A

LABORATORY REPORT

ON

EXPERIMENTAL WORK ON

FRCTIONAL DISTILLATION

WHICH WAS PERFORMED ON

THE 31ST OF MARCH, 2021

BY

ADEKOYA IFEOLUWA ISAIAH

CHE/2016/006

OF

GROUP 2

AND SUBMITTED TO

DR. O. SANDA

IN PARTIAL FULFILMENT OF THE REQUIREMENTS FOR

UNIT OPERATIONS LABORATORY I

(CHE 409)

DEPARTMENT OF CHEMICAL ENGINEERING,

OBAFEMI AWOLOWO UNIVERSITY,

ILE-IFE,

OSUN STATE.

JUNE, 2021.
 Department Of Chemical Engineering,

Obafemi Awolowo University,

Ile-Ife,

Osun state.

June, 2021.

The Coordinator,

Unit Operations Laboratory I (CHE 409),

Chemical Engineering Department,

Obafemi Awolowo University,

Ile-Ife,

Osun state.

Dear Sir,

LETTER OF TRANSMITTAL

I, Adekoya Ifeoluwa Isaiah, with student registration number CHE/2016/006, write to

submit the report on the laboratory experiment conducted on “Fractional Distillation”.

The experiment was performed on the 29th of March, 2021 in the Chemical

Engineering department of Obafemi Awolowo University, Ile-Ife, Osun state.

This is done in partial fulfilment of the requirements for Unit Operations Laboratory I

(CHE 409).

Yours Faithfully,

Adekoya Ifeoluwa Isaiah

CHE/2016/006

II
 ABSTRACT

The calibration and testing of a fractional distillation column is carried out in order for

it to be utilized later to separate mixtures occurring in the processes under

investigation by improving the process, and the bi-methanol water system is

employed as the test system. The experiment's goals were to calculate the system's

mass-energy balance equation, record column phase temperatures, and determine feed

and distillate concentrations, as detailed in the report.

The approach employed was well outlined in this paper, which included detailed

descriptions of the numerous stages used throughout the experiment. The equipment

and supplies utilized are likewise meticulously documented.

The result includes computations, graphs, and tables for the data gathered during the

experiment as well as data that is predicted to be derived from the obtained

environmental data. This report details the different procedures that were conducted

throughout the experiment and explains the approach utilized. This report includes

calculations, graphs, and tables of the data collected during the experiment.

