University of Santo Tomas CHE 514L:

Faculty of Engineering Chemical Engineering Laboratory II

Department of Chemical Engineering Formal Laboratory Report
Name of Members:
1. Avendano, Jay Russell
2. Purugganan, Stephanie
3. Sison, Kelly Sheine
4. Vicencio, Jeelaine
Section: 5ChE-A Group No: 2 Instructor: Ma’am Mardie Pacia

Experiment1: 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 non-heat-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. This reaction is in the
form
A+B→C+D
And the rate equation is
-dCA kmol
r= =kCA 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
𝑘 = 𝐴𝑒 (−𝑅𝑇)
𝐸𝑎 1
ln 𝑘 = ln 𝐴 − 𝑥( )
𝑅 𝑇
Methodology Commented [S1]:

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 minutes
𝑚𝑙
with a flowrate of 40 .
𝑚𝑖𝑛

For the shutdown proper, the chemicals and water used were drained from the equipment. It was washed with
water in order for it 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.

TRIAL 1
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
00:30:00 8.252 0.520 0.062 -2.781 0.028
00:35:00 8.184 0.530 0.064 -2.749 0.028
00:40:00 8.135 0.540 0.067 -2.703 0.028
00:45:00 8.096 0.540 0.069 -2.674 0.028
𝑘𝑗
Temperature (°C): 20°C Computed Activation Energy (E): −1450.417
𝑚𝑜𝑙
Temperature (K): 293

TRIAL 2
Measured Conversion of Specific Rate
Time (min) Conductivity NaOH Constant Ln K 1/T
00:00:00 8.0762 0.5400 0.0690 -2.6736 0.0285
00:05:00 8.0469 0.5400 0.0700 -2.6593 0.0286
00:10:00 8.0273 0.5500 0.0700 -2.6593 0.0286
00:15:00 8.0273 0.5500 0.0700 -2.6593 0.0288
00:20:00 9.6680 0.3200 0.0190 -3.9633 0.0288
00:25:00 11.6406 0.0600 0.0020 -6.2146 0.0287
𝑘𝑗
Temperature (°C): 30°C Computed Activation Energy (E): −3193.807
𝑚𝑜𝑙
Temperature (K): 303

TRIAL 3
Measured Conversion of Specific Rate
Time (min) Conductivity NaOH Constant Ln K 1/T
00:00:00 12.99 0.5400 0.0020 -6.2146 0.0289
00:05:00 13.62 0.5400 0.0020 -6.2146 0.0265
00:10:00 14.60 0.5500 0.0030 -5.8091 0.0236
00:15:00 15.66 0.5500 0.0030 -5.8091 0.0210
00:20:00 16.52 0.3200 0.0030 -5.8091 0.0193
00:25:00 17.21 0.0600 0.0030 -5.8091 0.0182
𝑘𝑗
Temperature (°C): 40°C Computed Activation Energy (E): −18.541
𝑚𝑜𝑙
Temperature (K): 313
 The graph 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 for trial
2, however, it is almost constant on trial 3.

The graph of the specific rate constant vs time shows that the specific rate constants is same throughout at
the same temperature. This is shown on trials 2 and 3.
Analysis and Interpretation of Data
1. What is the relationship between the conductivity and degree of conversion of ethyl acetate and sodium
hydroxide?
The conversion of sodium hydroxide and ethyl acetate decreases with time while the conductivity increases
during the first few minutes, decreases as it reached its constant value.

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

The conversion of sodium hydroxide decreases with time because it is being consumed and turned it into
a new product

3. What is the relationship between specific rate constant and temperature of reaction?
The specific rate constant increases as the temperature increases but it will reach its maximum or constant
value throughout the process.

4. What is the reason of deviation of experimental values of frequency factor and activation energy?
Errors such as human errors and mechanical error from the equipment are some reasons why there was
deviation in the experiment. From the preparation of the chemicals and the efficiency of the equipment.

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?
The conversion for each run would differ as the flow rate varies even if the temperature was kept constant
for the whole experiment.

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?
The best condition to achieve highest conversion would be lowering the flow rates but with high stirring
speed of the CSTR.

3. Briefly explain the need to operate at high temperature. Give example wherein high operating
temperature is desired.
In order for a reaction to achieve faster conversion, high temperature is needed. If a researcher wants to
speed up the process and achieve almost a 100% conversion, temperature should be set to its highest.

Conclusion and Recommendation

Saponification of ethyl acetate using a CSTR is affected with different factors such as temperature and flow rate.
These factors alter the conversion of the reactants to the desired product. As these factors increases, the conversion
of the reactants also increases. It is also shown through the experimental data obtained that there were 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, in order to avoid errors, calibrate every equipment before using them.

References
• Macku, Lubomir (2011). WSEAS TRANSACTIONS on HEAT and MASS TRANSFER

• (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