A

LABORATORY REPORT ON

FRACTIONAL DISTILATION EXPERIMENT

SUBMITTED BY

ALADELO OYINDAMOLA ENIOLA

CHE/20216/023

GROUP 4

SUBMITTED TO:

DR SANDA

DEPARTMENT OF CHEMICAL ENGINEERING

OBAFEMI AWOLOWO UNIVERSITY

ILE-IFE

ON

21ST JUNE,2021

IN PARTIAL FUFILMENT OF THE REQUIREMENT FOR CHEMICAL

ENGINEERING UNIT OPERATIONS LABORATORY I

(CHE 409)

DATE OF EXPERIMENTAL CLASS: 31ST MARCH,2021

 Department of Chemical Engineering,

Obafemi Awolowo University,

Ile-Ife, Osun State.

June 15th 2021.

The SIWES coordinator,

Dr Sanda,

Department of Chemical Engineering,

Faculty of Technology,

Ile-Ife, Osun State.

Dear Sir,

LETTER OF TRANSMITTAL

I hereby write to inform you that I have fully participated in the Unit Operations Laboratory I

(CHE409) for every part four chemical engineering students. I commenced the course on 6 th

May 2021 and completed the course on 23rd May 2021. The report contains detailed

experimental work and result.

Yours Faithfully,

Aladelo Oyindamola.

ii
 ABSTRACT

Fractional distillation column was calibrated and tested for the separation of mixtures

that occur in processes under consideration by Process Development.

The binary methanol-water system was selected as the test system based on the following

considerations:

(1) Both methanol and water are available in high-purity and at low cost, and

(2) The properties of the pure components and of their mixtures are readily available

Mathematical models describing the operations of the column was obtained through

this process both material and energy balance. Temperature was also used to determine the

compositions of the methanol vapor at the different times

The following were determined after the experiment:

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

number of stages at total reflux, the overall column efficiency and the Murphree efficiency of

each plate with the column operated at steady state with total reflux.

iii
 Table of Contents

LETTER OF TRANSMITTAL ........................................................................................................... ii

ABSTRACT .......................................................................................................................................... iii
LIST OF FIGURES .............................................................................................................................. v
LIST OF TABLES ............................................................................................................................... vi
NOMENCLATURE ............................................................................................................................ vii
CHAPTER ONE ................................................................................................................................... 1
1.1 INTRODUCTION....................................................................................................................... 1
1.2 Scope of the experiment .............................................................................................................. 1
1.3 Objectives of the experiment...................................................................................................... 1
1.4 Fractional Distillation ................................................................................................................. 2
1.5 THEORY OF EXPERIMENT ................................................................................................... 3
CHAPTER TWO .................................................................................................................................. 5
METHODOLOGY ............................................................................................................................... 5
2.1 Materials and Equipment........................................................................................................... 5
2.2 PROCEDURES ........................................................................................................................... 8
CHAPTER THREE ............................................................................................................................ 10
RESULTS AND DISCUSSION ......................................................................................................... 10
3.1 PARAMETERS......................................................................................................................... 10
3.2 CALCULATIONS .................................................................................................................... 15
CHAPTER FOUR ............................................................................................................................... 17
CONCLUSION AND RECOMMENDATION ................................................................................ 17
4.1 CONCLUSION ......................................................................................................................... 17
4.2 RECOMMENDATION ............................................................................................................ 17
REFERENCES .................................................................................................................................... 18
APPENDIX .......................................................................................................................................... 19
APPENDIX A .................................................................................................................................. 19
APPENDIX B .................................................................................................................................. 20
APPENDIX C .................................................................................................................................. 21

iv
 LIST OF FIGURES

Figure 1 A typical tray in a distillation column ......................................................................... 2

Figure 2 A simple McCabe-Thiele diagram .............................................................................. 4

Figure 3 Schematic Diagram of a fractional distillation column ............................................... 6

Figure 4 Factional distillation setup ........................................................................................... 7

Figure 5Plot of Refractive index Vs Liquid mole fraction of methanol .................................. 11

