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CDB 3052 Chemical Engineering

Laboratory II Jan 2016


Experiment 4 Batch Packed Distillation
Unit
Lab Instructor : Sahal Irfan
Group Members
No

1.0 OBJECTIVES

:
Name

ID

Maryam binti Nasaruddin

19076

Sugentther A/L Chantravarnam

19054

Nur Kamarul Syaabah Ng binti Mohamad Hafiz

19155

Abdul Aiman bin Abdul Latif

19310

Wan Intan Nadiah binti Borharuddin

18857

The experiment of batch packed distillation unit was divided into


two experiments. In the first experiment, the objectives were to determine
the height equivalent theoretical plates (HETP) at total reflux and the
effect of liquid and vapor loading on the HETP at total reflux.
Meanwhile, the second experiment objective was to conduct the
batch distillation at constant reflux. We need to examine the change in top
and bottom composition, and the height equivalent theoretical plated
(HETP) over time in a batch distillation. Beside, mass balance calculations
on the distillation unit have to carry out.
Before the experiment is being conducted it is necessary to
differentiate what type of category the batch distillation column is in.
There are vital information for each of us to know, which is to differentiate
between a unit operation and unit process. The packed bed distillation is
categorized under unit operation as it has mechanical process which
results in the physical change that is visible to us.
2.0 THEORY
Batch distillation, is very important equipment used in many
industries. It is very efficient and easy to use equipment. It allows the
fractionation of multicomponent mixture into its pure constituents in a
single column. Due to its numerous advantages such as low capital cost,
easy approach method and so forth the batch distillation is used as a
source of separation. At the same time the batch distillation consume too
much of energy and also could degrade the feed substances due to high
temperature which results the materials to decompose.
In order to increase the performance the batch packed distillation
(BPD) unit is developed. It is used to separate mixtures at the atmospheric
pressure in a batch column. This batch packed is mainly designed to
expose the students on the behavior of the BPD and for research
purposes. Compare to batch distillation there are some different in the
unit operation. For example, we can obtain the top and bottom product to
determine the refracting index and also for mass balance calculations. We
also could determine the flow rate by manual calculations.

3.0 EXPERIMENT DESIGN


3.1 EXPERIMENT 1: Batch Distillation at Total Reflux
1. Firstly, we recorded the top (distillate) and bottom temperatures.
2. Then we collected the samples from the distillate and the bottom
product.
3. We measured the refractive index for both of the samples and
determined their compositions.
4. For the other vapor and liquid loading, we adjusted the heater
power settings in W1 and W2. By doing that it will decrease the
heating duty and the vapor flow in the column. It will also cause the
liquid flow to decrease.
5. We changed the heater power settings and waited approximately 15
minutes for the distillation unit to reach a stable condition. After
waiting, we repeated step 1 to 4 for the next heater power settings
for 80%, 60%, 40% and 20%.

3.2 EXPERIMENT 2: Batch Distillation at Constant Reflux


1. Firstly, we set the power settings to 70%.
2. We waited approximately for 15 minutes for the distillation unit to
reach stable condition. Then we recorded the top and bottom
temperature.
3. We have collected the samples from the distillate and the bottom
product. For all the samples collected, we compiled all of the
distillate and bottom samples into separate containers for later use
in mass balance calculations.
4. Then we measured the refractive index for both of the samples and
determined their compositions. This will constitute the composition
at the beginning of the experiment.
5. We set the reflux divider to give a ratio of 1 and allowed the process
to run for about 10 minutes.
6. After waiting, we collected the samples from the distillate and
bottom product. We measured the refractive index for both of the
samples and determined their compositions.
7. We measured the distillate flow rate by:
I. Closing valve V4 and started the time immediately
II.
Collected the distillate in the measuring vessel B3 and
stopped the timer once it reached a certain volume.

