A laboratory report on

Fractional Distillation Experiment

By

MARTINS, Olamide Oluwaseun

CHE/2017/048

Group 6

Submitted to:

Dr Sanda

Department of Chemical Engineering

Obafemi Awolowo University

Ile-Ife

In partial fulfillment of the requirement for

Chemical Engineering Unit Operations Laboratory I (CHE409)

February 2023
 Department of chemical engineering,

Obafemi Awolowo University,

Ile-Ife, Osun State.

February 21st, 2023.

The SIWES coordinator,

Dr Sanda,

Department of Chemical Engineering,

Faculty of Technology,

Obafemi Awolowo University,

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 23 rd May 2021. The report contains detailed

experimental work and result.

Yours Faithfully,

Martins Olamide

CHE/2017/048
 ABSTRACT

In this experiment, we collected samples making use of a syringe bottle in steady state, as

there was no temperature change or build-up, to determine the composition of methanol

vapor at various stages and time intervals. At several phases, sensors were analyzed to

measure the temperature. Distillate samples taken were only taken at the final step.

The actual number of stages and the calculated number of stages on the equipment are then

being compared. Then, the fractional distillation device was calibrated. These

results(obtained and experimental) are compared using a process simulation package as

HYSYS or CHEMCAD.
 TABLE OF CONTENTS
LETTER OF TRANSMITTAL.......................................................................................................

ABSTRACT...................................................................................................................................

LIST OF TABLES..........................................................................................................................

LIST OF FIGURES.......................................................................................................................

CHAPTER ONE..............................................................................................................................

INTRODUCTION...........................................................................................................................

1.0 Distillation.........................................................................................................................

1.1 Scope of the experiment....................................................................................................

1.2 Objective of the experiment..............................................................................................

1.3 Literature Review..............................................................................................................

CHAPTER TWO.............................................................................................................................

2.0 Experimental procedure........................................................................................................

2.1 Materials and Equipment..................................................................................................

CHAPTER THREE.........................................................................................................................

4.0 Result and Discussion...........................................................................................................

4.1 Parameters.........................................................................................................................

4.2 Calculations.....................................................................................................................

CHAPTER FOUR.........................................................................................................................

Conclusions....................................................................................................................................

CHAPTER FIVE...........................................................................................................................
Recommendation...........................................................................................................................

References......................................................................................................................................

Appendix........................................................................................................................................

Appendix A................................................................................................................................

Appendix B................................................................................................................................

Appendix C................................................................................................................................

Appendix D................................................................................................................................

Appendix E.................................................................................................................................

Appendix F.................................................................................................................................

List of Group 6 members........................................................................................................

 LIST OF TABLES
Table 1. Showing the calibration plot data......................................................................................

Table 2. Fractional distillation experimental data.........................................................................

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

Table 4. Showing the rotameter readings......................................................................................

Table 5. For Plate 1........................................................................................................................

Table 6. For Plate 2........................................................................................................................

Table 7. For plate 3........................................................................................................................

Table 8. For plate 4........................................................................................................................

Table 9. For plate 5........................................................................................................................

 CHAPTER ONE

INTRODUCTION

1.0 Distillation

Distillation is the process that occurs when a liquid sample is volatized to produce a vapor

that is subsequently condensed to a liquid richer in the more volatile components of the

original sample.

Distillation, as applied in gas-liquid operations, is a unit operation which involves separation

of a solution depending upon the distribution of the substances between gas and liquid phase.

It applies to cases where all components are present in both phases.

The separation of a mixture into its constituent components is known as fractional distillation.

Heating chemical compounds to a temperature where one or more fractions of the mixture

evaporate enable them to be separated. If the boiling points of the components are too close

together, a simple distillation is unlikely to achieve significant purification. The lower boiling

compound is always enriched in the distillate of a simple distillation.

Fractional distillation is used to filter reagents and products as well as refining. In oil

refineries, fractional distillation is used to separate a complex mixture into fractions with

similar boiling points and thus molecular weights and characteristics.

1.1 Scope of the experiment

The experiment focuses on the process of testing and calibrating a small-scale fractional

distillation column so it can be used to separate the mixture that emerge in

process development.
To achieve this goal, the binary methanol-water system was selected as the test system based

on the considerations that:

• 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 in

Textbooks.