III
 TABLE OF CONTENTS

LETTER OF TRANSMITTAL ……………….…………………………….……….II

ABSTRACT ...………………………..……………..……………………………….III

TABLE OF CONTENTS .………………………..………………….……….……IV

LIST OF FIGURES …..……………………………….………………………….…VI

LIST OF TABLES ……...……………………….…..……………………………...VII

CHAPTER ONE: INTRODUCTION

1.1 A Brief Background On Fractional Distillation ………..……..……………1

1.2 Literature Review ……………………………………………………….….1

1.3 Theoretical Background ……………………………………………………...2

1.4 Objective Of Experiment ………………………………….……………….…4

1.5 Scope Of Experiment ………………………………………………………...5

CHAPTER TWO: EXPERIMENTAL PROCEDURES

2.1 Apparatus And Materials Used .………...………………..…………………..6

2.2 Starting Up The Fractional Distillation Apparatus ……..………………….8

2.3 Shutting Down The Fractional Distillation Apparatus …...………………..9

2.4 Assumptions ……………………………………………………………….…9

2.5 Precautions And General Notes ……………………………………………...9

CHAPTER THREE: RESULTS AND DISCUSSIONS

3.1 Results And Conclusions ……………………..………………………..…..11

CHAPTER FOUR: CONCLUSION AND RECOMMENDATIONS

IV
 4.1 Conclusion ……………………………………………………………….17

4.2 Recommendations ..………………………………………………………17

REFERENCES …..…………..………………………………………………………18

APPENDIX A: PARTS OF FRACTIONAL DISTILLATION COLUMN ………...19

APPENDIX B: DEFINITION OF TERMS………………………………………….22

APPENDIX C: GROUP MEMBERS ……………………………………………….24

V
 LIST OF FIGURES

Figure 1: Distillation Curve …………………………………………………………..3

Figure 2: Fractional Distillation Column …………………………………………….6

Figure 3: Schematic Diagram Of fractional Distillating Column …………………….7

Figure 4: Plot of refractive index against liquid mole fraction ……………………..12

VI
 LIST OF TABLES

Table 1: Showing the calibration data plot …………………………………………..11

Table 2: Fractional distillation experimental data …………………………………...12

Table 3: Showing the liquid mole fraction for the distillate and bottoms ………….13

Table 4: Showing the rotameter readings …………………………………………..13

VII
 CHAPTER ONE

INTRODUCTION

1.1 A Brief Background On Fractional Distillation

Distillation is a separation method that is used in separating two miscible liquids with

appreciable differences in boiling temperatures. If the boiling points of the

components are too close together, however, a simple distillation is incapable of

achieving considerable purification. When the difference in boiling points is less than

100 degrees Celsius, a modification is required, which involves inserting a

fractionating column between the distillation flask and the three-way adapter (in

laboratory-scale fractional distillation).

Without disassembling the equipment, a fractionating column effectively enables for

several consecutive distillations to take place at the same time. Indentations or a

packing material with a lot of surface area can be found in a fractionating column.

The vapours condense on these surfaces for a short time, and the heat from the

distillation permits the liquid pools to evaporate again. Every

vaporization-condensation occurrence (also known as a "theoretical plate") is

analogous to a simple distillation in that it enriches the distillate in the lower boiling

component (McCabe et al., 2005).

In industrial scale fractional distillation, the fractionating column is much larger than

the one used in laboratories. However, both scales follow the same laws and can be

modelled in exactly the same way.

1.2 Literature Review

The subject of distillation has gathered a huge library of resources as well as years of

testing and experiments. As a result, we now have a wealth of knowledge on the

1
subject. This growth can also be attributed to its widespread usage as a separation

method in industry and laboratories.

Distillation takes use of several physic-chemical characteristics of fluids, despite the

fact that it is commonly used. It simply happens due to differences in certain of these

characteristics among molecules in a combination. However, there are words

connected with the entire process that must be understood before comprehending the

mechanism.

McCabe et al. (2005) gives an in-depth analysis of the distillation theory, distillation

parameters, and modelling. Great care was also taken in explaining binary systems

and binary distillation as a separation process.

1.3 Theoretical Background

Methanol and water were chosen for use in this experiment because they are both

available in high purity and at low cost, and because the properties of the pure

components and of their mixtures are readily available in the literature. A distillation

curve such as the one shown below can be used to demonstrate fractional distillation

principles.

2
 Figure 1: Distillation Curve

McCabe et al. (2005) offers sufficient insight into the theories developed in the use of

fractional distillation as a separation process, including laws and mathematical models.

Some of these laws and equations were used in calculations made in the course of this

experiment and are discussed below.

For pure substances, the Antoine equation belongs to a family of semi-empirical

correlations that describes the relationship between vapour pressure and temperature.

The Clausius–Clapeyron relation is used to generate the Antoine equation. Louis

Charles Antoine (1825–1897), a French engineer, proposed the equation in 1888

(Roizard, 2015). Antoine devised an equation for predicting the vapor pressure of

pure liquids (vaporization) and solids (sublimation) (Antoine, 1891). It is worth

mentioning that, due to its precision, this equation is still extensively employed today.

Mathematically, this equation is:

3
 �
log10 (�) = � − (1)
� + �

where:

p = absolute vapour pressure

T = temperature (in Celsius)

A, B, C = Antoine constants (constant specific)

Also, the quantity of heat required to move from a hot side to a cold side over a unit

of time is known as the condenser's heat duty. Mathematically,

Q = MCp ∆T (2)

Where:

Q = heat duty

M = mass flow rate of fluid

Cp = heat capacity of fluid

∆T = temperature change

1.4 Objective Of Experiment

The material and energy balances of the methanol-water system were modelled and

used to mathematically describe the operations of the column. A record of the

temperatures of the column stages (T1 - T6) were recorded and used determine the

compositions of the methanol vapour at the different times using Antoine equation.