Mole fraction
ethanol
0
0.03
0.07
0.12
0.17
0.24
0.32
0.42
0.55
0.64
0.74
0.85
1
4.0 RESULTS

Mole fraction of
water
1
0.97
0.93
0.88
0.83
0.76
0.68
0.58
0.45
0.36
0.26
0.15
0

Refractive
index
1.33299
1.34119
1.34302
1.34947
1.35488
1.35838
1.36125
1.36295
1.36364
1.36358
1.36359
1.36154
1.35978

Table A: Table for Preparation of Refractive Index vs


Composition Plot

Graph of Refractive Index vs Mole Fraction of Ethanol

Figure A shows the graph of refractive index vs mole fraction of


ethanol

EXPERIMENT 1: Batch Distillation At Total Reflux


Heater
W1,
W2
power
100%
80%
60%
40%
20%

Bottom

Distillate
Number
Mole
of
Refract.
Mole
Refract.
fractio
stages
Index
fraction
Index
n
1.35471
0.18
1.36151
0.3
1
1.35545
0.22
1.35797
0.26
1
1.35772
0.26
1.36196
0.34
1
1.3551
0.2
1.36203
0.35
1
1.35489
0.18
1.36196
0.3
1
Table 1: Results of HETP values for different heater power.

HETP
(mm)
1120
1120
1120
1120
1120

100 % He ate r Powe r Equilibrium Diagram for Ethanol Wate r Syste m at 1 atm

01

Xb

Xd

Figure 1.1 shows 100 % Heater Power Equilibrium Diagram for Ethanol
Water System at 1 atm

80 % Heater Power Equilibrium Diagram for Ethanol Water System at 1 atm

01

Xb

Xd

Figure 1.2 shows 80 % Heater Power Equilibrium Diagram for Ethanol


Water System at 1 atm
60 % Heater Power Equilibrium Diagram for Ethanol Water System at 1 atm

01

Xb

Xd

Figure 1.3 shows 60 % Heater Power Equilibrium Diagram for Ethanol


Water System at 1 atm

40 % Heater Power Equilibrium Diagram for Ethanol Water System at 1 atm

01

Xb

Xd

Figure 1.4 shows 40 % Heater Power Equilibrium Diagram for Ethanol


Water System at 1 atm
20 % Heater Power Equilibrium Diagram for Ethanol Water System at 1 atm

01

Xb

Xd

Figure 1.5 shows 20 % Heater Power Equilibrium Diagram for Ethanol


Water System at 1 atm

Graph of HETP vs He ate r Powe r

Figure 1.6 shows the relationship between HETP and Heater Power

EXPERIMENT 2.1: Batch Distillation At Constant Reflux


Table 2.1: Results of HETP values at different time.

Distillate

Time
(min)
Refract.
Index

Mole
fraction

Bottom product
Flow
rate(mL/
min)

Refract.
Index

Numb HET
er of
P
stage (m
s
m)

Mole
fractio
n
1

1.36194

0.37

71.4286

1.35607

0.26
1

10

1.36182

0.35

30

1.36212

0.3

20

1.36172

0.33

12.5

1.36106

0.28

30

1.35975

0.31

0.1799

1.36161

025

40

1.35993

0.28

0.1798

1.35984

0.26

50

1.36119

0.32

0.1792

1.35999

0.28

1
1
1
1
1
60

1.36231

0.36

0.1678

1.36141

0.32

112
0
112
0
112
0
112
0
112
0
112
0
112
0

0 min Equilibrium Diagram for Ethanol-Water System at 1 atm

01

xd

Xb

Figure 2.1 shows 0 min Equilibrium Diagram for Ethanol-Water System at


1 atm

10 min Equilibrium Diagram for Ethanol-Water System at 1 atm

01

xd

Xb

Figure 2.2 shows 10 min Equilibrium Diagram for Ethanol-Water System at


1 atm
20 min Equilibrium Diagram for Ethanol-Water System at 1 atm

01

xd

Xb

Figure 2.3 shows 20 min Equilibrium Diagram for Ethanol-Water System at


1 atm

30 min Equilibrium Diagram for Ethanol-Water System at 1 atm

01

xd

Xb

Figure 2.4 shows 30 min Equilibrium Diagram for Ethanol-Water System at


1 atm
40 min Equilibrium Diagram for Ethanol-Water System at 1 atm

01

Xd

Xb

Figure 2.5 shows 40 min Equilibrium Diagram for Ethanol-Water System at


1 atm

50 min Equilibrium Diagram for Ethanol-Water System at 1 atm

01

Xd

Xb

Figure 2.6 shows 50 min Equilibrium Diagram for Ethanol-Water System at


1 atm
50 min Equilibrium Diagram for Ethanol-Water System at 1 atm

01

Xd

Xb

Figure 2.7 shows 60 min Equilibrium Diagram for Ethanol-Water System at


1 atm

EXPERIMENT 2.2: Amount of Ethanol


Table 2.2 : Results of Amount of Ethanol
Time
(min)

