Module 4 :

BKF2741 Chemical Reaction Engineering Laboratory I

1.0 Title Of Experiment

Effect Of Flowrate On Continous Stirred Reaction Process
2.0 Objective
To study the effect of flowrate on saponification of ethyl acetate and sodium hydroxide in CSTR.
3.0

Introduction
In chemical engineering, chemical reactors are vessels designed to contain chemical reactions.

The design of a chemical reactor deals with multiple aspects of chemical engineering. Chemical engineers
design reactors to maximize net present value for the given reaction. Designers ensure that the reaction
proceeds with the highest efficiency towards the desired output product, producing the highest yield of
product while requiring the least amount of money to purchase and operate. Normal operating expenses
include energy input, energy removal, raw material costs, labor, etc. Energy changes can come in the form
of heating or cooling, pumping to increase pressure, frictional pressure loss (such as pressure drop across
a 90o elbow or an orifice plate), agitation, etc.
There are three main basic models used to estimate the most important process variables of
different chemical reactors:

batch reactor model (batch),

continuous stirred-tank reactor model (CSTR), and

plug flow reactor model (PFR).

In a CSTR, one or more fluid reagents are introduced into a tank reactor equipped with an
impeller while the reactor effluent is removed. The impeller stirs the reagents to ensure proper mixing.
Simply dividing the volume of the tank by the average volumetric flow rate through the tank gives the
residence time, or the average amount of time a discrete quantity of reagent spends inside the tank. Using
chemical kinetics, the reaction's expected percent completion can be calculated. Some important aspects
of the CSTR:
__________________________________________________________________________________
FKKSA/BKF2741/Module/Rev01/2/08/10

Module 4 :

BKF2741 Chemical Reaction Engineering Laboratory I

At steady-state, the flow rate in must equal the mass flow rate out, otherwise the tank will
overflow or go empty (transient state). While the reactor is in a transient state the model
equation must be derived from the differential mass and energy balances.

All calculations performed with CSTRs assume perfect mixing.

The reaction proceeds at the reaction rate associated with the final (output) concentration.

Often, it is economically beneficial to operate several CSTRs in series or in parallel. This

allows, for example, the first CSTR to operate at a higher reagent concentration and
therefore a higher reaction rate. In these cases, the sizes of the reactors may be varied in
order to minimize the total capital investment required to implement the process.

In this experiment, the reaction need to be studied is

NaOH CH 3 COOC 2 H 5 CH 3 COONa C 2 H 5 OH
Saponification is the hydrolysis of an ester under basic conditions to form an alcohol and the salt
of a carboxylic acid. The process is commonly used to refer to the reaction of a metallic alkali (base) with
a fat or oil to form soap. Here, sodium hydroxide is a caustic base. The alkali breaks the ester bond and
releases the fatty acid salt and glycerol. Soaps maybe precipated by salting it out with saturated sodium
chloride. The saponifacation value is the amount of base required to saponify a fat sample. The extent of
the reaction is determined by monitoring sodium hydroxide and sodium acetate concentrations using
conductivity measurements.

_________________________________________________________________________________
_FKKSA/BKF2741/Module/Rev01/2/08/10

Module 4 :

BKF2741 Chemical Reaction Engineering Laboratory I

4.0 Experimental Procedure

4.1

1. CSTR

2. Beakers

3. Measuring Cylinders

5. Sodium Hydroxide

6. Sodium Acetate

7. Ethyl Acetate

4. Stop Watch

Preparation of calibration curve for Conversion vs. Conductivity

1. Prepare 1-L of 0.1 M sodium hydroxide (NaOH) solution and 1-L of 0.1 M sodium acetate
(Na(Ac)) solution.
2. Determine the conductivity for each conversion values by mixing the following solutions into
100 mL of deionised water.
i. 100 mL NaOH for 0% conversion
ii. 75 mL NaOH + 25 mL Na(Ac) for 25% conversion
iii. 50 mL NaOH + 50 mL Na(Ac) for 50% conversion
iv. 25 mL NaOH + 75 mL Na(Ac) for 75 % conversion
v. 100 mL Na(Ac) for 100% conversion
3. Plot the calibration curve of conversion vs. conductivity. Determine the slope and y-axis
intersept.

4.2. Experimental Procedure

1. Charge 10-L of 0.1 M Et(Ac) solution into feed tank T1.
2. Charge 10-L of 0.1 M NaOH solution into feed tank T2.
3. Set the 3-way valve V1 position towards pump P1 and 3-way valve V2 position towards pump
P2.
4. Open valves V3, V4 and V5.
5. Switch on pumps P1 and P2.
6. Adjust the needle valves V3 and V4 to obtain flowrates of approximately 100 mL/min on both
_________________________________________________________________________________
_FKKSA/BKF2741/Module/Rev01/2/08/10

Module 4 :

BKF2741 Chemical Reaction Engineering Laboratory I

flowmeters FT1 and FT2. Make sure the flowrates are always maintained the same and check
that no air bubbles are trapped in the piping.
7. Allow both liquids to fill up all three reactors. Switch on stirrers 1, 2 and 3. Set the stirrer speeds
to approximately 200 rpm.
8. Start the stop watch.
9. Start monitoring the conductivity values (CT1, CT2 and CT3) and temperature values (TT1,
TT2 and TT3) every two minutes until they do not change over time (steady state). Stop the stop
watch and record the time and conductivity values. Determine the conversion in each reactors
from the calibration curve.
10. Repeat the experiment (steps 6 to 9) by changing the flowrate to 150mL/min.

4.3. Shutdown
1. After complete the experiment, drain off any liquids from the reactor and make sure that the
reactor and tubing are cleaned properly. Flush the system with de-ionized water until no traces
of salt are detected.
2. Dispose all liquids immediately after each experiment. Do not leave any solution or waste in the
tanks over a long period of time.
3. Wipe off any spillage from the unit immediately.

5.0 Additional Information

Molar mass of ethyl-acetate = 88.11g/mol
Molar mass of sodium hydroxide = 40 g/mol
Density of ethyl-acetate =0.895 g/ml

_________________________________________________________________________________
_FKKSA/BKF2741/Module/Rev01/2/08/10

Module 4 :

6.0

BKF2741 Chemical Reaction Engineering Laboratory I

Discussion
1. Plot the calibration curve of conversion vs. conductivity and discuss relationship between these
parameters.
2. Plot a graph of conductivity / conversion vs. time for each flowrate. Discuss a plotted graph and
make a comparison in term of conversion for each flowrate.
3. Give the advantages of CSTR and compare with other types of reactors.

4.

Give several applications of CSTR in chemical process or industries (at least 3 applications).

_________________________________________________________________________________
_FKKSA/BKF2741/Module/Rev01/2/08/10

Module 4 :

BKF2741 Chemical Reaction Engineering Laboratory I

Process Diagram for Stirred Tank Reactors in Series

_________________________________________________________________________________
_FKKSA/BKF2741/Module/Rev01/2/08/10