and hence, it will
be difficult to separate the two components by distillation [1]. Distillation is a unit operation
capable of producing pure substance from liquid mixtures.

1.1.2 Application of Distillation

Distillation has long been used as the separation process in chemical and petroleum
industries
Distillation technology is applied in pharmaceutical, chemical, food, and alcohol industries
Distillation is used in refineries for fractionating crude oil to produce many chemicals
It is used in distillery for producing alcohol

1.1.3 Types of Distillation Columns

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There are many types of distillation columns, each designed to perform specific types of separations
and each design differs in terms of complexity.

A few common types are given below:

As batch and continuous processes based on how they are operated.
As binary or multi-component distillation processes based on the number of components in
the feed.
As tray or packed distillation columns based on the type of column internals.

1.2 Packed Bed Column

Packed bed columns are used most often for absorption, liquid-liquid extraction and distillation.
This experiment was conducted to study the operation of packed bed distillation column. The
packing provides a large surface area for vapour - liquid contact. The feed mixture contains
components of different volatilities, and enters the column approximately at the middle. The liquid
flows downward through the packing, and the vapour flows upward through the column [2].
Differences in concentration cause the less-volatile components to transfer from the vapor phase to
the liquid phase. After the feed mixture enters the column it flows down the column through the
packing counter currently and contacts the rising vapour stream. The liquid at the bottom enters a
reboiler. Two streams exit the reboiler; a vapour stream, which returns to the column, and a liquid
product stream. The vapour stream flows upward through the packing, picks up the more volatile
components, exits the column, and enters a condenser. After the vapour condenses, the stream enters
a reflux drum, where it is split into an overhead product stream, known as the distillate, and a reflux
stream that is recycled back to the column [2].

1.2.1. Advantages of Packed Bed Column

Most cost-efficient distillation column when the diameter of the column is less than 0.6 m.
Because packing can be made from inert materials, packed beds are able to handle corrosive
materials [2].
Lower pressure drop than in plate columns.
Good for thermally sensitive liquids

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1.2.2. Disadvantages of Packed Bed Column

Packing can break during installation, or due to thermal expansion.

Not cost efficient for high liquid flow rates.
Contact efficiencies are decreased when the liquid flow rate is too low [2].

2. MATERIALS AND METHODS

VALVE
V1 Feed Supply Valve for Funnel
V2 Air Vent Valve of Vessel
V3 Water Flow Control Valve
V4 Air Vent Valve of Condenser
V5 Valve for Distillation Collection
V6 Drain Valve of Vessel

2.1 Starting Procedure

1. Methanol water solution is prepared by mixing known amount of water and methanol
2. The total amount of solution is 15L
3. The volume of water and methanol was noted down
4. V1- V6 valves was closed
5. All the switches on the panel were ensured to be at OFF position.
6. The water is filled in the cold water tank
7. The reboiler was filled with methanol water solution by opening the valve V 1 and air vent
valve V2
8. Valve V1 and V2 was closed
9. The electricity was connected to the set.
10. The process temperature was set at 90 C.
11. The heater and cooling water pump was started.
12. The cold water flow was adjusted by the rotameter valve to a moderate value.
13. The cyclic temperature was set for total reflux.
14. Wait 25-30 minute for the system to achieve steady state.
15. Samples from the bottom & distillate stream were taken out.
16. The samples were cooled to room temperature and the refractive indices were measured

2.2 Closing Procedure

1. The water supply was stopped when the experiment was over.
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2. The pump, heater and the main power supply was switched off.
3. Column, reflux drum, receiving tank and water tank were drained.
4. The vessels were drained after the temperature fell down to atmospheric pressure by
opening valve V6.

