1.

Abstract

This experiment was carried out to observe and know more details about Continuous Stirred
Tank Reactor (CSTR) 40 L on how its operate and to carry out the saponification reaction
between NaOH and Et(Ac) in CSTR. Other than that, this experiment was carried out to
determine the effect of the residence time onto the reaction extent of conversion and also to
determine the reaction rate constant. Before the experiment started, we ensured the general start
up procedure was carried out properly so that the reactor will run without any disturbance. After
the start up process was done, we began the experiment by opening valves V5 and V10 to obtain
the highest possible flow rate into the reactor. This experiment is done by varying the residence
time by manipulating the flow rate of the system. For this experiment, the feed flow rates were
adjusted for 100 ml/min, 150 ml/min, 200 ml/min, 250 ml/min and 300 ml/min. For each flow
rate, 50 mL sample was taken to be used in the back titration procedure. The 50 mL samples
were titrated with NaOH for saponification reaction. The amounts of NaOH titrated were
recorded. A few calculations had been conducted to determine the conversion, residence time and
concentration of NaOH. Based on the result achieved, graph of conversion VS time was plotted
to study the effect of residence time on the conversion.
From the result, the percentage of conversion of NaOH is increasing with the increase of
residence time. When the residence is 50 min, the conversion is 95.6%. Then as the total flow
rate provided for the system is increased, the residence time is decreasing and that makes the
conversion of NaOH to decrease as well. When the residence time is 16.667 min, the conversion
is decreasing to 90.4%. The lower flow rate gives a higher residence time and helps increasing
the conversion of the reaction in the CSTR.

1.2

Introduction

In chemical engineering, a chemical reactor design deals with multiple aspects of chemical
engineering and chemical reactions. As designers they will always ensure that the reaction held
in the reactor proceeds with the highest efficiency towards the desired output product and
producing the highest yield of product that required the least amount of money to purchase and
operate (Schmidt & Lanny, 1998). Every industrial chemical process is designed to produce
economically a desired product from a variety of starting materials through a succession of
treatment steps. The raw materials undergo a number of physical treatment steps to put them in
the form in which they can be reacted chemically then pass through the reactor.
Chemical reactors are vessels that contain chemical reaction. Different types of chemical,
biological and physical processes take place in reactors and the degree of mixing and residence
time in reactors affect the degree of completion of reactions within the reactor (Dey, Herzog, &
Srinivasan, 2007). The design of a chemical reactor deals with multiple aspects of chemical
engineering. Chemical engineers design reactors to maximize the 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 (Nanda & M.Pharm, 2008).
Continuous stirred tank reactor is a type of reactor that consists of a well-stirred tank where there
is a continuous flow of reacting material and from which the reacted material passes
continuously. This is due to that vessels are squat in shape or known as cylindrical vessels that
good in stirring of their contents or otherwise there will be a bulk streaming of the fluid occur in
between inlet and outlet and much of the volume of the vessels would be essentially dead space
(K.G.Denbigh & J.C.R.Turner, 1984).
Stirring is the most important characteristic of continuous stirred tank reactor. The most
appropriate approximation to estimate its performance is based on the assumption that its content
are perfectly mixed (K.G.Denbigh & J.C.R.Turner, 1984).
Apart from that, continuous stirredtank reactors are open systems where material is free to enter
or exit the system that operate on a steadystate basis and the conditions in the reactor does not
2