1.2 Objective of the experiment

The objectives of the experiment conducted are:

• To determine the compositions of methanol vapor at different times.

• To obtain concentrations of the system at steady state, condenser heat duty, enthalpies

of the feed distillate and bottoms as well as the feed quality.

• To determine the overall column efficiency and the Murphree efficiency of each plate.

• To compare experimental result with those that would be obtained using a process

simulation package.

• To construct the equilibrium curve for methanol-water binary system at atmospheric

pressure.

1.3 Literature Review

Methanol is a commonly used solvent, and its mixtures with water are usually observed,

being necessary to separate these volatile solvents for future applications. Distillation is one

of the major importance separation processes in chemical engineering in which the separation

is reached because of the volatility difference of the components.

In the extractive distillation is required a third component, an entrainer, which modifies the

relative volatility of the mixture components. The entrainer selection is an important step

because the separation effectiveness depends on the interactions between this component and

the azeotropic mixture.

Methanol-acetone mixture is usually observed with water as entrainer. The acetone-methanol

system has a minimum boiling point azeotrope, and the extractive distillation is a possible

method to separate this azeotropic mixture. Many works have studied the vapor-liquid

equilibrium of this system and suggest water as an entrainer.

 CHAPTER TWO

2.0 EXPERIMENTAL PROCEDURE

2.1 Materials and Equipment

The materials and equipment used for the experiment are given below

• Fractional distillation unit equipped with a condenser

• Refractometer

• Dropper

• Sample collector

• Funnel

• Beaker

• Micropipette
 • Water-methanol mixture

• Gloves

Figure 1. Schematic diagram of the fractional distillation unit.

Figure 2. Fractional distillation unit
The procedures carried out in this experiment can be classified into 2, the Start-up procedure and

The feed (8 gallons of the mixture) was poured into reservoir tank through the spring-loaded

opening C1 to be distilled. The boiler top was connected to the flex-tubing feed line through the

quick-disconnect coupling Q1, for charging. 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 was switched on, followed by the feed pump switch and noted from the pilot

lights. The liquid level was observed as it rises in the boiler sight glass. As the liquid approached the

3/4-full mark, the bypass F3 was shut and valves F2 and F4 was opened to meter the remaining charge

through the rotameter. The heating cycle was initiated.

The boiler power switch was turned on; a pilot light indicated the heat input. Water was

allowed through the condenser, setting the rotameter at a low value. As the boil-up proceeds, the

rotameter was adjusted until the top section of the condenser near the vapor 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 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, the distillate line valve R1 leading to the suction side of the reflux pump were closed, and the

recycle pump should be off.

The temperature was Observed as the distillate was collected in plates above the boiler.

Steady-state operation should be attained.

 CHAPTER THREE

RESULT AND DISCUSSION

3.1 Parameters

Feed conditions: Refractive index = 0.378

Temperature on entry = 80°C

Distillate Refractive Index = 0.566

Bottoms Refractive Index = 0.0032

Rotameter Reading for Feed = 99

Rotameter reading for reflux = 66

Table 1: Calibration plot 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
 Refractive index against liquid mole fraction of methanol
0.8

0.7

0.6
Refractive index of methanol

0.5

0.4

0.3

0.2

0.1

0
0 0.2 0.4 0.6 0.8 1 1.2

Liquid mole fraction of methanol

Figure 3. Plot of refractive index against liquid mole fraction of methanol.

0.30188−0.22641
The slope of the graph above = =0.7547.
0.4−0.2

The y-intercept of the graph is 0.

Therefore the equation of the linear graph is y=0.7547 x. This equation is used to determine the

liquid mole fraction of methanol at different refractive indices and to calculate the liquid mole fraction

of methanol for the distillate refractive index and the bottom refractive index.
Table 2. Fractional distillation experimental data.

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

(min) 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 58kPa Plate 5 Plate 5

2 50 46 46 46 51.5 0.73958 0.980

4 52 48 52 52 52 0.71920 0.953

6 55 55 55 55 57 0.53884 0.714

8 60 59 60 60 68 0.25583 0.339

10 68 65 65 65 69.5 0.22640 0.300

12 69 72 72 72 72 0.18037 0.239

14 73 73 73 73 73 0.16376 0.217

16 76 76 76 - 77 0.10113 0.134

18 78 78 78 - 78 0.08679 0.115

20 79 79 78 - 79 0.07320 0.097

22 79 79 78 - 79 0.07320 0.097

24 80 80 79 - 82 0.03547 0.047

26 80 80 - - 84 0.01207 0.016

30 81 - - - 84.5 0.00604 0.008

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

Refractive index Liquid mole fraction

Distillate 0.5660 0.750

Bottoms 0.0032 0.00424

Calibration of the Rotameter is given by:

F= 1.99R-14.4 for feed

F= 2.04R-13.2 for reflux

Table 4. Showing the rotameter readings.