Distillate composition,
y

Bottom composition, x

0.37

0.26

10

0.35

0.27

20

0.33

0.29

30

0.33

0.3

40

0.34

0.31

50

0.35

0.31

60

0.36

0.32

1
y x
9.090
9
12.50
00
25.00
00
33.33
33
33.33
33
25.00
00
25.00
00

Graph of 1/ Xd - Xb vs Xb

Figure 2.8 shows the graph of 1/xd-xb vs Bottom Ethanol (Xb)

EXPERIMENT 2.3: Amount of Ethanol based on Mass Balance Calculations


Condition
Initial
Final

Reboiler
volume (L)
15.0
13.65

Reboiler
composition
0.26
0.32

Distillate
volume (L)
1.35

Distillate
composition
0.36

Based on the mass balance, the calculated initial bottom composition of


ethanol is 0.1814. Meanwhile, the experimental value obtained is 0.2226
which gives the percentage error of 43.33%. The sample calculations to
find the theoretical amount of ethanol are shown in the appendix.

5.1

DISCUSSION

Based on the appendix A, the refractive index for 13 samples of


ethanol water mixture with different volumes of water and ethanol is
measured. The refractive index is measured by using a refractometer,
which is an analytic instrument that proposed originally by Snells law. Its
a formula used to study the relationship between the angle of incident and
refraction when a specific light passing through a boundary of the
medium. The values of refractive index then are used to produce a
calibration graph of refractive index versus mole fraction of ethanol and
the best linear graph is determined. As a result, the calibration graph
enables us to determine the mole fraction of ethanol at the entire distillate
and bottom product.
Next for Appendix B, we know that the effective column height is
1120m and constant throughout our experiment. From that, we will be
able to calculate the height equivalent theoretical plates (HETP) value by
dividing the effective column height with the number of theoretical plates.
The value for theoretical plates can be referred from the X-Y Equilibrium
Diagram for Ethanol-Water System at 1 atm graphs at the appendices. For
the result, we know that even though the heater power is kept increasing,
the HETP just kept constant. Refer to the graph of HETP vs Heating Power.
Lastly for Appendix C, the system was set at constant reflux. Our
experimental value finds that the numbers of theoretical stages are
increasing and then fall down again. This also happen to the HETP value
as we as we kept increase the time of boiling. This is because there are
some errors in determining the Refractive Index values for the bottom and
top distillate. Due to high temperature in the boiler, the samples should be
cool down for 10 min, because the temperatures can affect the RI
values. We also observe that the concentrations of ethanol in the reboiler
over time are decreasing.
Safety Precautions
1. Wear a safety glove when taking the samples out of the valves to
avoid scalding.The distillate and the bottom product can be hot as it
is heated at 80 degree celcius.

2. It is advised be careful when handling ethanol as its highly


flammable.
Error and Modifications
Throughout the experiment, some possible error can be identified and we
come out with several modifications to make improvement.
Possible errors:
1. Measurement of refractive index : The refractive index of the
samples is mostly measured while it is not completely cool down .
2. Parallax error : The position of eye is not directly perpendicular to
the scale of measuring cylinder
3. Fluctuation of temperature reading : The temperature reading is
hardly reached stable. It is difficult to collect the reading .
Modifications:
1. The refractive index must be measured when the samples are
completely cooled down.
2. The position of eye should be directly perpendicular to the scale of
measuring cylinder
3. Record several temperature and calculate the average temperature
For the purpose of calibration, the refractive index of 13 samples of
ethanol-water mixture with different volumes of water and ethanol is
measured to produce a refractive index versus mole fraction of ethanol
graph. This can be made possible by using refractometer, an analytical
instrument that is governed by Snells Law, a formula used to describe the
relationship between the angles of incidence and refraction, when
referring to light or other waves passing through a boundary between two
different isotropic media, such as water and glass. Having done that, the
values of refractive index are tabulated along with its respective ethanolwater compositions of volume. Next, a graph of refractive index versus the
composition of ethanol, Xethanol is constructed and the best linear graph is
determined. As a result, an equation of y = 0.026x + 1.3343 is obtained
which then, enables the determination of the mole fraction of ethanol in
the entire distillate and bottom product, x from any arbitrary value of
refractive index, y.
6.0 CONCLUSION
All in all, the objectives of the experiment are not fulfilled due to the
discrepancies observed between the result of the experiment and the
established theory. The conclusions that can be drawn from these
experiments are as follow.