change with time. Reactants are continuously introduced into the reactor, while products are
continuously removed. CSTRs are very well mixed, so the contents have relatively uniform
properties such as temperature, density, etc. throughout. Also, conditions in the reactor's exit
stream are the same as those inside the tank. Continuous stirredtank reactors are most
commonly used in industrial processing, primarily in homogeneous liquidphase flow reactions,
where constant agitation is required where they may be used in series or in a parallel.
One of the great advantages of the continuous stirred reactor is that ease of temperature control
apart from simplicity of construction. The reagents entering the first vessel plunge immediately
into a large volume of partially reacted fluid and because of the stirring, local hot spots does not
occur. Besides that, continuous stirred reactor also provides a very large area of cooling surface.
It is also easy to clean this reactor because of the openness of the construction. This makes it
easy to clean the internal surfaces and this is important in the case of reactions where there is a
tendency for solid matter to be deposited.
CSTR that used in the experiment (model: BP 143) is designed for students experiments on
chemical reaction in liquid phase which is under adiabatic and isothermal conditions. The CSTR
consists of two tanks of solutions and one reactor that consists of jacketed reaction fitted in the
agitated and condenser. The unit comes complete with vessels for raw materials and products,
feed pumps and thermostat that set at 500C. The reactor is modelled in order to perform the
saponification reaction where the reaction is occur between sodium hydroxide, NaOH and ethyl
acetate, Et(Ac). The saponification process between this compounds produced sodium acetate in
a batch and the continuous stirred tank reactor evaluate the rate data needed to design a
production scale reactor.

1.3

Aims

There are several objectives for this experiment:

i.
ii.
iii.

1.4

To carry out saponification reaction between NaOH and Et(Ac) in a CSTR 40L
To determine the effect of residence time onto the reaction extent of conversion
To determine the reaction rate constant

Theory
4

Saponification is the hydrolysis of ethyl acetate to produce sodium acetate and ethyl alcohol
using NaOH. The stoichiometric representation of saponification reaction between ethyl acetate
and sodium hydroxide is given by:
NaOH + CH3COOC2H5CH3COONa + C2H5OH
This is an irreversible reaction with overall second-order and first order with respect to each
reactant. The rate expression is represented by:
-rNaOH = -rEtOAc = kCNaOHCEtOAc
In this reaction, hydroxyl ions are consumed and acetate ions are produced. Since hydroxyl ions
are more conductive than the acetate ions, a decrease in the conductivity is observed as the
reaction progresses. Thus, the change in conductivity is used to monitor the alkaline hydrolysis
of ethyl acetate.
The rate of reaction is defined as the change in the number of molecules of reacting species per
unit volume per unit time. It is also defined to be proportional to the concentration of reacting
species raised to a certain power called the order of reaction. It is usually taken as the rate at
which the reactant disappear or the rate at which the product is formed. The rate at which the
reactant a is disappearing is proportional to its concentration at any instance:
Rate (r) = k (a - x)
Where,
k = rate constant
The concept of rate of reaction is very important in evaluating chemical reacting systems. It is
the core factor in the development of performance models to stimulate reactor functional
parameters.

Conversion is an improved way of quantifying exactly how far has the reaction moved, or how
many moles of products are formed for every mole of A has consumed. Conversion X A is the
number of moles of A that have reacted per mole of A fed to the system. As seen below:
X A=

mole s of A reacted
moles of A fed

The residence-time distribution (RTD) of a reactor is a characteristic of the mixing that occurs in
the chemical reactor. This omission is reflected in the RTD since there is no axial mixing in a
plug flow reactor. The residence time is determined experimentally by injecting an inert
chemical, molecule or atom called a tracer into the reactor at some time t = 0 and then the tracer
concentration, C is measured in the effluent stream as a function of time. The tracer should have
physical properties similar to those of the reacting mixture and be completely soluble in the
mixture. Besides that, it also should not adsorb on the walls or other surfaces in the reactor. In an
ideal plug-flow reactor, all the atoms of material leaving the reactor have been inside it for
exactly the same amount of time. The time the atoms have spent in the reactor is called the
residence time of the atoms in the reactor.

1.5

Apparatus
1.
2.
3.
4.
5.

Continuous stirred tank reactor. Model: BP 143

50 mL burette
200 mL beaker
Conical flask
Solution :
i.
Sodium hydroxide, NaOH (0.1M)
ii.
Ethyl acetate, Et (Ac) (0.1M)
iii.
Deionised water
iv.
Phenolphthalein
6. Conductivity probe
7. 100 mL measuring cylinder.

