ADDIS ABABA SCIENCE AND TECHNOLOGY UNIVERSITY

COLLEGE OF BIOLOGICAL AND CHEMICAL ENGINEERING

Chemical Engineering Department

Reaction Engineering Laboratory (ChEg 3123)

CSTR Reactor (QRCAC)

Laboratory Manual

Prepared by Assefa Alene (MSc.)

AASTU, 2020
 Experiments in CSTR Reactor

Introduction
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 usually referred to as the continuous-stirred tank reactor (CSTR) or

back mix reactor, and is used primarily for liquid phase reactions. More specifically, continuous
stirred tanks are used for relatively slow reactions of liquids and slurries. Its normal operation is
at steady state and it’s assumed to be perfectly mixed. Consequently, there is no time dependence
or position dependence of the temperature, the concentration, or the reaction rate inside the CSTR.
In other words, the concentration and temperature is the same at every point inside the reactor.
Therefore, the temperature and concentration in the exit stream are modeled as being the same as
those inside the reactor. This is an extremely helpful and important point because otherwise, in
systems where mixing is not ideal, we would not know the concentration of the exit stream using
a well-mixed model and would have to resort to other methods, such as residence-time
distributions to obtain meaningful results. Ideally, stirred tank reactors run most efficiently when
the liquid level is equal to the tank diameter, although at higher pressures slimmer diameters are
more economical and would decrease residence times. The residence time along with space
velocity and product distribution are usually found from a pilot plant. Also, the CSTR can either
be used by itself or, as part of a series or battery of CSTRs. A battery of four or five in series is
often used. It is also important to note that the mixer power input to a homogeneous reaction stirred
tank is usually 0.1-0.3 kW/m^3, but three times this amount when heat is to be transferred.

The hydrolysis of a fat or oil in alkaline condition produces soap for cleaning purpose and the
reaction which occurs in the alkaline conditions is called saponification [1]. Saponification is the
hydrolysis of an ester under basic conditions to form an alcohol and the salt of a carboxylic acid
(carboxylates) and it is commonly used to refer to the reaction of a metallic alkali with a fat or oil
to form soap. Thus, the hydrolysis of ethyl acetate (CH3OOC2H5) by sodium hydroxide (NaOH)
to produce sodium acetate (CH3COONA) and ethanol (C2H5OH) is saponification reaction
although the end product is not soap. There are so many studies available in the literature on the
process improvement for this saponification reaction.
 𝐶𝐻3 𝐶𝑂𝑂𝐶𝐻2 𝐶𝐻3 + 𝑁𝑎𝑂𝐻 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶𝐻3 𝐶𝐻2 𝑂𝐻

Saponification reaction of ethyl acetate by sodium hydroxide is studied experimentally in a

continuous stirred tank reactor at 1 atmospheric pressure. The aim of this study is to investigate
the influence of operating conditions on the conversion and specific rate constant. The parameters
considered for analysis are temperature, feed flow rate, residence time, volume of reactor and
stirrer rate. The steady state conversion of 0.45 achieved after a period of 30 minutes. Conversion
decreases with increase of reactant flow rate due to decrease of residence time. The stirrer rate has
a positive effect on the conversion and rate constant. Specific rate constant and conversion increase
with temperature within the studied temperature range. Within the range of reactor volume selected
for analysis, conversion increases with increase in reactor volume. The results obtained in this
study may be helpful in maximizing the conversion of ethyl acetate saponification reaction at
industrial scale in a CSTR.

The continuous stirred tank reactor is specially used for the kinetic study of homogeneous liquid
– liquid reactions.

