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
