EKB 2131 Chemical Engineering Lab - III

Bachelor of Chemical Engineering (Hons)

LAB REPORT

EKB 2131 - CHEMICAL ENGINEERING LAB - III

EXPERIMENT TITLE SIEVE PLATE DISTILLATION COLUMN

NAME OF CANDIDATE
SHAMINI SATHIVEL
WITH REG NO.
SESSION DATE 05th NOVEMBER 2015, Thursday
DATE OF SUBMISSION 19th NOVEMBER 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 Uttaran
Mr.Arasu CONTENTS
Lab Report

CHEM. ENGG. LAB-IV INCHARGE

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Total (Dr. TVN. Padmesh/Arasu Uttran)
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 8

4 Conclusions and Recommendations 9

5 References 10

Appendix 10

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ABSTRACT

The experiment was carried out to study the process of sieve plate distillation column. The moles
fraction of methanol in feed, bottom 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 0.3 moles. The mole fraction of methanol of bottom B was determined to be 0.35
moles. The mole fraction of methanol of distillate D was to be 0.75. The error that was calculated is
-0.1086. Rayleigh equation for batch distillation was verified.

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

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It is used in distillery for producing alcohol

1.1.3 Types of Distillation Columns

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 Sieve Plate Distillation Column

A sieve plate is designed to bring a rising stream of vapor into intimate contact with a descending
stream of liquid. The liquid flows across the plate and passes over a weir to a downcomer leading to the
plate below. In a sieve tray, the vapour passes through a large number of "holes" known as perforations
(sieves) and emerges through the liquid in a vertical direction [2]. The sieve tray has the simplest
design among the various tray types. There are no mechanical moving parts. There is no liquid seal and
it is the passage of vapour that effectively prevents the loss of liquid through the sieves. A phenomenon
known as weeping in which occur at low vapour flow and/or high liquid rates when the liquid height on
the tray exceeds the tray pressure drop. Typical sieve sizes used industrially range from as small as
1/16-inch to 1-inch. Small sieves are not suitable for fouling or corrosive services as they may be
susceptible to blockage, leading to excessive pressure drop and premature flooding [2]. Small holes
have better turndown characteristics because they reduce tray weeping and therefore increase tray

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capacity. In terms of cost, larger holes are cheaper as the holes can be punched, and there are fewer
holes to be punched. Smaller holes are more expensive as drilling may be required.

1.2.1 Advantage and Disadvantage of Sieve Plate Distillation Column

Advantages
Least expensive column for diameters greater than 0.6m
The liquid-vapor contact in the cross-flow of plate columns is more effective than
countercurrent-flow in packed columns.
Cooling coils can be easily added to the plate column
Can handle high liquid flow rates.

Disadvantages
Higher pressure drops than packed columns
Foaming can occur because the liquid is agitated by the vapor flowing up through it.

2. MATERIALS AND METHODS

Valve
V1 Feed Supply Valve of Funnel
V2 Air Vent Valve for Vessel
V3 Product Outlet Valve of Tray 1

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V4 Product Outlet Valve of Tray 2

V5 Product Outlet Valve of Tray 3
V6 Product Outlet Valve of Tray 4
V7 Product Outlet Valve of Tray 5
V8 Product Outlet Valve of Tray 6
V9 Product Outlet Valve of Tray 7
V10 Air Vent Valve for Condenser
V11 Valve for Distilate Collection
V12 Water Flow Control Valve
V13 Drain Valve for Vessel

2.1 Starting Procedure

1. The ON/OFF switches given on the panel was ensured at OFF position.

2. Vessel was filled with methanol-water solution by opening the funnel valve V 1 and air vent valve

3. The funnel valve V1 and the air vent valve V2 were then closed.

4. The main power supply was switched ON.

5. The temperature of solution above boiling point of methanol was set at 90C
6. The heater was switched ON.

7 The cyclic timer was on and the total reflux condition was set.

8. The air vent valve V10 was open which is provided at the top of condenser and after observing
vapour coming out, the valve V10 was closed.

9. The pump and the condenser cooling water flow rate was set by adjusting the valve V 12.

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10 Waited till required temperature achieved steady state condition .

11 The temperatures of each tray were note down.

12. The samples from each tray were taken down by opening the valve V 3-V9.

13. The distillate and bottom product was also collected by opening the valve V 11 and V13 respectively.

14. The samples were cool down to room temperature and their refractive indices was measured.

2.2 Closing Procedure

1. The water supply was stopped when the experiment was over.
2. The main power supply was switched off.
3. After 10 minutes, the water supply was stop.
4. The vessel was drained after temperatures fall down to atmospheric values by opening the valve
V13.