Also, the condenser heat duty, enthalpies of feed, distillate and bottoms, feed quality

and number of stages at total reflux were calculated theoretically and used to check

for correspondence with experimental values.

Finally, the overall column efficiency and Murphee efficiency of each plate were

determined. The results were then compared with the values obtained using a

simulation package.

4
1.5 Scope Of Experiment

This experiment covers distillation, in particular fractional distillation of

methanol-water system, and mathematical modelling using Process Dynamics.

5
 CHAPTER TWO

EXPERIMENTAL PROCEDURES

2.1 Apparatus And Materials Used

Methanol and water were the materials used in the fractional distillation experiment in

this laboratory session.

The apparatus used in this laboratory session was a small-scale fractional distillation

column.

Figure 2: Fractional Distillation Column

6
To better understand the procedures that went into the laboratory session, a schematic

diagram is provided below.

Figure 3: Schematic Diagram Of Fractional Distillation Column

7
Appendix A provides a detailed breakdown of the parts of the Fractional Distillation

Column used in this experiment.

2.2 Starting Up The Fractional Distillation Apparatus

The feed reservoir tank was charged through the spring-loaded opening C1 with 8

gallons of the mixture to be distilled Afterwards, the boiler was charged by

connecting the flex-tubing feed line to the boiler top through the quick-disconnect

coupling Q1.

Thereafter, the feed line was traced from the reservoir tank through the pump and feed

rotameter, opening valves F1 and bypass F3, closing the drain valve D-1 and

rotameter valves F2 and F4.

The main power switch was then turned on, and then the feed pump switch. The pilot

lights indicated that these units were on. The liquid level was observed as it rose in

the boiler sight glass. When the liquid approached the 3/4-full mark, the bypass F3

was shut off and the valves F2 and F4 were opened to meter the remaining charge

through the rotameter.

Then the heating cycle began by checking both the thermocouple and sample port

tube fitting connections to ensure that they were properly sealed on each plate

location. The boiler power switch was then turned on and a pilot light indicated heat

input.

After, a flow of water was started through the condense with the rotameter set at a low

value. As the boil-up proceeded, the rotameter was adjusted until the top section of

the condenser near the vapour inlet line was just warm to the touch. The proportional

power control switch for the boiler was set to the desired heating rate value to

8
expedite the start-up. The boiler temperature was monitored constantly with the

bimetallic thermometer T13, attached to the boiler front.

While the system was heating up, the distillate receiver overflow valve R2 was

opened to permit venting back to the reservoir tank. The distillate drain valve R3 was

closed and the the distillate line valve R1, which led to the suction side of the reflux

pump, were closed. The recycle pump was also turned off.

The temperature was observed as the distillate began to collect in plates above the

boiler. Steady-state operation took roughly 30 minutes. As the distillate collected in

the distillate receiver, the reflux pump was turned on and using valve R4, a reflux rate

was maintained. This reflux rate was a value that was sufficient to manually control

the level in the distillate receiver.

The pressure relief values (PRV) were then set to open at approximately 1.0 psig.

2.3 Shutting Down The Fractional Distillation Apparatus

The boiler power switch was turned off. When the condensate no longer collected in

the distillate receiver, the reflux pump was turned off. The valve R1 was closed and

the valve R3 was opened. The valve R3 was left opened so the system remained

vented. After, the main power control switch was turned off.

2.4 Assumptions

The column operating pressure is assumed to be 760 mmHg.

2.5 Precautions And General Notes

The following precautions were observed during the course of the laboratory session:

1. Great care was taken in handling methanol as it is a toxic material. The liquid can

9
be absorbed through the skin and the vapour through the lungs via inhalation, and has

debilitating effects on the nervous system, the optic nerves and retinas.

2. It was necessary to periodically monitor the liquid level in the boiler during the

course of the experiment. This was in case the liquid level were to drop below the

electrical heating coils in the boiler, for any reason. In case of this, a thermal overload

switch, set to respond at 240oF, would interrupt the power line. This overload switch

is in the 250-Watt auxiliary heater located on the right side of the boiler. The thermal

overload switch, however, is the red button located in the centre of the apparatus.