In total reflux condition, the Height Equivalent Theoretical Plates (HETP) at


total reflux can be determined by stepping off the theoretical stages from
the mole fraction of distillate, XD until the mole fraction of bottom, XB to
the 45o line. The effect of liquid and vapor loading on the HETP a total
reflux condition is also examined. Since the effective column height is a
constant, the HETP value is inversely proportional to the number of
theoretical stages. Hence, the greater the power of the heater, the greater
the HETP value.
In constant reflux condition, the change in the overhead and bottom
composition, and HETP over time in a batch distillation unit is determined.
Theoretically, the mole fraction of ethanol in both the distillate and bottom
product decreases over time. As time elapse, the mole fraction of ethanol
in the evaporator decreases, the number of theoretical stages decreases,
HETP increases. At constant reflux, the amount of moles left in the
evaporator at any time can be determined by using the Rayleigh equation.
The mass balance calculation on the distillation unit has also been
performed.

7.0 APPENDIX
Table A.1: Sample Table for Refractive Index vs Composition Plot
Volume
of
ethanol
(mL)
0
1
2
3
4
5
6
7
8
8.5
9
9.5
10

Volume
of water
(mL)

Mole fraction
ethanol

Mole
fraction of
water

Refractiv
e index

10
9
8
7
6
5
4
3
2
1.5
1
0.5
0

0
0.03
0.07
0.12
0.17
0.24
0.32
0.42
0.55
0.64
0.74
0.85
1

1
0.97
0.93
0.88
0.83
0.76
0.68
0.58
0.45
0.36
0.26
0.15
0

1.33299
1.34119
1.34302
1.34947
1.35488
1.35838
1.36125
1.36295
1.36364
1.36358
1.36359
1.36154
1.35978

Table A.2 : Raw data For Experiment 1


Time

Distillate

Bottom product

(min)
0
10
20
30
40
50
60

Tem
p
74.6
76.4
75.8
75.5
75.6
75.6
75.6

Refract.
Index
1.36194
1.36182
1.36172
1.36161
1.35984
1.36119
1.36141

Mole
fraction
0.37
0.35
0.33
0.31
0.29
0.3
0.3

Flow
rate(mL/min)
71.4286
30
12.5
0.1799
0.1798
0.1792
0.1678

Tem
p
80
80.1
80.1
80.2
80.2
80.3
80.3

Refract.
Index
1.35607
1.36212
1.36106
1.35975
1.35993
1.35999
1.36231

Mole
fraction
0.26
0.3
0.28
0.25
0.26
0.26
0.28

Table A.3: Raw Data for Experiment 2


Time
(min)
0
10
20
30
40
50
60

Tem
p
74.6
76.4
75.8
75.5
75.6
75.6
75.6

Refract.
Index
1.36194
1.36182
1.36172
1.36161
1.35984
1.36119
1.36141

Distillate
Mole
fraction
0.37
0.35
0.33
0.31
0.29
0.3
0.3

Flow
rate(mL/min)
71.4286
30
12.5
0.1799
0.1798
0.1792
0.1678

Tem
p
80
80.1
80.1
80.2
80.2
80.3
80.3

Sample Calculations
1.1 Molar Volume
Ethanol
Specific gravity = 0.789
Molecular weight = 46.07 g/mol

Molar volume=

Molecular weight
Specific gravity of component i density of water

Molar Volume ( Ethanol )=

g
1
1L
(
(
=0.05839 L /mol
( 46.07
)
)
1 mol
0.789
1000 g )

Water

g
1L
(
=0.01802/mol
( 18.02
)
1 mol
1000 g )

Molar Volume ( Water )=

Bottom product
Refract.
Mole
Index
fraction
1.35607
0.26
1.36212
0.3
1.36106
0.28
1.35975
0.25
1.35993
0.26
1.35999
0.26
1.36231
0.28

