Professional Documents
Culture Documents
NUM
1.0
CONTENTS
Abstract
PAGE
1
2.0
Introduction
3.0
Theory/Literature Review
4.0
Methodology
6
7
5.0
6.0
Conclusion
17
7.0
References
17
8.0
Appendices
17
1.0 ABSTRACT
The experiment aims to study the saponification reaction of sodium hydroxide
an ethyl acetate in a ContinuousStirred Tank Reactor (CSTR). In this experiment,
the aims also include investigating the operational behaviour of a reaction in the
CSTR system, techniques when using CSTR for a reaction process and effect of
flow changes on the reaction. Before all apparatus is set-up, the conductivity
calibration curve with different molar concentration were prepared to determine
the conversion of the reactants to products in the reactor since we cannot
distinguish the mixture of reactants and products easily from the mixture. Then,
both sodium hydroxide and ethyl acetate were prepared according to the given
volume and concentration before transferred to the tanks. When the process
starts, the conductivity and temperature of the reaction were recorded in every
two minutes for 30 minutes. When the liquid level in the CSTR reached 2L, the
space time as well as conductivity and temperature was recorded. After flow the
reaction medium into the buffer tank, the readings are recorded for another 10
minutes. Then, all valves and pumps were closed, and all liquid will be discarded
through valve V4. The process is repeated several times using different feeds of
flow rates. Theoretically, as the time goes once the experiment starts, the conductivity
values should gradually close up its value to the conductivity value of pure product that is
determined before the reaction starts. The conversion should gradually increase as the time
goes by. From the result obtained, it shows that on the graph concentration versus time, we
get the value of rate constant which is in this experiment we get k = 0.6342 L/mol. min and
little bit differ by using by formula which is k = 1.317 L/mol .min. Other than that, the
reaction order is successfully to approve which is second order of reaction based on linear
graph of concentration versus time. The errors and recommendations also were discussed in
the discussion section. The conclusion section concludes all the objectives and calculations
on this experiment.
2.0 INTRODUCTION
The Continuous- Stirred Tank Reactor (CSTR) is common type of reactor used
in industrial processing which is primarily used for liquid phase reaction. The
reactor was operate in steady state condition with continuous flow of reactants
and products and assumed as perfectly mixed. The feed assumes a uniform
composition throughout the reactor; exit stream has the same composition as in
the tank. There is no time dependence or position dependence of the
temperature, the concentration and the reaction rate in the tank. The usage of
the CSTR is when agitation is required and series configurations for different
concentration streams. Besides that, the advantages using this reactor compare
to the other are it has good temperature control, easily adapt to two phases, low
operating cost and easy to clean. But, the CSTR has lowest conversion per unit
volume and requires large volume to obtain the desired conversions. When high
conversions of reactants are needed, several CSTRs in series can be used.
Equally good results can be obtained by dividing a single vessel into
compartments while minimizing back-mixing and short-circuiting. The larger the
number of CSTR stages, the closer the performance approaches that of a tubular
plug-flow reactor.
This experiment was carried out to study the saponification reaction between
sodium hydroxide and ethyl acetate in a continuous stirred tank reactor (CSTR).
This process was conducted to produce soap, usually from fat and lye.
Technically, the saponification process involves base (caustic soda NaOH)
hydrolysis of triglycerides, which are ester of fatty acids, to form sodium salt of
carboxylate. Beside saponification reaction, the other scopes of this experiment
are to investigate the operational behavior of a reaction in CSTR, to calculate the
reactant conversion based on the conductivity calibration curve. Also, the
significant of doing this experiment was to verify the reaction order obtained
from the hypothesis of the experiment and to determine the rate constant of
saponification reaction between sodium hydroxide and ethyl acetate using
graphical and analytical technique. The result of CSTR of the reaction kinetics,
rate law and conversion is compared with a batch reactor for the same reaction
as stated in scope of experiment.
The reaction kinetics and rate law of saponification reaction in a CSTR can
be determined using conductivity calibration curve. Conductivity is a measure of
how well a solution can conducts electricity. A solution must contain charged
particles, or ions to carry a current. Most conductivity measurements are made in
aqueous solutions, and the ions responsible for the conductivity come from
electrolytes dissolved in the water. There are two ways to calibrate conductivity
sensors. The sensor can be calibrated against a solution of known conductivity or
it can be calibrated against a previously calibrated sensor and analyzer.