Note that this device is manually reset and cannot be reset until the boiler temperature

drops below the trigger value.

3. The boiler was turned to full power before boiling began, but throttled back to the

desired value when boiling began.

4. The pressure relief valves (PRV) are located at the top of the distillate receiver and

on the shell side of the condenser.

10
 CHAPTER THREE

RESULTS AND DISCUSSION

3.1 Results And Discussion

Refractive index = 0.378

Temperature on entry = 800C

Rotameter reading for feed = 95

Rotameter reading for reflux = 63

Table 1: Showing the calibration data plot

Liquid mole fraction of methanol Refractive index

0 0

0.1 0.07547

0.2 0.15094

0.3 0.22641

0.4 0.30188

0.5 0.37735

0.6 0.45282

0.7 0.52829

0.8 0.60376

0.9 0.67922

1 0.75469

11
 Figure 4: Plot of refractive index against liquid mole fraction

Table 2: Fractional distillation experimental data.

Time Plate 1 Plate 2 Plate 3 Plate 4 Plate 5 Refractive Liquid mole

(mins Temp. Temp. Temp. Temp. Temp. index of fraction of

) (°C) at (°C) at (°C) at (°C) at (°C) at distillate at methanol at

54Kpa 48kPa 46kPa 40kPa 57kPa Plate 5 Plate 5

2 50 46 46 46 46 1.020347 1.296

4 52 48 52 52 52 0.735827 1.0003

6 55 55 55 55 55 0.62036 0.8213

8 60 59 60 60 60 0.4596 0.6090

10 68 65 65 65 65 0.3306 0.4380

12 69 72 72 72 72 0.1879 0.2490

14 73 73 73 73 73 0.1706 0.2260

16 76 76 76 - 75 0.1381 0.1830

12
18 78 78 78 - 78 0.09358 0.1240

20 79 79 78 - 79 0.07924 0.1050

22 79 79 78 - 79 0.07924 0.1050

24 80 80 79 - 80 0.06566 0.08700

26 80 80 - - 81 0.05283 0.07000

30 81 - - - 83 0.02868 0.03803

Table 3. Showing the liquid mole fraction for the distillate and bottoms.

Refractive index Liquid mole fraction

Distillate 0.5660 0.74997

Bottoms 0.0032 0.00424

F= 1.99R-14.4 for feed

F= 2.04R-13.2 for reflux

Table 4. Showing the rotameter readings.

Rotameter reading

Feed 95

Reflux 63

For feed,

F = 174.65 cm3/min

For reflux,

13
F = 115.32 cm3/min

Temperature on entry is 80˚C

F=D+B

��� = ��� + ���

Solving simultaneously,

D = 116.32 cm3/min

B = 58.34 cm3/min

Antoine equation is used to get the saturated pressures for the plates at different

temperatures.

���� �
ln =�−
��� � °C + �

where A, B and C are constants gotten from tables and t is the temperature in degree

Celsius

For methanol,

A = 16.5785

B = 3638.37

C = 339.50

For water,

A = 16.3872

B = 3885.70

C = 230.170

and

������ − �0 �����
����ℎ���� =
�0 ���ℎ���� − �0 �����

14
 ����ℎ���� ∗ �0 ���ℎ����
����ℎ���� =
������

Hence,

i) Condenser heat duty = Mass flow rate (latent heat of condensation-latent heat

of vaporization) = 100.02 cm3/min* 0.7913g/ cm3*(-1100) J/g

=-87060J/min=-1451Watts.