Rotameter reading

Feed 99

Reflux 66

Substituting the rotameter reading of the feed and reflux into the calibration equations for feed and

reflux respectively gives;

Feed (F) = 1.99(99) – 14.4 = 182.61 cm3/min

Reflux = 2.04(66) – 13.2 = 121.44 cm3/min

Also, by substituting the values of the refractive of the feed, distillate and bottoms into the equation of

the graph of refractive index vs liquid mole fraction, x F =0.501 , x D =0.750 , x B=0.00424 .

Substituting the values of F, x F , x D , x B into equations (1) and (2) stated in the theoretical background

(F = D + B and F x F =D x D + B x B ) and solving them simultaneously,

To get the flow rate of the distillate and bottoms (D and B respectively), the values of F, x F , x D , x B are

substituted into equations (1) and (2) stated in the theoretical background (F = D + B and

F x F =D x D + B x B) and the resulting equations are solved simultaneously.

 D = 121.64 cm3/min

B = 60.97 cm3/min

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

sat
P B
log =A−
mmHg t ° C )+C
(

( ) × 1.01325
B 2
sat
A−
t ( ° C ) +C × 10 kPa
P (kPa)= e
760 mmHg

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

For methanol,

A = 8.0724

B = 1547.99

C = 238.87

For water,

A = 8.07131

B = 1730.63

C = 233.426

sat
Ptotal−P water
Xmethanol= sat sat
P methanol−P water

sat
Xmethanol × P methanol
Ymethanol=
Ptotal

Temperature ( sat sat Liquid mole Vapor mole

P methanol P water
°C¿ fraction of fraction of
 (kPa) (kPa) methanol (x- methanol (y-

methanol) methanol)

51.5 59.32 13.29 0.971 0.993

52 60.61 13.62 0.945 0.987

57 74.83 17.32 0.707 0.912

68 116.11 28.57 0.336 0.673

69.5 122.98 30.5 0.297 0.63

72 135.18 33.96 0.238 0.555

73 140.33 35.44 0.215 0.52

77 162.59 41.9 0.133 0.373

78 168.59 43.67 0.115 0.334

79 174.77 45.49 0.097 0.292

79 174.77 45.49 0.097 0.292

82 194.45 51.36 0.046 0.154

84 208.55 55.61 0.016 0.058

84.5 212.2 56.72 0.008 0.029

 90
Temperature vs mole fraction

80

70

60
Temperature

50

40

30

20

10

0
0 0.2 0.4 0.6 0.8 1 1.2

y-methanol, x-methanol
y-methanol x-methanol

Figure 4: Boiling point diagram of methanol for plate 5 of the distillation column

3.2 Calculations

i) Condenser heat duty:

QC = ṁ× γ Where ṁ = mass flow rate = Volumetric flow rate × density=V̇ × ρ

γ is the latent heat of condensation

V̇ =121.44 cm /min, ρ=¿0.7913g/ cm3, γ =1165 J /g

3

3 3
QC =121.44 cm /min× 0.7913 g/cm ×1165 J / g

QC =111951 J /min ¿ 1865.9Watts

ii) Enthalpies of feed (hf):

h f =mC p T =mole × molar mass ×C P T

Where T is the feed temperature and Cp is the specific heat capacity of methanol

h f =0.501mol × 32 g /mol ×2.53 J / g ℃ ×80 ℃=3244.9 J

Enthalpy of distillate (hd):

h d=m C p T =mole × molar mass ×C P T

Where T is the distillate temperature and Cp is the specific heat capacity of methanol

h d=0.750 mol × 32 g /mol ×2.53 J / g ℃ ×58 ℃=3521.76 J

Enthalpy of bottoms (hb):

h b=mC p T =mole × molar mass × C P T

Where T is the bottoms temperature and Cp is the specific heat capacity of methanol

h d=0.00424 mol ×32 g/mol × 2.53 J /g ℃ × 80℃=17.85 J

Feed Quality:

iii) At total reflux, the operating lines of stripping and rectifying section coincide with

the 45℃ line. The resulting equilibrium curve is given below;