Figure 6 Graph of mole fraction Vs x Methanol...................................................................... 14

Figure 7 Graph of Temperature Vs Mole Fraction ............................................................................... 15

v
 LIST OF TABLES

Table 3-0-1 Table showing calibration test data ...................................................................... 10

Table 3-2 Fractional distillation experimental data ................................................................. 12

Table 3-3 Table showing the liquid mole fraction for the distillate and bottoms .................... 13

vi
 NOMENCLATURE

Psat = Vapor pressure of mixture [kPa]

vpa = Vapor pressure of component a [kPa]

vpb = Vapor pressure of component b [kPa]

ya = mole fraction of component a in vapor phase (dimensionless)

vpa = vapor pressure of component a [kPa]

xa = mole fraction of component a in liquid phase (dimensionless)

Psat = Vapor pressure of mixture [kPa]

x = mole fraction of more volatile in liquid

y = mole fraction of more volatile in vapor

D = moles of distillate withdrawn as overhead per unit time

xD= mole fraction of more volatile component in distillate

o = total moles overflow from one plate to next per unit time

V = total moles vapor passing from one plate to next per unit time

W = moles residue per unit time

n = number of plate under consideration counting from feed

m = number of plate under consideration counting from still

H = enthalpy, or heat content of vapor

h = enthalpy, or heat content of liquid

vii
 CHAPTER ONE

1.1 INTRODUCTION

Distillation is a separation method in which mixtures of liquids are separated into their

individual components. It is also used to purify some liquids by separating impurities from

them.

It separates the mixtures based on their differences in boiling points. The mixture is heated to

separate it into the various components, the gas of desired product is then condensed back

into liquid form and collected. Repeating the process on the collected liquid to improve the

purity of the product is called double distillation.

1.2 Scope of the experiment

The main focus of this experiment was on the calibration and testing of the

fractional distillation column for the separation of mixtures that occur in processes

under consideration by process development using the binary methanol-water system.

This binary methanol-water system was used because both methanol and water are

available in high-purity and at low cost and the properties of the pure components and

of their mixtures are readily available.

1.3 Objectives of the experiment

1. To determine the compositions of methanol vapor at different intervals.

2. The feed quality, number of stages at total reflux, condenser heat duty, the

overall column efficiency, the enthalpies of the feed and the Murphree

efficiency of each plate with the column operated at steady state with total

reflux.

1
 3. To determine overall column efficiency.

4. To construct the equilibrium curve for methanol-water binary system.

1.4 Fractional Distillation

There are different kind of distillation such as simple, fractional, steam, vacuum and short path

distillation. But our main focus in this experiment is Fractional distillation.

In fractional distillation several simple distillations are carried out in one apparatus. It is used

when the boiling points of the components of a mixture are close to each other, as determined

using Raoult's law. A fractionating column is used to separate the components used a series

of distillations called rectification. In fractional distillation, a mixture is heated so vapor rises

and enters the fractionating column. As the vapor cools, it condenses on the packing material

of the column. The heat of rising vapor causes this liquid to vaporize again, moving it along

the column and eventually yielding a higher purity sample of the more useful when the

normal boiling point exceeds the decomposition temperature of a compound.

Figure 1 A typical tray in a distillation column

2
1.5 THEORY OF EXPERIMENT

Distillation is a common process in engineering, basically used to separate various components

of a liquid solution which depends upon the distribution of these components between a vapor

phase and a liquid phase, also all components must be present in both phases and the vapor

phase is created from the liquid phase by vaporization at the boiling point.

as stated by (Geankoplis). .

At a specific temperature and pressure, a certain amount of the mixture moves into the vapour

phase until the vapour reaches the mixture's vapour pressure. The point where this occurs is

known as the vapour-liquid equilibrium. Volatility is a measure of a pure component's vapour

pressure at a set pressure and temperature in a specific mixture. The boiling point of a

mixture is based on the total vapour pressure of a mixture, which is the sum of the vapour

pressures of each component in the mixture. This is known as Dalton's law.

