CSTR Unit Ops Lab

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Sison, Kelly Sheine O.

5ChE-A

CONTINUOUS STIRRED TANK REACTOR

Introduction
A continuous stirred tank reactor (CSTR) is a batch reactor equipped with an impeller or other
mixing device to provide efficient mixing. In chemical engineering the name CSTR is often used to refer
to an idealized agitated tank reactor used to model operation variables required to attain a specified
output.
Saponification can be defined as a “hydration reaction where free hydroxide breaks the ester bonds
between the fatty acids and glycerol of a triglyceride, resulting in free fatty acids and glycerol,” which
are each soluble in aqueous solutions. This process specifically involves the chemical degradation of
lipids, which are not freely soluble in aqueous solutions. Heat-treated lipid residues are more difficult to
remove than nonheat-treated residues due to polymerization.
In this experiment, saponification of ethyl acetate in the presence of sodium hydroxide is used to
demonstrate the saponification reaction. The saponification of ethyl acetate reaction is as follows.
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
When it comes to chemical kinetics, this reaction is a prominent second order reaction. [1] This
reaction is in the form
A+BC+D
And the rate equation is
-d CA kmol
r= =k CA CB 3
dt m ∙s
The specific constant, k, is determined by analyzing the effect of temperature in the reaction using
Arrhenius law expression.
− Ea
( )
RT
k=Ae
E 1
ln k =ln A− x( )
R T

Methodology
3

1
Figure 1. Set up and Materials

The materials and equipment that was used during the experiment are Armfield Continuous Stirred
Tank (1), Sodium Hydroxide and Ethyl Acetate amber bottles (2), hot water circulator (3), drain (4) and
operation controller (5) which can be seen in Figure 1. Distilled water, beaker, top loading balance,
stirring rod, and watch glass were all used in the preparation of the chemicals for the experiment.
Sodium Hydroxide and Ethyl Acetate were both prepared at large volumes with a concentration of 0.1M
before starting the experiment to avoid insufficient amount of chemicals inside the reactor as the
process is continuous.

For the system start-up, the computer was switched on and connected to the CSTR. CEM software
was launched and the appropriate experiment was chosen from the menu. The telephone icon from the
tab was clicked to allow control of the CSTR through the software. After successfully connecting the
CSTR, the hot water circulator was filled with water up to the low-level electrode which is 30 cm from
the top.
For the experiment proper, three trials were performed at different temperatures running up to 45
minutes each. The temperatures are 20°C, 30°C and 40°C respectively. The data were set to be recorded
every five (5) minutes. The flow rate for all runs is 40 mL/min.
To shutdown the system after the trials, the chemicals and water used were drained from the
equipment. It is then washed with water to remove chemical residues. After recording the data, the
software was closed, and the computer is disconnected from the CSTR. Both the computer and the CSTR
system was switched off and disconnected to power supply afterwards.

Results and Discussion


The data acquired from each trial of the experiment is shown in the table below.
Measured Conversion of Specific Rate
Time (min) Conductivity NaOH Constant Ln K 1/T
00:00:00 5.771 0.840 0.841 -0.173 0.027
00:05:00 9.902 0.300 0.016 -4.135 0.028
00:10:00 9.043 0.420 0.034 -3.381 0.028
00:15:00 8.584 0.480 0.049 -3.016 0.028
00:20:00 8.418 0.510 0.055 -2.900 0.028
00:25:00 8.320 0.520 0.600 -0.511 0.028

Table 1. Data Acquired on CSTR: Experiment with Heater


Run 1
Temperatur Computed Frequency  1.161x101
7
  e (oC): 20 Factor (A)
Temperatur Computed Activation
e (K) 293 Energy (E) -1551.75
Specific
Time Measured Conversio
Rate Ln K 1/T
(min) Conductivity n of NaOH
Constant
0 0.47 1.55 0.136  -1.995  0.00327 
5 9.49  0.32  0.018  -4.017 0.00327
10 8.64  0.44  0.037  -3.297 0.00327
15 8.19  0.50  0.052  -2.956 0.00327
20 8.02  0.52  0.061  -2.797 0.00327
25 7.98  0.53  0.064  -2.749  0.00327
30 7.99  0.53  0.064  -2.749  0.00327
35 7.99  0.53  0.065  -2.733 0.00327
40 8.00  0.53  0.064  -2.749  0.00327
45 8.03  0.53  0.063  -2.765  0.00326

Table 1. Data Acquired on CSTR: Experiment with Heater


Run 2
Temperatur Computed Frequency  6.197x105
5
  e (oC): 30 Factor (A)
Temperatur Computed Activation
e (K) 303 Energy (E) -4807.666
Specific
Time Measured Conversio
Rate Ln K 1/T
(min) Conductivity n of NaOH
Constant
0 0.27 1.57  0.129   -2.048 0.00329 
5 9.40 0.30  0.016  -4.135 0.00329
10 8.35 0.45  0.041   -3.194 0.00329
15 7.81 0.53  0.065   -2.733 0.00328 
20 7.57 0.57  0.083   -2.489 0.00328
25 7.50 0.58  0.091   -2.397  0.00328
30 7.50 0.58  0.090   -2.408 0.00328
35 7.47 0.59  0.096   -2.343 0.00327
40 7.46 0.60  0.097  -2.333  0.00327
45 7.45 0.60  0.1   -2.303  0.00327

