MANIPAL INTERNATIONAL UNIVERSITY

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)
Mr.Arasu Uttaran
Lab Report
CHEM. ENGG. LAB-IV INCHARGE
Total (Dr. TVN. Padmesh/Arasu Uttran)

School of Science and Engineering

EKB 2131 – Chemical Engineering Lab - III

TABLE OF CONTENTS

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
• It is used in distillery for producing alcohol

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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 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.

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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
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

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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 V1 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 90°C
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 V12.

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 V3-V9.

13. The distillate and bottom product was also collected by opening the valve V11 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.

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2.3 Formulae used

To calculate the moles of methanol in feed

𝑭 = (𝝆𝑽)/(𝑴𝑴 × 𝟏𝟎𝟎𝟎) (1)

To calculate the moles of methanol in residue

𝒙𝑭 −𝒙𝑫
𝑩= ×𝑭 (2)
𝒙𝑩 −𝒙𝑫

𝑭𝒙
𝑰𝒏[𝑩𝒙𝑭 ] (3)
𝑩

𝑭(𝟏−𝒙 )
𝜶𝑰𝒏 [𝑩(𝟏−𝒙𝑭 )] (4)
𝑩

To calculate the error

𝑭𝒙 𝑭(𝟏−𝒙 )
E = 𝑰𝒏[𝑩𝒙𝑭 ] - 𝜶𝑰𝒏 [𝑩(𝟏−𝒙𝑭 )] (5)
𝑩 𝑩

To calculate minimum number of plates

𝒙 (𝟏−𝒙𝑩 )
[𝑰𝒏 𝑫 ]
𝒙𝑩 (𝟏−𝒙𝑫 )
𝑵𝒎 = { }–1 (6)
𝑰𝒏𝜶

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

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Figure 1: Block Diagram of Sieve Plate Distillation Column

3. RESULTS 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 95°C. 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 couldn’t 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 couldn’t
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 wasn’t 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 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

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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 α 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 95°C
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 (ρ) at temperature T_F from data book:

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

𝝆𝑽
F =𝑴 (1)
𝒎 ×𝟏𝟎𝟎𝟎

= [(725) (2.5)]/ (3.2 x 1000)

= 0.566 k mole

𝑿 −𝑿𝑫
B = 𝑿𝑭 ×𝑭 (2)
𝑩− 𝑿𝑫

0.3−0.75
= 0.35−0.75 x 0.0564

= 0.0635 kmole

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𝑭×𝑿
In [ 𝑩×𝑿 𝑭 ] (3)
𝑩

0.0564 x 0.3
= ln[0.0635 𝑥 0.35]

= -.0.2789

𝐅(𝟏−𝐗 )
𝛂 𝐈𝐧 𝐁(𝟏−𝐗𝐅 ) (4)
𝐁

0.0564(1−0.3)
=3.32 x ln[0.0635(1−0.35)]

= -.0.1712

𝑭×𝑿 𝑭(𝟏−𝑿 )
E =In [𝑩×𝑿𝑭 ] - 𝜶 𝑰𝒏 𝑩(𝟏−𝑿𝑭 ) (5)
𝑩 𝑩

= -0.2798-(-0.1712)
= -0.1086

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

𝒙 (𝟏−𝒙𝑩 ) 𝟎.𝟕𝟓(𝟏−𝟎.𝟔𝟓)
𝐥𝐧 [ 𝑫 ] 𝐥𝐧 [ ]
𝒙𝑩 (𝟏− 𝒙𝑫 ) 𝟎.𝟑𝟓(𝟏−𝟎.𝟐𝟓)
Nm = –1= –1 (6)
𝐥𝐧 𝛂 𝐥𝐧 𝟑.𝟑𝟐

= 0.43 ≈ 1

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