Normally, the sensor should be calibrated at a point near the midpoint of the
operating range calibration changes the cell constant. For this experiment, the
calibration curve is prepared using different molar concentration of sodium
hydroxide and sodium acetate.
3.0
LITERATURE REVIEW
In this experiment we are going to use continuous stirred tank reactor (CSTR)
to react sodium hydroxide and ethyl acetate to produce sodium acetate. Based
on H. Scott Fogler, Elements of Chemical Reaction CSTR normally operated at
steady state and is assumed to be perfectly mixed. Based on this statement, the
temperature of the reactor and reaction mixture should not have any major
change throughout the experiment. Concentration and volume of the reactants
should be the same as another reactant since it is a one-to-one ratio for the
reaction. The reactants are well mixed and so the reaction must be efficient.
However, reactants and products are always mixed well together in the reactor
making it difficult to determine the product conversion. That is why a standard
conductivity calibration curve has to be prepared before the experiment.
Conductivity of the mixture will indicate the percent products present which is
determine using conductivity meter.
Theory
Saponification between sodium hydroxide (NaOH, denotes as A ) and ethyl
acetate (EA, denotes as B) is basically second order elementary reaction. For
steady state constant volume isothermal CSTR, the design equation is :
V=
v CA 0 X
r A
r A=k C A C B
Basically, reactant conversion, X, can be calculated using the following equation :
X =1
CA
CA 0
X =1
CB
C B0
C A =C A 0 ( 1X )
C B=C B 0 ( 1 X )=C A 0 (1X ) ,
when
C B 0=C A 0
Therefore,
r A=k C 2A 0 (1X )2
If we combine the above equation, we see that
V=
v CA 0 X
k C 2A 0 (1 X)2
V=
vX
k C (1 X)2
A0
4.0
METHODOLOGY
B. Operating procedure
1. 9L solution of 0.1M NaOH (8g per 2L H2O) and 9L solution of 0.1M EA
(19.6mL per 2L H2O) are prepared and these solutions were poured into
tanks T1 and T2 respectively.
2. Next, pumps P1 and P2, and stirrer S1 are switched on. The feed flow rates
into the CSTR are adjusted to be at 40 cm 3/min using valves F1 and F2.
The stopwatch was started immediately as the pumps and stirrer were
switched on. The conductivity and temperature of the reaction medium in
the CSTR were measured for every 2 minutes for over 30 minutes.
3. When liquid level inside the CSTR reached 2000 cm 3(2L), the space time,
conductivity and temperature of the reaction medium were recorded.
4. Then, the reaction is flowed into the buffer tank by opening valve V3.
Measurements were continued taken for 10 minutes.
5. After 30 minutes, valves F1 and F2 were closed, and pumps P1 and P2
were stopped. All liquids were discharged through valve V4.
6. The experiment was repeated for different feed flow rates at 60 cm 3, 100
cm3 and 120 cm3.
7. All
residual
NaOH
and
Ethyl
Acetate
were
discharged
once
the
Callibration
Data
Conversion
Conductivity
(S)
0.1M NaOH
0.0
0.05M NaOH +
0.05M Sodium
Acetate
0.5
0.1M Sodium
Acetate
1.0
12.17
8.69
5.17
0.8
Conversion
0.6
0.4
0.2
0
4
10
11
12
13
Conductivity (S)
Conductivity Temperature
(S)
(C)
Conversion
CA
(mol/L)
CB
(mol/L)
CC
(mol/L)
CD
(mol/L)
1/CA
(L/mol)
0.02033
0.08713
0.02033
0.08713
12.55
0.10307
0.06849
0.04105
0.04334
0.04448
0.04605
0.04691
0.04834
0.04920
0.05020
0.05134
0.05163
0.05249
0.05306
0.05334
0.10307