Theory

As with all continuous flow reactors, CSTRs are almost always operated at steady state. In
addition, the contents inside the reactor are assumed to be perfectly mixed. As a result, there is no
time or position dependence of the temperature, concentration or reaction rate inside the CSTR.
Therefore, all variables are the same at any point within the reaction vessel.

i) Material balance: The general mole balance equation for j species is

𝑑𝑁𝑗
𝐹𝑗0 − 𝐹𝑗 + ∫ 𝑟𝑗 𝑑𝑉 = 𝑑𝑡

𝑑𝑁𝑗
For CSTR reactor, since it is operated at steady state, there is no accumulation term, = 0 and
𝑑𝑡

due to the presence of uniform (perfect) mixing, ∫ 𝑟𝑗 𝑑𝑉 = 𝑟𝑗 𝑉. Therefore, the general material
balance equation is reduced to

𝐹𝑗0 − 𝐹𝑗 + 𝑟𝑗 𝑉 = 0
Calculating for V and gives as

𝐹𝑗0 − 𝐹𝑗
𝑉=
−𝑟𝑗

 This is the design equations for CSTR reactor

ii) Conversion: In chemical reactions, it is often that one of the reacting species depletes before
the others. When this occurs, the reaction terminates, and thus this reagent is termed the limiting
reactant. In most instances, it is best to choose the limiting reagent as the basis of stoichiometric
calculations.

Consider a general reaction.

𝑎𝐴 + 𝑏𝐵 𝑐𝐶 + 𝑑𝐷

where the uppercase letters represent chemical species and the lowercase letters represent
stoichiometric coefficients (moles). Suppose that species A were to be the limiting reagent, we
then divide the reaction expression by the coefficient of species A, to obtain

𝑏 𝑐 𝑑
𝐴+𝑎𝐵 𝐶 +𝑎𝐷
𝑎

Now that the other chemical species are on a “per mole of A” basis, we would then want to know
how far the reaction proceeds to the right, or how many moles of A are consumed to form one
mole of C. These can be determined by defining a parameter called conversion.

For CSTR reactor, the conversion of chemical species A is simply the number of molar flow rates
of A that have reacted per molar flow rates of A fed into the system.

𝑀𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝐴 𝑟𝑒𝑎𝑐𝑡𝑒𝑑 𝐹𝐴0 − 𝐹𝐴

𝑋𝐴 = =
𝑀𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝐴 𝑓𝑒𝑑 𝐹𝐴0

For CSTR reactor, conversion can also be expressed in terms of concentrations

𝐶𝑜𝑛𝑐𝑒𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐴 𝑐𝑜𝑛𝑠𝑢𝑚𝑒𝑑 𝐶𝐴0 − 𝐶𝐴

𝑋𝐴 = =
𝐶𝑜𝑛𝑐𝑒𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝐴 𝑓𝑒𝑑 𝐶𝐴0
iii. Saponification Reaction: Now that we understand the basic chemistry and chemical
engineering involved in chemical reactors, consider a chemical reaction between an ester and
sodium hydroxide. This process is also known as saponification. The reaction is reversible, and is
described by

𝐶𝐻3 𝐶𝑂𝑂𝐶𝐻2 𝐶𝐻3 + 𝑁𝑎𝑂𝐻 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶𝐻3 𝐶𝐻2 𝑂𝐻

Ethyl acetate Sodium hydroxide Sodium acetate Ethanol

𝐶𝐻3 𝐶𝑂𝑂𝐶𝐻2 𝐶𝐻3 + 𝑂𝐻 − + 𝑁𝑎+ 𝐶𝐻3 𝐶𝑂𝑂 − + 𝑁𝑎 + + 𝐶𝐻3 𝐶𝐻2 𝑂𝐻

The ethyl acetate molecules split into acetate ions and ethanol molecules, consuming hydroxide
ions provided by the sodium hydroxide in the process. The progress of the reaction can thus be
tracked accurately by the change in hydroxide ions. This can be observed by the conductivity
change in the reactor vessel, since the presence of hydroxide ions increase the conductivity in a
solution.