Enthalpy = mCpT where m = mass, Cp = Specific heat capacity of methanol, T =

Temperature difference, J is Joules, W is watts

ii) Enthalpies of feed(hf)= 0.50086mol*32g/mol*2.53J/gK*80K= 3243.97J,

Enthalpy of distillate = 0.7499mol*32g/mol*2.53J/gK *58K = 3521.29J

and Enthalpy of bottoms= 0.00424mol*32g/mol*2.53J/gK *82K= 28.15 J,

iii) Feed quality(q) = Heat needed to vaporize 1 mole of feed at entering

conditions/molar latent heat of vaporization= Hv-Hf/Hv-Hl where, Hl =

enthalpy of liquid at boiling point =0.296mol*32g/mol*2.53J/gK * 64.7K

=1550.48J, Hv = enthalpy of vapour at boiling point=

0.632mol*35.21kJ/mol=22.25kJ = 22252J, q=

22252-3243.97/22252-1550.48 = 0.918

iv) The number of stages at total reflux = 5.3stages as shown in Figure 4.5a

above which corresponds to the actual number of stages on the equipment.

v) Overall column efficiency= Ratio of Theoretical to Actual number of stages=

5.3/6 =0.8833

15
and the Murphree efficiency of each plate = EMV = yn - yn+1/ yn * - yn+1 = actual change

in vapor /change in vapor at equilibrium

For Plate 1 = 0.094-0.04 /0.16-0.04= 0.45

For Plate 2 = 0.984-0.094/1-0.094= 0.8802

For Plate 3= 0.998-0.984/1-0.984 = 0.875

For Plate 5= 0.984-0.956/1-0.956 = 0.6363

16
 CHAPTER FOUR

CONCLUSION AND RECOMENDATIONS

4.1 Conclusion

The results of the experiment revealed that for optimal distillation efficiency, the

distillation rate must be kept steady and slow. The most essential variable is the

distillation rate.

4.2 Recommendations

The fractional distillation process and modellings associated with this separation

process should be studied as a purely practical course to further aid students’ learning

and understanding of the concept in Chemical Engineering.

17
 REFERENCES

Antoine C (1891) Annales de Physique et de Chimie 22: 281; ibid, Annales de

Physique et de Chimie (1892) 26: 426; Comptes Rendus Acad Sci (Paris) (1888)

107: 1143

McCabe, W. L., Smith, J. C., & Harriott, P. (2005). Unit operations of chemical

engineering.

Roizard D. (2014) Antoine Equation. In: Drioli E., Giorno L. (eds) Encyclopedia

of Membranes. Springer, Berlin, Heidelberg.

https://doi.org/10.1007/978-3-642-40872-4_26-1

18
 APPENDIX A

Parts Of Fractional Distillation Column

1. Feed Tank Reservoir: The feed tank has a capacity of about 10 gallons with a

sloping bottom for proper drainage. The reservoir is fitted with a liquid-level sight

glass.

2. Still Boiler: The boiler tank (capacity approximately 5 gallons) is fitted with a

quick disconnect coupling inlet, a pressure measurement port and a sight glass for

visual liquid level indication. The main heating element is a stainless steel sheathed

bayonet-type cartridge heating element. This element has a continuously-variable

control and is rated at 2500 Watts. Precise liquid level control is obtained by means

of a float-type control element that actuates a solenoid-operated valve which recycles

excess liquid from the still boiler to the feed reservoir. The boiler also has a dial-type

temperature indicator.

3. Condenser: The condenser is a shell-and-tube heat exchanger which contains the

equivalent of 1.5 sq. ft. of spiral-tube heat exchange surface. The tube side coolant is

water for this project. Countercurrent coolant flow through the tube is metered by

means of a rotameter. For pressure safety, a spring-loaded relief valve (set for 1.0 psig)

is connected to the shell side of the condenser. The shell side condensate drains

through a 3/8-inch line to the distillate receiver.

4. Distillate Receiver: Condensate enters from the condenser through a 3/8-inch

stainless steel tube into the top of the receiver. The top flange also contains a spring

loaded pressure relief valve set at 1.0 psig. From the bottom are three connections: a

valve drain, a valve inlet to the reflux pump, and an overflow standpipe return to the

main feed reservoir.

19
5. Instrumentation and Control Panel: The panel includes a voltmeter and ammeter

for power input and indication, a boiler liquid level control switch for automatic

operation (not in use at this time), a boiler thermal-overload indicator, on-off

electrical switches for feed and reflux pumps, and a continuously variable control

element for the main boiler heater. The main system power is controlled by means of

a circuit breaker, on-off switch, and indicator light. In addition, indicator lights are on

circuits for the feed and reflux pumps.