0.06849
0.04105
0.04334
0.04448
0.04605
0.04691
0.04834
0.04920
0.05020
0.05134
0.05163
0.05249
0.05306
0.05334
10.75
28.5
0.2033
0.07967
0.07967
18.27
30.2
-0.8713
4
6
8
10
12
14
16
18
20
22
24
26
28
30
32
4.96
7.38
9.30
9.14
9.06
8.95
8.89
8.79
8.73
8.66
8.58
8.56
8.50
8.46
8.44
30.0
30.0
30.0
30.0
30.1
30.1
30.1
30.2
30.2
30.2
30.3
30.3
30.3
30.3
30.3
1.0307
0.6849
0.4105
0.4334
0.4448
0.4605
0.4691
0.4834
0.4920
0.5020
0.5134
0.5163
0.5249
0.5306
0.5334
0.18713
0.00307
0.03151
0.05895
0.05666
0.05552
0.05395
0.05309
0.05166
0.05080
0.04980
0.04866
0.04837
0.04752
0.04694
0.04666
0.18713
0.00307
0.03151
0.05895
0.05666
0.05552
0.05395
0.05309
0.05166
0.05080
0.04980
0.04866
0.04837
0.04752
0.04694
0.04666
5.34
325.56
31.74
16.96
17.65
18.01
18.54
18.84
19.36
19.68
20.08
20.55
20.67
21.05
21.30
21.43
Conductivity
(S)
Temperature
(C)
Conversion
3.46
30.6
1.2451
9.79
30.8
0.3405
9.56
30.7
0.3734
9.09
30.7
0.4405
9.02
30.7
0.4505
8.81
30.7
0.4806
8.60
30.7
0.5106
8.38
30.8
0.5420
8.26
30.8
0.5591
CA
(mol/L)
0.02451
0.06595
0.06266
0.05595
0.05495
0.05194
0.04894
0.04580
0.04409
CB
(mol/L)
0.02451
CC
(mol/L)
0.12451
0.06595
0.03405
0.06266
0.03734
0.05595
0.04405
0.05495
0.04505
0.05194
0.04806
0.04894
0.05106
0.04580
0.05420
0.04409
0.05591
CD
(mol/L)
0.1245
1
0.0340
5
0.0373
4
0.0440
5
0.0450
5
0.0480
6
0.0510
6
0.0542
0
0.0559
1
1/CA
(L/mol)
-40.81
15.16
15.96
17.87
18.20
19.25
20.43
21.83
22.68
18
20
22
24
8.18
30.8
0.5706
8.04
30.8
0.5906
8.00
30.8
0.5963
7.96
30.9
0.6020
0.04294
0.04094
0.04037
0.03980
0.04294
0.05706
0.04094
0.05906
0.04037
0.05963
0.03980
0.06020
0.0570
6
0.0590
6
0.0596
3
0.0602
0
23.29
24.43
24.77
25.13
Conductivity
(S)
Temperature
(C)
Conversion
1.1250
CA
(mol/L)
0.01250
CB
(mol/L)
0.01250
4.30
31.1
10.10
CC
(mol/L)
0.11250
31.0
0.2962
0.07038
0.07038
0.02962
9.03
31.0
0.4491
0.05509
0.05509
0.04491
9.42
31.0
0.3934
0.06066
0.06066
0.03934
9.05
31.0
0.4463
0.05537
0.05537
0.04463
10
8.77
31.0
0.4863
0.05137
0.05137
0.04863
12
8.60
31.0
0.5106
0.04894
0.04894
0.05106
14
8.52
31.0
0.5220
0.04780
0.04780
0.05220
16
8.47
31.0
0.5291
0.04709
0.04709
0.05291
18
8.43
31.0
0.5349
0.04651
0.04651
0.05349
CD
(mol/L)
0.1125
0
0.0296
2
0.0449
1
0.0393
4
0.0446
3
0.0486
3
0.0510
6
0.0522
0
0.0529
1
0.0534
9
1/CA
(L/mol)
CD
(mol/L)
0.1316
5
0.0409
1
0.0499
1
0.0544
9
0.0590
6
1/CA
(L/mol)
-79.98
14.21
18.15
16.48
18.06
19.47
20.43
20.92
21.24
21.50
Conductivity
(S)
Temperature
(C)
Conversion
1.3165
CA
(mol/L)
0.03165
CB
(mol/L)
0.03165
2.96
31.0
9.31
CC
(mol/L)
0.13165
31.0
0.4091
0.05909
0.05909
0.04091
8.68
30.9
0.4991
0.05009
0.05009
0.04991
8.36
30.9
0.5449
0.04551
0.04551
0.05449
8.04
30.9
0.5906
0.04094
0.04094
0.05906
-31.59
16.92
19.97
21.97
24.43
10
7.90
30.9
0.6106
0.03894
0.03894
0.06106
12
7.88
30.9
0.6134
0.03866
0.03866
0.06134
14
7.79
30.9
0.6263
0.03737
0.03737
0.06263
16
7.70
30.9
0.6392
0.03608
0.03608
0.06392
18
7.66
30.9
0.6449
0.03551
0.03551
0.06449
10
15
20
25
30
35
0.00
1/CA (L/mol) -10.00 0
10
15
20
25
-20.00
-30.00
-40.00
-50.00
Time, t (min)
30
0.0610
6
0.0613
4
0.0626
3
0.0639
2
0.0644
9
25.68
25.87
26.76
27.71
28.16
20.00
0.00
1/CA (L/mol)
-20.00 0
10 12 14 16 18 20
-40.00
-60.00
-80.00
-100.00
Time, t (min)
f(x) = 2x + 0.58
R = 0.45
10.00
1/CA (L/mol)
0.00
-10.00 0
10 12 14 16 18 20
-20.00
-30.00
-40.00
Time, t (min)
Space
time,
(min)
Conductivity
(S)
Temperature,
T (C)
Conversion
k
(L/mol.