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 F x D
B= F (2)
x Bx D

F xF
[ ] (3)
BxB

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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)
N m=
In

Figure 1 shows the set-up consists of column with seven sieve trays. A vessel is provided with
funnel, at the bottom of the column. A sight glass is provided with it and two other sight glasses is
given at middle of the column. Safety valve and pressure gauge are given at vessel. A tank is provided
to collect the bottom product. Shell and tube type condenser is provided to condensate the vapour.
Reflux drum is provided to collect the condensate. Receiving tank is for collecting the distillate. Seven
valves are provided at each plate for collecting the samples. Drain valves are provided for drainage
purpose. Temperature sensors are fitted at the appropriate place to measure the temperatures
Figure 1: Block Diagram of Sieve Plate Distillation Column

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3. R
E
S
U
L
T
S

AND DISCUSSION

Table 1 shows the readings of the mole fraction of feed, bottom and distillate are based on the
corresponding value to refractive index readings respectively from the R.I vs x graph as shown in
Figure 4 in Appendix. In this experiment the volume of methanol used is 25 litres. The temperature of
the feed is 95C. Since the experiment was conducted in total relux condition, therefore the R value is
1.

Table 1: Mole fraction of feed, bottom and distillate

R.I x
Feed (R.I.F) 0.3 (x.F)
Bottom (R.I.B) 0.35 (x.B)
Distillate (R.I.D) 0.75 (x.D)

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Table 2 shows the refractive index readings of each tray samples at total reflux condition. The
refractive index readings in each tray show different values. The experimental value of mole fraction of
methanol in liquid phase couldnt be determined. This is because in order to determine the
experimental mole fraction, the refractive index should be less than 1.3370 based on the table 3 shown
in Appendix. However some of the refractive index samples that are obtain is more than 1.3370.
Therefore the experimental value of mole fraction for each sample couldnt be determined. There could
be some error while conducting the experiment. Parallax error might have occurred as the eye might
have been wrongly positioned while taking the readings of refractive index of samples. Moreover there
wasnt a proper source of light while taking the refractive index reading in the refractometer. This
causes difficulties while taking the readings.

Table 2: Readings of refractive index samples from each tray

TOTAL REFLUX CONDITION

Sr.No Valve T( C) R.I
1 3 94.5 1.3358
2 4 94.4 1.33265
3 5 93.8 1.33795
4 6 93.3 1.339105
5 7 92.3 1.332125
6 8 90.7 1.332513
7 9 87.2 1.33115

4. CONCLUSIONS AND RECOMMENDATION

The experiment was carried out to study the process of sieve plate distillation column. The error
that was determined is -0.1086. From this experiment Rayleigh equation for sieve plate distillation
column was verified. There is little recommendation that should be considered for this experiment. A
proper source of light should be provided while taking the readings of refractive index through the
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refractometer. This can ensure an accurate reading of refractive index. There were less conical flasks to
collect the sample for each tray. Some conical flask was reused to collect sample for other trays. The
mixture of different samples could have affected the refractive index readings. More conical flasks
should be provided to collect the sample from each trays of sieve plate distillation column.

5. REFERENCES

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

2. http://www.separationprocesses.com/Operations/POT_Chp02a.htm
3. http://seperationtechnology.com/distillation-column-tray-selection-1/

APPENDIX
Data obtain

Relative volatility 3.32

Molecular weight of methanol M 32 g/mole
Molecular weight of water Mw 18 g/mole
Actual number of plates NA 7
Enthalpy of feed HF 0 kJ/kmole

R 1
V 2.5 Litre
TF 95C
R.IF 1.3447
R.IB 1.34475
R.ID 1.3358

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Figure 4: Graph of R.I vs x

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

V = 722 kg/m3
xF = 0.3
xD = 0.75
xB = 0.35

V
F = (1)
M m 1000
= [(725) (2.5)]/ (3.2 x 1000)
= 0.566 k mole

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X B XD

B = X F X D F (2)

0.30.75
= x 0.0564
0.350.75
= 0.0635 kmole

F XF
In [ ] (3)
B X B
0.0564 x 0.3
= ln[ ]
0.0635 x 0.35
= -.0.2789

F(1X F )
(4)
B(1X B )
0.0564 (10.3)
=3.32 x ln[ ]
0.0635(10.35)
= -.0.1712

F XF F(1X F )
E =In [ ] - (5)
B X B B(1X B )
= -0.2798-(-0.1712)
= -0.1086

Number of minimum stages can be calculated using the Fenske equation below:

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x D ( 1x B ) 0.75 (10.65 )
ln [ ] ln [ ]
Nm = x B ( 1x D ) 1= 0.35 (10.25 ) 1 (6)
ln ln3.32
= 0.43 1

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