Psat= (vpa+ vpb…) (1)

Raoult's law can be used to determine the volatility or "K-value" of a substance. The mole

fraction of a component in the vapour phase can be found from this.

ya= vpa ∙ xa psat (2)

Not all mixtures obey Raoult's law. Some components that have high solubility with each

other form azeotrope. An azeotrope is a mixture that has either a higher or lower boiling point

than the boiling point of any of the pure components. This means that when a mixture reaches

an azeotrope, such as ethanol and water at 95.6 % water, it behaves as a pure substance.

Determining the size of the tower and the number of trays needed was historically a very

difficult process involving many calculations. The McCabe-Thiele method greatly simplified

that process. The method uses a graphical representation of the material balance equations as

3
operating lines on a graph of the liquid composition (x-axis) and the vapour composition (y-

axis).

Figure 2 A simple McCabe-Thiele diagram

4
 CHAPTER TWO

METHODOLOGY

2.1 Materials and Equipment

Materials and equipment used for the experiment include:

 Fractional distillation unit equipped with a condenser

 Refractometer

 Dropper

 Sample collector

 Funnel

 Beaker

 Micropipette

 Water-methanol mixture

 Gloves

5
Figure 3 Schematic Diagram of a fractional distillation column

6
Figure 4 Factional distillation setup

7
2.2 PROCEDURES

The experiment begins by charging the feed reservoir tank through the spring-loaded opening

C1 with 8 gallons of the mixture to be distilled. The boiler is then charged by connecting the

flex-tubing feed line to the boiler top through the quick disconnect coupling Q1 and then the

feed line was traced from the reservoir through the pump and feed rotameter, valves F1 was

opened by bypassing F3 and closing the drain valve D-1 and rotameter valves F2 and F4.

The main power was switched on and also the feed pump switch, the liquid level was

observed and has the liquid approached the ¾ full-mark, F3 was shut bypass and the valves of

F2 and F4 was opened to meter the remaining charge through the rotameter. The heating

cycle was then started and the thermocouple alongside the sample port tubing connections

was checked to ensure that they are properly sealed on each plate location.

The boiler was powered on and a flow of water was started in the condenser, the rotameter

was set to a lower value and it was adjusted as the boil-up proceeded till the top section of the

condenser near the vapor inlet line was warm to the touch. The proportional power control

switch for the boiler was set to the desired heating rate value to expedite the start-up. The

boiler temperature alongside the bimetallic thermometer, T13 was monitored constantly and

has the system started heating up. The distillate receiver valve, R2 was opened to allow the

venting back to the reservoir tank.

The temperature was observed as the distillate began to gather in their plates above the boiler.

For roughly 30 minutes, steady-state operation was obtained and has distillate was collected

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

was maintained.

Pressure Relief Valves (PRV) was set to approximately 1.0 psig. The liquid level in the boiler

was then periodically monitored.

8
If for any reason the liquid level were to drop below the electrical heating coils in the boiler,

a thermal overload switch, set to respond at 240 degrees Fahrenheit, would interrupt the line

power. This overload switch is in the 250-Watt auxiliary heater located on the right-hand side

of the boiler. The thermal overload switch is the red button located in the center of this

module.

This device is manually reset and cannot be reset until the boiler temperature drops below the

trigger value.

At the end of the experiment, the boiler’s power switch was turned off. When the condensate

no longer collects in the distillate receiver, the reflux pump was turned off and valve R1

closed. Valve R3 was then opened so that the system remains vented.

Then after, the main power control switch is turned off.