 Plot of y-methanol vs x-methanol
1.2

0.8
y-methanol

0.6 Equilibrium curve

Operating line

0.4

0.2

0
0 0.2 0.4 0.6 0.8 1 1.2

x-methanol

From the graph above, the theoretical number of stages is approximately 5.5 because the last line

touching the equilibrium curve is short.

iv) Overall column efficiency:

Actual number of stages on the equipment = 6

Theoretical number of stages = 5.5

Theoretical number of stages 5.5

Overall column efficiency = = =0.917
Actual number of stages 6

Murphree plate efficiency is the ratio of the increase in mole fraction of vapor of a volatile

component passing through a plate in a column to the same increase when the vapor is in

equilibrium. The vapor mole fractions passing through each plate is not given. Therefore the

Murphree efficiency for each plate cannot be calculated.

 CHAPTER FOUR

4.0 CONCLUSIONS
The fractional distillation was efficient as it had an overall efficiency of 0.833. The simulation of the

experiment was identical with to the one we performed.

We were able to determine the compositions of methanol vapor at different times, obtain

concentrations of the system at steady state, condenser heat duty, enthalpies of the feed distillate and

bottoms as well as the feed quality, determine the overall column efficiency and the Murphree
efficiency of each plate, compare experimental result with those that would be obtained using a

process simulation package and finally construct the equilibrium curve for methanol-water binary

system at atmospheric pressure. Thereby concluding the objective of the experiment.

 CHAPTER FIVE

5.0 RECOMMENDATION
I recommend that the experiment is being performed with active group members who would actively

and wholeheartedly record the readings from the distillation unit and the refractometer.

Fractional distillation is more efficient than other types of distillation. Fractional distillation

completes several simple distillations in one apparatus.

 REFERENCES
Batista, E., & Meirelles, A. (1997). Simulation and thermal integration SRV in extractive
distillation column. J. Chem. Eng. Jpn 3(1), 45-51.
Griswold, J., & Buford, C. B. (1949). Separation of synthesis mixtures vapor-liquid equilibria
of acetone methanol water. Industrial and Engineering Chemistry 41(10), 2347-2351.
Iglesias, M., Orge, B., & Marino, G. (1999). Vapor-liquid equilibria for the tenary system
acetone + methanol + water. Chem. Eng. Data 44, 661-665.
Kotai, B., Lang, P., & Modla, G. (2007). Batch extractive distilation as a hybrid process.
Separation of minimum boiling azeotropes. Chem. Eng. Sci. 62, 6816-6826.
Vercher, E., Orchilles, A. V., & Miguel, P. J. (2006). Isobaric vapor-liquid equilibria for
acetone-methanol. Fluid Phase Equilib 250, 131-137.
 APPENDIX
Appendix A
Table 5. For Plate 1