2.3 Formulae used

To calculate the moles of methanol in feed

M
(1)
F V

To calculate the moles of methanol in residue

x FxD
B F (2)
x BxD

F xF
(3)
BxB

F 1x F
In (4)
B 1x B

To calculate the error

F xF F 1x F
E= - In (5)
BxB B 1x B

To calculate minimum number of plates

x D 1x B
x B 1x D 1 (6)
Nm
In

Figure 1 shows the block diagram of packed bed distillation column. The set-up consists of packed
column, which is packed with glass rasching rings. An electrically heated reboiler is installed at the

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bottom of the column. A tank is provided to collect the bottom product. Shell and tube type
condenser is provided to condensate the vapour. A tank with pump and rotameter is provided for
circulation of cooling water. Reflux drum is provided to collect the condensate. Receiving tank is
for collecting the distillate. Drain valves are provided for drainage purpose.

Figure 1: Block Diagram of Packed Bed Distillation Column

3. RESULTS AND DISCUSSION

From the graph shown in Figure 2 as shown in Appendix, the mole fraction of methanol in feed, F
was determined to be 0.38 moles. The mole fraction of methanol of residue B was determined to be
0.25 moles. The mole fraction of methanol of distillate D was to be 0.057. Table 1 shows the
readings of refractive index of the sample taken for every 5 min interval. From table 1 it can be seen
that the temperature increases as the time increase and decrease at the final time taken. The
refractive index changes throughout the experiment. This error could be occurred while taking the
readings in decimal places through refractometer as the difference between the consecutive readings
are very small.
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Table 1: Refractive index reading

Total reflux condition
Time T oC R. I
5 85.1 1.3330
10 87.2 1.3348
15 89.6 1.3369
20 90.2 1.3360
25 89.3 1.327

Table 2 shows the theoretical and experimental values of mole fraction of methanol in liquid phase.
It can be seen that the values of mole fraction of methanol experimental are higher values than the
values of mole fraction in theoretical. This could be due to some errors during the experiment. The
error could be while calculating the readings with decimal places to solve the following required
variables.

Table 2: Theoretical and Experimental values of mole fraction of methanol in liquid phase
Time X X the
10 0.0544 0.225
20 0.0558 0.320
30 0.1856 0.662
40 0.1281 0.444
50 0.0369 0.156
60 0.0538 0.215

4. CONCLUSIONS AND RECOMMENDATION

The experiment was carried out to study the process of packed bed distillation column. The
experiment was conducted under total reflux condition. The error that was calculated is 2.61. The
value of minimum plates, Nm that was calculated is 0.84. There is little recommendation that
should be considered for this experiment. More readings should be taken to see the steady state of
the distillation process. A proper source of light should be provided while taking the readings of
refractive index through the refractometer.

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5. REFERENCES

1. Treybal, R. E. (1981). Mass Transfer Operation. McGraw Hill.

2. http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/DistillationColumns/D
istillationColumns.html

3. https://www.scribd.com/doc/219202796/Application-of-Packed-Bed-Column-Distillation-
in-Industry

APPENDIX
Data

Relative volatility 3.32

Molecular weight of methanol MM 32 g/mole
Molecular weight of Water MW 18 g/mole
Enthalpy of feed HF 0 kJ/kmole
Packed height Z 0.90 m

Figure 2: R.I vs x

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Table 3: Value of R.I based on theoretical mole fraction of methanol

Total Reflux Condition

R 1
V 2.5 Litre
Tf 90C
R.I F 1.3300
R.I B 1.3356
R.I D 1.327

The property of methanol of methanol () at temperature T_F from data book:

V = 782.771 kg/m3
XF = 0.38
XD = 0.057

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XB = 0.25

M
M 1000 (1)
F V
782.771 X 15
= 32 x 1000

= 0.37 kmole

x FxD
B F (2)
x BxD
0.380.057
= 0.37
0.2500.057

= 0.619 k.mole

F xF
(3)
BxB
0.37 0.37
= In [ 0.040 0.240 ]

= 10.33

F 1x F
In (4)
B 1x B
0.37 10.036
=3.32 In 0.04010.240

= 8.17

F xF F 1x
E= BxB
- In B 1x
F
(5)
B

= 10.33 -8.17

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= 2.16

x D 1x B
x B 1x D 1 (6)
Nm
In

0.056 10.240
= 0.240 10.056 -1
3.32
= 0.84

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