6. Thermocouples: The system includes twelve thermocouples: one in the still boiler,

six in the column (one for each sieve plate tray), two on the condenser inlet and outlet

lines, one for the distillate line, and one for each preheater.

7. Rotameters: The calibration for the reflux rotameter (calibrated with water at 21

oC over the range 20 to 100 on the tube scale) is given by:

F = 2.04R − 13.2

where F is the flow rate in cm3/min, and R is the rotameter reading. For the feed

rotameter (calibrated with water at 17oC over the range 10 to 100 on the tube scale).

F = 1.99R − 14.4

8. Column: The column consists of 6 sieve plate sections, each assembled from a 5-

inch-long, 3-inch ID glass pipe section, and a stainless steel process ring with four

connections. Each section contains fittings for feed, pressure measurement, liquid and

vapor sampling, and weir-downcomer adjustment. The plate column, when assembled,

is approximately 30 inches in height. On each plate the weir and downcomer are

readily accessible for adjustment purposes.

9. Plates: Each plate in the column is perforated with 36 holes of 3/32-inch diameter,

with center-to-center spacing of 0.265 inches (square pitch). The plate thickness is

20
0.125 inches; the space between plates is 6 inches. The opening for the downcomer

has a diameter of 0.534 inches.

21
 APPENDIX B

Definition Of Terms

1. Distillation: This is the the process of separating components or substances

from a liquid mixture by using selective boiling and condensation. It exploits

the relative volatility of the components in a mixture. It is a unit operation and

is considered a physical separation process.

2. Fractional Distillation: Fractional distillation is a type of distillation which

involves the separation of miscible liquids. The process involves repeated

distillations and condensations. The mixture is then usually separated into

component parts. The separation happens when the mixture is heated at a

certain temperature where fractions of the mixture start to vaporize. The basic

principle of this type of distillation is that different liquids boil and evaporate

at different temperatures. So when the mixture is heated, the substance with

lower boiling point starts to boil first and convert into vapours.

3. Batch Distillation: Batch distillation is the use of distillation in batches such

that a mixture is distilled to separate it into its component fractions before

the distillation column is fed with more mixture and the process is repeated.

4. Boiling Point: The boiling point of a liquid is the temperature at which its

vapour pressure is equal to the pressure of the gas above it. It is the

temperature at which the vapour pressure of the liquid is equivalent to one

atmosphere (760 torr).

5. Volatility: Volatility is a material quality which describes how readily a

substance vapourizes. In at a given temperature and pressure, a substance with

high volatility is more likely to exist as a vapour, while a substance with low

22
 volatility is more likely to be a liquid or solid. It can also be a measurement of

the tendency of a vapour to condense into a liquid or solid.

6. Condensation: Condensation is a change in state from gas or vapour form

into liquid form. It generally happens when vapour in warm air encounters a

cool surface. But condensation doesn't need a solid surface to take place, as

it can occur when a warm pocket of vapour encounters colder gasses.

7. Reflux: Reflux is a distillation technique involving the condensation of the

distilled product vapours and the return of a portion of the condensate to

the distillation system from which it originated.

23
 APPENDIX C

Group Members

CHE/2016/006 ADEKOYA IFEOLUWA ISAIAH

CHE/2016/019 AKINLEYE OYINBAYODE PETERS

CHE/2016/025 ANIFOWOSE MOYINOLUWA BLESSING

CHE/2016/036 EFUNYOLA DAVID OPEYEMI

CHE/2016/042 FAJOBI DAVID OLANREWAJU

CHE/2016/055 OBAZENU OGHENETEGA ILERIOLUWA

CHE/2016/063 OLADELE EMMANUEL

CHE/2016/073 OSIJONWO OLUWATOMISIN PRECIOUS

CHE/2016/079 SANNI MUHAMMED OPEOLUWA

CHE/2016/095 OBIENYI PEACE OLUEBUBE

CHE/2016/100 ONUK UTIBEABASI ETETIM

24