9
 CHAPTER THREE

RESULTS AND DISCUSSION

3.1 PARAMETERS

Entry Temperature = 80oC

Distillate Refractive Index = 0.566

Bottoms Refractive Index = 0.0032

Rotameter Reading for Feed = 87

Rotameter reading for reflux = 57

Table 3-0-1 Table showing calibration test data

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

10
 Refractive index
0.8
0.7 y = 0.7547x + 2E-06

0.6
Refractive Index

0.5
0.4
0.3
0.2
0.1
0
0 0.2 0.4 0.6 0.8 1
Liquid Mole Fraction

Figure 5Plot of Refractive index Vs Liquid mole fraction of methanol

11
Table 3-2 Fractional distillation experimental data

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

Time Temp. Temp. Temp. Temp. Temp. index of fraction of

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

54Kpa 48kPa 46kPa 40kPa 59kPa Plate 5 Plate 5

2 50 46 46 46 46 1.020347 1.352

4 52 48 52 52 52 0.735827 0.975

6 55 55 55 55 55 0.620359 0.822

8 60 59 60 60 60 0.459609 0.609

10 68 65 65 65 65 0.330556 0.438

12 69 72 72 72 72 0.187919 0.249

14 73 73 73 73 73 0.170561 0.226

16 76 76 76 - 75 0.138109 0.183

18 78 78 78 - 78 0.093582 0.124

20 79 79 78 - 79 0.079243 0.105

22 79 79 78 - 79 0.079243 0.105

24 80 80 79 - 80 0.065658 0.087

26 80 80 - - 81 0.052829 0.070

30 81 - - - 83 0.028678 0.038

12
Table 3-3 Table 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

Reflux Rotameter given by; (F = 2.04 R - 13.2) = 103.08 cm3/min

Feed Rotameter given by; (F = 1.99 R - 14.4) = 158.73 cm3/min
Rotameter Reading Feed = 87

Rotameter Reading Bottom = 57

For the feed, F = 158.73cm3/min

For the reflux, F = 103.08 cm3/min

xd = 0.749967, xb = 0.00424, xf = 0.500861

F=D+B

Fxf = Dxd + Bxb

Solving simultaneously,

D = 105.71 cm3/min

B = 53.02 cm3/min

Antoine equation is used to get the saturated pressures for the plates at different temperatures.
𝑃 𝐵
ln =𝐴−
𝑘𝑃𝑎 𝑡 (°C) + 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

13
 C = 339.50
For water,
A = 16.3872
B = 3885.70
C = 230.170

and
𝑃𝑡𝑜𝑡𝑎𝑙 − 𝑃 𝑤𝑎𝑡𝑒𝑟
𝑋𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 =
𝑃 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 − 𝑃 𝑤𝑎𝑡𝑒𝑟

𝑋𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 ∗ 𝑃 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙
𝑌𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 =
𝑃𝑡𝑜𝑡𝑎𝑙

y methanol V x methanol
1.000
0.900
0.800
0.700
y methanol

0.600
0.500
0.400
0.300
0.200
0.100
0.000
0.000 0.100 0.200 0.300 0.400 0.500 0.600 0.700 0.800 0.900 1.000
x methanol

y Methanol x Methanol

Figure 6 Graph of mole fraction Vs x Methanol

14
 Temperature V Mole Fractions
90
80
70
60
Temperature

50
40
30
20
10
0
0 0.2 0.4 0.6 0.8 1
y Meth, x Meth

Figure 7 Graph of Temperature Vs Mole Fraction

3.2 CALCULATIONS

1. Condenser heat duty = Mass flow rate (latent heat of condensation-latent heat of

vaporization)

= 103.08 cm3/min * 0.7913g/ cm3*(-1100) J/g =-87060J/min

= 89723.92J/min (1495.40W)

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

Temperature difference, J is Joules, W is watts

2. 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,

3. 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 vapors at

15
 boiling point= 0.632mol*35.21kJ/mol=22.25kJ = 22252J, q= 22252-3243.97/22252-

1550.48 = 0.918

4. The number of stages at total reflux = 5.3stages as shown in Figure 4 above which

corresponds to the actual number of stages on the equipment.

5. Overall column efficiency= Ratio of Theoretical to Actual number of stages= 5.3/6

=0.8833

6. 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= 0.88

For Plate 3= 0.998-0.984/1-0.984 = 0.88

For Plate 5= 0.984-0.956/1-0.956 = 0.64

16
 CHAPTER FOUR
CONCLUSION AND RECOMMENDATION

4.1 CONCLUSION

The effect of batch distillation is different on corresponding index of refraction of the

distillates. The index of refraction was studied using different distillates corresponding to

different trays.