Experiment 1: Calibration graph plot

This graph is a calibration plot which relates conductivity and conversion, and is prepared by
taking three and more points and plot. Taking more than three points are preferable to increase the
relevancy of linearity. For this case, five points are selected

Experimental procedures

1. Prepare the following solutions:

 1 liter of sodium hydroxide 0.05 M

 1 liter of sodium acetate 0.05 M

2. Determine the conductivity for each conversion value by mixing the following solutions.

i. 0% conversion: Take 400 ml 0.05 M NaOH from the stock solution and read
conductivity

ii. 25% conversion: Take 300 ml of 0.05 M NaOH and 100 ml of 0.05 M Na (Ac)
from the stock solutions, mix them up and read conductivity of the solution.
 iii. 50% conversion: Take 200 ml of 0.05 M NaOH and 200 ml of 0.05 M of Na (Ac)
from the stock solutions, mix them up and read conductivity of the solution.

iv. 75% conversion: Take 100 ml of 0.05 M NaOH and 300 ml of 0.05 M Na (Ac)
from the stock solution, mix them up and read conductivity of the solution.

v. 100% conversion: Take 400 ml of 0.05 M Na (Ac) from the stock solution and
read conductivity it.

Results:

 Record all the results in appropriate table

 Plot calibration curve of conductivity vs conversion and develop mathematical equation
relates conductivity and conversion.

Experiment 2: Experimental determination of steady state CSTR conversion

Objective
To determine the conversion achieved in the reaction between ethyl acetate and sodium hydroxide
in a CSTR operated at 25oC

Experimental Procedures

1. Preparation reagent solutions

 Prepare 1 litre of 0.05M ethyl acetate solution

 Prepare 1 litre of 0.05M sodium hydroxide solution
2. Start the QRC unit.
3. Select the type of reactor to be used. QRCAC in this case is used.
4. Press the START button and enter in the new window the name of the file that will contain
data.
5. Set the desired working temperature: 25ºC.
6. Place the products outlet stainless steel tube as low as possible (its height can be regulated
by unscrewing the brass nut) so that the product can be easily discharged without stop.
7. Set the same flow for both reagents.
 8. Record the conductivity at the moment when the reaction mixture “touches” the
conductivity cell.
9. When the reactant level reaches the stirrer’s blades, start the stirring system.
10. Keep the system, working for 1 hour.
11. Stop the system.
12. Measure the conductivity at every minute.
Calculations and Results
 Record all the results in appropriate table
 Convert conductivity to conversion using calibration curve plotted in experiment 1.
 Plot conversion vs time graph
 Find steady state conversion
 Calculate the space time (residence time) and fed rate using design equation of CSTR.
Discussion
Discuss on the results obtained
Conclusion
Based on results from experiment, draw your conclusion for this experiment
Experiment 3: Determination of effect of feed flow rate on the conversion in a
Continuous Stirred Tank Reactor (CSTR)
Objective
The objective of this experiment is to determine the conversion achieved by varying feed rate in
to the CSTR reactor.
Elements required
QRC unit with thermostat bath, balance, sodium hydroxide, ethyl acetate, distil water, volumetric
flask, measuring cylinder, beaker, portable conductivity meter
Experiment procedures
1. Prepare reagent solutions
 Prepare 1 litre of 0.05M ethyl acetate solution
 Prepare 1 litre of 0.05M sodium hydroxide solution
2. Start the QRC unit.
3. Select the type of reactor to be used. QRCAC in this case is used.
 4. Press the START button and enter in the new window the name of the file that will contain
data.
5. Set the desired working temperature: 25ºC.
6. Place the products outlet stainless steel tube as low as possible (its height can be regulated
by unscrewing the brass nut) so that the product can be easily discharged without stop.
7. Set the new but the same flow rate (30rpm) for both reagents.
8. Record the conductivity at the moment when the reaction mixture “touches” the
conductivity cell.
9. When the reactant level reaches the stirrer’s blades, start the stirring system.
10. Keep the system, working until reagents completely flow in to the reactor vessel.
11. Stop the system when all reagents flow in.
12. Measure the conductivity at the product outlet.
13. Repeat the experiment at feed rate of (50 rpm).
14. Make sure that the working temperature is maintained constant(at 25oC) for all
experiments
Results
 Record all the results in appropriate table
 Plot calibration graph of conductivity vs. conversion
 Plot a graph of conversion vs. time.
 Plot a graph of conversion vs. (flow rate) residence time
Discussion
Discuss the effect of flow rate on the conversion.
Conclusion
Based on the experimental results taken, draw some conclusions to this experiment