Figure 1 Continous Stirred Tank Reactor (Model:BP 143)

1.6

Procedure

1.6.1 General start-up Procedures:

1. The following solution were prepared:

i40L of sodium hydroxide, NaOH (0.1 M)
ii40 L of ethyl acetate, Et (Ac) (0.1M)
iii1 L of hydrochloric acid, HCl (0.25M) , for quenching.
2. All valves were initially closed.
3. The feed vessels were charged as follows:
iThe charge port caps for vessels B1 and B2 were opened.
iiThe NaOH solution was carefully poured into vessel B1 and Et (Ac) solution was

4.
5.
6.
7.
8.

poured into vessel B2.

iiiThe charge port caps for both vessels were closed.
The power for control panel was turned on.
Sufficient water in thermostat T1 was checked. Refill as necessary.
The overflow tube was adjusted to give a working volume of 10L in the reactor R1.
Valves V2, V3, V3, V7, V8 and V11 were opened.
The unit was ready for experiment.

1.6.2 General shut-down Procedures:

1. The cooling water valve V13 was kept open to allow the cooling water to continue
flowing.
2. Pumps P1 and pumps P2 were switched off. Stirrer M1 was switched off.
3. The thermostat T1 was switched off. The liquid in the reaction vessel R1 was let to cool
down to room temperature.
4. Cooling water V13 was closed.
5. Valves V2, V3, V7, and V8 were closed. Valves V4, V9 and V12 were opened to drain
any liquid from the unit.
6. The power for control panel was turned off.

1.6.3 Preparation of Calibration Curve for Conversion vs Conductivity:

1. The following solution were prepared:
i1 L of sodium hydroxide, NaOH (0.1M)
ii1 L of sodium acetate , Et (Ac) (0.1M)
iii1 L of deionised water, H2O.
2. The conductivity and NaoH concentration for each valu were determined by mixing the
following solution into 100 mL of deionised water.
i0% conversion
: 100 mL NaOH
ii25% cinversion
: 75 mL NaOH + 25 mL Et (Ac)
iii50% conversion
: 50 mL NaOH + 50 mL Et (Ac)
iv75% conversion
: 23 mL NaOH + 75 mL Et (Ac)
v100% conversion
: 100 mL Et (Ac)
8

1.6.4 Back Titration Procedures for Manual Conversion Determination:

1. A burette was filled up with 0.1 M NaOH solution.
2. 10 mL of 0.25 M HCl was measured in a flask.
3. A 50 mL sample was obtained from the experiment and immediate the sample was added
to the HCl in the flask to quench the saponification reaction.
4. A few drops of pH indicator were added into the mixture.
5. The mixture was titrated with NaOH solution from the burette until the mixture was
neutralized. The amount of NaOH titrated was recorded.
1.6.5 Effect of Residence Time of The Reaction in a CSTR:
1. The general start-up procedures was performed.
2. Pump 1 and pump 2 were switched on and valves V5 and V10 were opened to obtain the
highest possible flow rate into the reactor.
3. The reactor was filled up with both of the solution until it is njust bout to overflow.
4. Valves V5 and V10 were readjusted to give a flow rate of about 0.1 L/min. the flow rate
for both valves must be same. The flow rate were recorded into a data.
5. The stirrer M1 was switched on and the speed was set about 200 rpm.
6. The conductivity value at Q1 was started monitoring until id does not change over time.
This is to ensure that the reactor has reached steady state.
7. The steady state conductivity value was recorded and the concentration of NaOH and
extent of conversion in the reactor was found out from the calibration curve.
8. Sampling valve V12 was opened and 100mL of sample was collected. It directly proceed
with the back titration procedures to manually determine the concentration of NaOH in
the reactor and extent of conversion.
9. The experiments was repeated (steps 5-9) for different residence times by adjusting the
feed flow rate of NaOH and Et(Ac) to about 0.15, 0.20, 0.25, and 0.30 L/min. the flow
rate for both must be same.