However, this study would give a firsthand knowledge about the problem and thus provide a

good insight into the complexities and parameters governing this batch distillation

experiment. Working with the multi-staged batch distillation, all through this distillation the

feed was entering the right plate and a change in the flow pattern between the bottom of the

column and the reboiler will be beneficial but not practical as analysed from the experiment.

4.2 RECOMMENDATION

Wrap the distillation column with an insulator like aluminium foil. The insulation will

allow the vapours to travel all the way to the top of the column and out the condenser. The

increase in efficiency results from the repeated interaction with the column packing.

17
 REFERENCES

Geankoplis Christie John Transport Process and Seperation Process Principles [Book].

DrDal Nogare, Juvet, Gas-Liquid Chromatography, Interscience Publishers, 1962.

Diener, Gerster, Ind. Eng. Chern., Process Design and Development, July, 1968.

Drickamer, Bradford, Trans. Am. Inst. Chern. Eng., v. 39, p. 319, 1943.

Gerster, Mizushina, Marks, and Catanach, A.I.Ch.E. Journal, December, 1955

18
 APPENDIX

APPENDIX A

List of Group 4 Members

CHE/2016/002 ADEBISI GBENGA POSI

CHE/2016/017 AJONGBADE ESTHER OLUWASEUN

CHE/2016/023 ALADELO OYINDAMOLA ENIOLA

CHE/2016/034 DADA VICTOR OLUWASEUN

CHE/2016/039 ELUGBADEBO AYOMIDELE JOHN

CHE/2016/052 NDUBISI CHINEDU OLUSEGUN

CHE/2016/059 OGUNREWO KEHINDE ADURAGBEMI

CHE/2016/071 OMOLOYE STEPHEN TOLUWASE

CHE/2016/077 SALAMI YETUNDE ADEYEMI

CHE/2016/093 FUNSHO JESUDARASIMI AYOBANJO

CHE/2016/098 OKUNUGA OLUWATOMISIN QUADRI

19
APPENDIX B

Total balance

𝒇𝒆𝒆𝒅 = 𝒅𝒊𝒔𝒕𝒊𝒍𝒍𝒂𝒕𝒆 + 𝒃𝒐𝒕𝒕𝒐𝒎

Component balance

𝒇𝒆𝒆𝒅 × 𝒎𝒐𝒍. 𝒇𝒆𝒆𝒅

= (𝒅𝒊𝒔𝒕𝒊𝒍𝒍𝒂𝒕𝒆 × 𝒎𝒐𝒍. 𝒇𝒓𝒂𝒄 𝒅𝒊𝒔𝒕𝒊𝒍𝒍𝒂𝒕𝒆)

+ (𝒃𝒐𝒕𝒕𝒐𝒎 × 𝒎𝒐𝒍𝒆. 𝒇𝒓𝒂𝒄 𝒃𝒐𝒕𝒕𝒐𝒎)

Mole fraction of feed (xf) = feed refractive index / 0.7547

0.378
= 0.5008
0.7547

Mole fraction of distillate (xd) = Distillate refractive index / 0.7547

0.566
= 0.74996
0.7547

Mole fraction of bottom (xb) = bottoms refractive index / 0.7547

0.0032
= 0.00424
0.7547

20
APPENDIX C

𝑃𝑡𝑜𝑡𝑎𝑙 − 𝑃 𝑤𝑎𝑡𝑒𝑟
𝑋𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 =
𝑃 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 − 𝑃 𝑤𝑎𝑡𝑒𝑟

Sample calculation

Plate 5

P total = 59kpa

P sat. Water = 𝐴 − (from Antoine equation)

.
= 16.39 − = 10.15
.

.
P sat. methanol = 16.58 − = 46.29
.

59 − 10.15
𝑋𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 = = 1.352
46.29 − 10.15

𝑋𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 ∗ 𝑃 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙
𝑌𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 =
𝑃𝑡𝑜𝑡𝑎𝑙

1.352 ∗ 46.29
𝑌𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 = = 1.060
59

Repeat same procedures for different temperature

21