1.2 Mole Fraction

Mole fraction of Ethanol=

Mole fraction of Water =

Moles of ethanol
Moles of Ethanol+ Moles of Water

Moles of water
Moles of Ethanol+ Moles of Water

Or Mole fraction of water = (1- Mole Fraction of Ethanol)

Volume of ethanol = 1 mL = 0.001 L


Volume of water = 9 mL = 0.009 L

Mole of component i=

Mole of ethanol=

Mole of water =

Volume of component ithe mixture


Molar volume of component i

0.001 L
=0.0171mol
0.05839 L/mol

0.009 L
=0.4994 mol
0.01802 L/mol

Mole fraction of Ethanol=

0.0171
=0.33
0.0171+ 0.04994

Mole fraction of Water =10.33=0.7

1.3 Mole Fraction of Ethanol using Linear Equation


From the graph of Figure A with refractive index as the y-axis and mole fraction
of ethanol as the x-axis is plotted using Excel. The calculation for mole fraction of
ethanol for batch distillation at total reflux can be done by tracing the value of
mole fraction with the references of refractive index that has been given.

1.4 Calculation of HETP


HETP can be easily found with the following equation

HETP=

Height of column
Number of stages

The height of the column used for batch distillation in this experiment is 1120
mm. To get the number of stages, we apply McCabe Thiele method by assuming
constant molar flow rate. An x-y equilibrium curve of water-ethanol mixture and
the line with the equation of y=x are plotted. Then, draw a vertical line straight
up crossing the x-y equilibrium curve, starting from the top and bottom
composition. Finally, determine the number stages required.

1.5 Mass Balance Calculations


Initial conditions
Reboiler volume = 15.0L
Reboiler composition = 0.26 (Xb taken at t = 0)
Final conditions
Reboiler volume = 13.33 L
Reboiler composition = 0.28 (Xb taken at t = 60 min)
Bottom product volume taken for IR determination = 200 mL
Distillate volume = 1.5 L
Distillate composition = 0.3 (Xd taken at t = 60 min)
Final reboiler volume = [Initial reboiler volume - Final distillate volume - Volume
taken for RI determination)
Assume that the volume taken for IR determination is small enough as compared
to others.
Final reboiler volume = 15.0 1.5 0.2 = 13.33 L

1.6 Area under the Graph

The area under the graph is calculated using the formula of finding the area of a
trapezoid.

Graph of 1/ Xd - Xb vs Xb

To calculate area under the graph:

[(

1
1
1
A= ( X bn X bn1)
n+
n1
2
xdxb
xdxb

) (

Time

Top
Composition,
Xd

Bottom
Composition,
xb

1/xd-xb

Area Under Graph


between xn-1 and xn

0.37

0.26

9.0909

0.108

10

0.35

0.27

12.5000

0.375

20

0.33

0.29

25.0000

0.292

30

0.33

0.3

33.3333

0.833

40

0.34

0.31

33.3333

0.5

50

0.35

0.31

25.0000

2.5

60

0.36

0.32

25.0000

Total

4.608

1.7 Calculation of Ethanol Left in the Reboiler


Rayleigh equation is used to find the amount of ethanol left in the reboiler.

n0

x0

dx
n0
=
=ln
dn
n1
n1 n
x1 y x
dx
y x
x0

x1

exp
n0
n 1=
Where:
toinitial = time at initial condition,
t(final) = time at final condition,
xb (ethanol) = bottom composition (from the table at time t = 0) = 0.26
xd (ethanol)= top composition (from the table at time t = 0) = 0.37

n1 ( ethanol )

= total number of moles of ethanol in the reboiler.

n1=0.666 L

1.8 Mass Balance on the Distillation Column


Overall mass balance
F=D+B
F = total mole/ molar flow rate in feed
D = total mole/ molar flow rate in distillate
B = total mole/ molar flow rate in reboiler
Component mass balance
FX0 = DXd + BXb
X0 = mole fraction of ethanol in feed
Xd = mole fraction of ethanol in distillate
Xb = mole fraction of ethanol in reboiler
15(X0) = 13.33(0.36) + 1.5(0.32)

X0 = 0.352

Percentage Error=

0.3520.432
=1.85
0.432

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