Theoretical
space time,
th(min)
min)
40
60
100
120
22.40
14.00
8.51
6.47
8.64
8.38
8.91
8.28
30.2
30.8
31.0
30.9
0.5048
0.5420
0.4663
0.5563
0.4117
0.5168
0.3274
0.5651
25.00
16.67
10.00
8.33
CALCULATION
Based on Graph 1 the conductivity calibration curve, we get the linear equation of the curve
as y = -0.1429x + 1.7395, where
y represents conversion value, X
x represents conductivity (S).
When flow rate is 40 cm3/min, the conductivity at time, t=10 min is 9.14 S,
the conversion value is
y
= -0.1429(9.14) + 1.7395
= 0.4334
For the concentration of NaOH after the reaction, CA
CA = CA0 (1 - X)
= 0.1 M (1 0.4334)
= 0.05666 M
= 0.05666 mol/L
For the concentration of Ethyl Acetate, CB
CB = C A
= 0.05666 mol/L
For the concentration of Sodium Acetate, CC
CC = CAO.X
= 0.1M (0.4334)
= 0.04334 M
= 0.04334 mol/L
For the concentration of Ethyl Alcohol, CD
CD = C C
= 0.04334 mol/L
Four linear graphs of 1/CA vs. time are plotted, which indicates the second order reaction of
the saponification process.
1/CA =1/CA0 + kt
By using graphical method, we know that the slope of the graph indicates the value of k.
Average value of k based on the four graphs (of different flow rates)
kav= (2.7364+1.3881+2.9988+2.0007)/4
= 9.124/4
= 2.281 L/mol.min
Whereas by using analytical method, from the equation simplified
v0 X
V= k C (1X )2
A0
v0 X
k=
V C A 0 (1 X)2
Discussion
At the end of our experiment and after done the calculation, we can
calculate the reactant conversion, verify the reaction order and determine the
rate constant.
1/CA =1/CA0 + kt
graph which is corresponding to the second order and the slope of the graph
referring to the positive rate of constant.
Batch Reactor
CSTR
Reaction
kinetics
Rate Law
Conversion
Some errors in the process of experiment include errors during preparation of the solutions,
side reaction occurs during the experiment and inconsistency of flow rates from tanks to
CSTR reactor. The flow rate went up and down due to possibly faulty valve since another
valve from another tank was working fine.
Some recommendations to improve the result include study the experiment before entering
the lab to conduct the experiment and always check for errors before starting the experiment
including preparation of reactants material (weighing and dissolving in solution) and
systematic errors like zero errors.
6.0 CONCLUSION
A common type of reactor used in industrial processing is the continuous-stirred tank
reactor (CSTR) which is used primarily for liquid phase reaction. It is normally operated at
steady state and assumed to be perfectly mixed. The conductivity calibration curve is
prepared using different molar concentration of sodium hydroxide and ethyl acetate. This
calibration curve can be used to determine the reaction kinetics and the rate law of the
process. Based on the graph concentration versus time, we get the value of rate constant
which is in this experiment we get k = 0.6342 L/mol.min and little bit differ by using by
formula which is k = 1.317 L/mol.min. Other than that, the reaction order is successfully to
approve which is second order of reaction based on linear graph of concentration versus time.
7.0 REFERENCES
H. Scott Fogler, Elements of Chemical Reaction Engineering, 4rd edition,
Pearson Education Limited, 2014.
8.0 APPENDICES
Figure shows Continuous stirred tank reactors, (a) With agitator and internal heat
transfer surface, (b) With pump around mixing and external heat transfer surface.
(a)
(b)
(c)
The figure show the (a) zero order reaction (b) first order reaction (c) second
order reaction