Experiment 5: Effect three equal size CSTR reactors arranged in series on conversion
Objective
To determine the basic hydrolysis of the ethyl acetate with the three reactors in a continuous
operation configuration
Theory
The size of all reactors are equal (V1 = V2 = V3 = V) which are known. The volumetric flow rate
of reactant/product mixture (𝜐0) is approximately taken to be the same for each reactor in the chain
for the steady state operation. Therefore, in this case, the space times in all sectors are equal
theoretically ( 𝜏1 = 𝜏2 = 𝜏3 = 𝜏)

Material balance for reactor 1

𝐶𝐴0 = 𝐶𝐴1 + (−𝑟𝐴 )𝑉/𝜐0 = 𝐶𝐴1 + (−𝑟𝐴 )𝜏
𝑉
Where 𝜏 = 𝜐 = ℎ𝑜𝑙𝑑𝑖𝑛𝑔 𝑜𝑟 𝑠𝑝𝑎𝑐𝑒 𝑡𝑖𝑚𝑒 𝑓𝑜𝑟 𝑒𝑎𝑐ℎ 𝑟𝑒𝑎𝑐𝑡𝑜𝑟
0

For first–order reaction

−𝑟𝐴 = 𝑘𝐶𝐴1 𝐶𝐵1
Since it is equi-molar, 𝐶𝐴1 = 𝐶𝐵1
−𝑟𝐴 = 𝑘𝐶𝐴1 𝐶𝐵1 = 𝑘𝐶𝐴1 2
𝐶𝐴0 = 𝐶𝐴1 + (𝑘𝐶𝐴1 2 )𝜏
𝐶𝐴0 − 𝐶𝐴1
𝜏=
𝑘𝐶𝐴1 2
Where 𝐶𝐴1 = 𝐶𝐴1 (1 − 𝑋𝐴1 )
Material balance for reactor 2
𝐶𝐴1 = 𝐶𝐴2 + (𝑘𝐶𝐴2 2 )𝜏
𝐶𝐴1 − 𝐶𝐴2
𝜏=
𝑘𝐶𝐴2 2
Where 𝐶𝐴2 = 𝐶𝐴0 (1 − 𝑋𝐴2 )
Material balance for reactor 3
𝐶𝐴2 = 𝐶𝐴3 + (𝑘𝐶𝐴3 2 )𝜏
𝐶𝐴2 − 𝐶𝐴3
𝜏=
𝑘𝐶𝐴3 2
 Where 𝐶𝐴3 = 𝐶𝐴0 (1 − 𝑋𝐴3 )

Total holding time/space time (𝜏𝑡 ) is the summation of all individual equal space times
𝜏𝑡 = 𝜏 + 𝜏 + 𝜏 = 3𝜏
Experimental Procedures
1. Preparation of reagent solutions
 Prepare 1 litre of ethyl acetate 0.05M solution
 Prepare 1 litre of sodium hydroxide 0.05M solution
2. Switch on the QRC unit.
3. Select the type of reactor to be used. QRSC in this case.
4. Press START and introduce in the new window the name of the file that will contain the
data.
5. Introduce the ethyl acetate and sodium hydroxide solutions in the corresponding reagent
tanks.
6. Switch on the thermostatization system and set a working temperature of 25ºC.
7. Adjust the volume of each reactor by placing the outlet pipe at the proper height (the height
of the stainless steel pipe can be adjusted by unscrewing the brass nut).
8. Set the reagent pumps to the desired flow manually and switch on the pumps (they will be
ready to be used).
9. Record on a table the different conductivity values obtained when the product reaches the
collector of the conductivity cell.
10. Switch off the system and clean it.

Results

 Record all the results in appropriate table

 Plot calibration graph of conductivity vs conversion
 Determine the exit conversions of each reactor?
 Calculate space time for each identical reactors?
Discussion
Discuss on conversion build up and space time.
Conclusion
Based on the experimental results taken, draw some conclusions to this experiment.