Table 1. Data Acquired on CSTR: Experiment with Heater


Run 3
Temperatur Computed Frequency
e (oC): 40 Factor (A) 4.05x10-9 
 
-
Temperatur Computed Activation 651.4192
e (K) 313 Energy (E) 3
Time Measured Conversio Specific Rate
Ln K 1/T
(min) Conductivity n of NaOH Constant
0  0.46 1.55 0.135  -2.002  0.00327 
5  10.72 0.28  0.015  -4.200  0.00321
10  9.97 0.54  0.067  -2.703  0.00311
15  9.36 0.57  0.084  -2.477  0.00313
20  9.02 0.58  0.088  -2.430  0.00315
25  8.84 0.58  0.085  -2.465  0.00317
30  8.72 0.57  0.081  -2.513  0.00319
35  8.42 0.59  0.092  -2.386  0.00320
40  6.45 0.83  0.765  -0.268  0.00320
45  6.04 0.89  1.828  0.603  0.00320
Plot of %conversion of NaOH vs Time
1.8
1.6
1.4
%conversion of NaOH

1.2
1 Run 1
Run 2
0.8
Run 3
0.6
0.4
0.2
0
0 5 10 15 20 25 30 35 40 45 50
Time

The plot of %conversion of NaOH over time shows that through time, the %conversion of NaOH
decreases. This is because the reactants get used up and the concentration of the product increases.
This is almost true on runs 1 and 3, however, it is almost constant on the 2 nd run.

Plot of Specific rate constant vs Time at different Temperatures


0.12

0.1
Specific rate constant

0.08
Run 1
0.06 Run 2
Run 3
0.04

0.02

0
0 5 10 15 20 25 30 35 40 45 50
Time

The plot of the specific rate constant vs time at different temperatures show that the specific rate
constants is same through out at the same temperature. This is also true on runs 1 and 3 but not on 2 as
it changed greatly especially on the 40-minute mark.

Analysis and Interpretation of Data


1. What is the relationship between the conductivity and degree of conversion of ethyl acetate
and sodium hydroxide?

A: Both the conversion of sodium hydroxide and ethyl acetate decreases with time while the
conductivity increases at first then decrease then stay constant.

2. What is the relationship between time and conversion of NaOH?

A: The conversion of sodium hydroxide decreases with time because it is getting used up and the
concentration of the product increases.

3. What is the relationship between specific rate constant and temperature of reaction?

A: Being a function of temperature, the specific rate constant increases with time but stays
almost constant throughout each run.

4. What is the reason of deviation of experimental values of frequency factor and activation
energy?

A: The deviation results from multiple errors such as human errors and mechanical error from
the equipment. From the preparation of the chemicals to the cleaning and the efficiency of the
equipment. All of these add up to the deviation of the experimental values to the theoretical
values.

Practical Questions
1. What will happen or what will be the change in conversion if the temperature for three runs is
kept constant with varying flow rates?

A: The change in conversion would also increase with the increase in flow rate even if the
temperature is kept the same.

2. What is the best condition in achieving the highest concentration, high flow rates with slow
stirring speed or low flow rates with high stirring speed?

A: Highest conversion would be achieved at high stirring speed of the CSTR. Agitation also
affects the conversion and with slower accumulation, the conversion would be faster.

3. Briefly explain the need to operate at high temperature. Give example wherein high operating
temperature is desired.

A: High temperature is needed when faster conversion is desired. If a company wants to


produce more products by manipulating only the temperature, the temperature must be raised
to do so.

Conclusion and Recommendation


For the saponification of ethyl acetate using a CSTR, factors such as temperature, agitation and flow
rate affects the conversion of the reagents to products. The greater these factors are, the faster the
conversion would be. The specific rate constant, however, remains constant at each temperature.
Run number 2 shows deviation of data from runs 1 and 3. This is caused by errors such as human
errors and mechanical error. It is recommended that the preparation and execution of the experiment
be done carefully and accurately. Also, the condition of the equipment must be checked using a
calibrating procedure to ensure that the equipment is in optimal condition.

References
 Walas, S. M. (1989). Reaction kinetics for chemical engineers. Boston: Butterworths.

 (n.d.). Retrieved from https://www.vapourtec.com/flow-chemistry/continuous-stirred-tank-

reactor-cstr/

 Kc, W. U. (2014). Aspen Plus Simulation of Saponification of Ethyl Acetate in the Presence of
Sodium Hydroxide in a Plug Flow Reactor. Journal of Chemical Engineering & Process
Technology, 5(6). doi:10.4172/2157-7048.1000205

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