Time(mins Temp Psat Psat x y x y

) methanol water methano methano water water

l l

2 50 55.21 12.41 0.972 0.994 0.028 0.006

4 52 60.18 13.69 0.867 0.966 0.133 0.034

6 55 68.34 15.82 0.727 0.920 0.273 0.080

8 60 83.99 20.01 0.531 0.826 0.469 0.174

10 68 115.21 28.66 0.293 0.625 0.707 0.375

12 69 119.71 29.93 0.268 0.594 0.732 0.406

14 73 139.22 35.53 0.178 0.459 0.822 0.541

16 76 155.51 40.28 0.119 0.343 0.881 0.657

18 78 167.23 43.74 0.083 0.257 0.917 0.743

20 79 173.36 45.56 0.066 0.212 0.934 0.788

22 79 173.36 45.56 0.066 0.212 0.934 0.788

24 80 179.67 47.44 0.050 0.165 0.950 0.835

26 80 179.67 47.44 0.050 0.165 0.950 0.835

30 81 186.17 49.39 0.034 0.116 0.966 0.884

Appendix B
Table 6. For Plate 2

Time(mins) Temp Psat methanol Psat water x methanol y x y

methanol water water

2 46 46.29 10.15 1.047 1.010 0.047 0.010

4 48 50.58 11.23 0.934 0.985 0.066 0.015

6 55 68.34 15.82 0.613 0.872 0.387 0.128

8 59 80.64 19.10 0.470 0.789 0.530 0.211

10 65 102.53 25.10 0.296 0.632 0.704 0.368

12 72 134.11 34.05 0.139 0.389 0.861 0.611

14 73 139.22 35.53 0.120 0.349 0.880 0.651

16 76 155.51 40.28 0.067 0.217 0.933 0.783

18 78 167.23 43.74 0.035 0.120 0.965 0.880

20 79 173.36 45.56 0.019 0.069 0.981 0.931

22 79 173.36 45.56 0.019 0.069 0.981 0.931

24 80 179.67 47.44 0.004 0.016 0.996 0.984

26 80 179.67 47.44 0.004 0.016 0.996 0.984

Appendix C
Table 7. For plate 3

Time (mins) Temp Psat Psat water x methanol y methanol x water y

methanol water

2 46 46.29 10.15 0.992 0.998 0.008 0.002

4 52 60.18 13.69 0.695 0.909 0.305 0.091

6 55 68.34 15.82 0.575 0.854 0.425 0.146

8 60 83.99 20.01 0.406 0.742 0.594 0.258

10 65 102.53 25.10 0.270 0.602 0.730 0.398

12 72 134.11 34.05 0.119 0.348 0.881 0.652

14 73 139.22 35.53 0.101 0.306 0.899 0.694

16 76 155.51 40.28 0.050 0.168 0.950 0.832

18 78 167.23 43.74 0.018 0.067 0.982 0.933

20 78 167.23 43.74 0.018 0.067 0.982 0.933

22 78 167.23 43.74 0.018 0.067 0.982 0.933

24 79 173.36 45.56 0.003 0.013 0.997 0.987

Appendix D
Table 8. For plate 4

Time(mins) Temp Psat methanol Psat water x methanol y methanol x y

water water

2 46 46.29 10.15 0.826 0.956 0.174 0.044

4 52 60.18 13.69 0.566 0.851 0.434 0.149

6 55 68.34 15.82 0.460 0.787 0.540 0.213

8 60 83.99 20.01 0.312 0.656 0.688 0.344

10 65 102.53 25.10 0.192 0.493 0.808 0.507

12 72 134.11 34.05 0.059 0.199 0.941 0.801

14 73 139.22 35.53 0.043 0.150 0.957 0.850

Appendix E
Table 9. For plate 5

Time(mins) Temp Psat methanol Psat water x methanol y methanol x y

water water
2 46 46.29 10.15 1.296 1.053 0.296 0.053
4 52 60.18 13.69 0.932 0.984 0.068 0.016
6 55 68.34 15.82 0.784 0.940 0.216 0.060
8 60 83.99 20.01 0.578 0.852 0.422 0.148
10 65 102.53 25.10 0.412 0.741 0.588 0.259
12 72 134.11 34.05 0.229 0.540 0.771 0.460
14 73 139.22 35.53 0.207 0.506 0.793 0.494
16 75 149.92 38.64 0.165 0.434 0.835 0.566
18 78 167.23 43.74 0.107 0.315 0.893 0.685
20 79 173.36 45.56 0.090 0.272 0.910 0.728
22 79 173.36 45.56 0.090 0.272 0.910 0.728
24 80 179.67 47.44 0.072 0.228 0.928 0.772
26 81 186.17 49.39 0.056 0.182 0.944 0.818
30 83 199.75 53.49 0.024 0.084 0.976 0.916
Appendix F

List of Group 6 members

CHE/2017/009 ADEKOLEOYE OYINDAMOLA ANTHONY

CHE/2017/018 AFOLABI ELIZABETH AJOKE
CHE/2017/027 AKOFIRANMI BABALOLA EMMANUEL
CHE/2017/037 EKUOBASE ESOSA JOSEPH
CHE/2017/048 MARTINS OLAMIDE OLUWASEUN
CHE/2017/057 ODUNLAMI EMMANUEL AYODEJI
CHE/2017/065 OLADIPO IFEOLUWA ANNE
CHE/2017/082 OYEMADE EMMANUEL AFOLABI
CHE/2017/099 OLAPADE OPEYEMI RUKAYAT