1.7 Results
Reactor Volume: 10L
Concentration of NaOH in feed vessel: 0.1M
Concentration of Et(Ac) in feed vessel: 0.1M
Flow Rate of NaOH (mL/min)
Flow Rate of Et(Ac) (mL/min)

100
100

150
150

200
200

250
250

300
300

Volume of NaOH titrated (mL)

Residence Time, (min)

23.9
50

23.5
33.333

23.4
25

23.0
20

22.6
16.667

Volume of Unreacted Quenching

9.56

9.4

9.36

9.2

9.04

HCL (mL)
Volume of HCL reacted with

0.44

0.6

0.64

0.8

0.96

NaOH (mL)
Conversion of NaOH in the

95.6

94

93.6

92

90.4

reactor, X (%)
Rate Constant, k x103 (m-1s-1)
Rate of reaction, -rA x10-3 (ms-1)
Conductivity (ms/cm)

0.198
0.958
2.43

0.157
1.41
2.32

0.183
1.87
2.28

0.144
2.30
2.31

0.118
2.71
2.37

10

Conversion VS Residence Time

98
96
94
Conversion (%)

92
90
88
86
15

20

25

30

35

40

45

Residence Time (min)

Graph 1 Conversion VS Residence Time

11

50

55

1.8

Calculations

1.8.1 Sample calculation:

Calculation for total flowrate of 0.2 L /min
Known quantities

Volume of sample,

= 10

Reactor Volume
Vs

Concentration of NaOH in the feed vessel, =

C NaOH

50 mL
0.1 mol/ L

Volume of HCl for quenching,

V HCl

Concentration of HCl in standard solution, =

C HCl

10 mL

0.25 mol /L

Volume of titrated NaOH,

V1

Concentration of NaOH used for titration, =

C NaOH

23.9 mL
0.1 mol/ L

i.

C NaOH

ii.

C NaOH

Concentration of NaOH entering the reactor,

=

Volume of unreacted quenching HCl,

1
C
2 NaOH

1
(0.1)
2

0.05 mol /L

V2

V2

C NaOH
V 1
C HCl
s

12

0.1
23.9
0.25

9.56 mL

V3

iii.

Volume of HCl reacted with NaOH in sample,

V3

V HCl V 2

109.56

0.44

iv.

Moles of HCl reacted with NaOH in sample,

n1

v.

Moles of unreacted NaOH in sample,

( C HCl V 3 ) /1000

0.25 0.44 /1000

0.00011 mol

n2
=

n1

0.00011 mol

Concentration of unreacted NaOH in the reactor,

C NaOH

vii.

n1

n2

vi.

Conversion of NaOH in the reactor,

C NaOH

n2 /V s 1000

0.00052/50 1000

0.0022 mol/ L

13

viii.

C NaOH
100
C NaOH
0

100
(1 0.0022
0.05 )

95.6

Residence time,

ix.

V CSTR
F0

10
0.20

50 min

Reaction rate constant, k

( C A C A )
0

C 2A

x.

Rate of reaction,

( 0.050.0022 )
2
50 0.0022

0.198 10 M min

r A

r A

1.9

Discussion
14

kC 2A

0.198 103 0.00222

9.58 104 mol / L. min

In this experiment, saponification reaction between NaOH and Et(Ac) were carried out in the
plug flow reactor. These two solutions react together in the plug flow reactor to complete
saponification reaction. This experiment was conducted to achieve three objectives which is to
carry out saponification reaction between NaOH and Et(Ac) in a CSTR 40L, to determine the
effect of residence time onto the reaction extent of conversion and lastly, to determine the
reaction rate constant. Based on the result achieved, graph of conversion vs residence time was
plotted. Continuous stirred reactor (CSTR) 40L was used in this experiment. The feed which is
NaOH and Et(Ac) enter at one end of a cylindrical tube and leaves product from the end of
cylindrical tube. At the end of the experiment, we are able to calculate the reaction rate constant
by using specific formula and can determine the effect of residence time on the conversion in the
plug flow reactor.
The CSTR is normally run at steady state and is usually operated to be quite well mixed. The
conductivity value in the CSTR is assumed as the same anywhere in the reactor. From the
experiment, the conductivity of the reactant decreases as the conversion decreases. The 95.6%
conversion gives a conductivity value of 2.43 mS/cm. The conversion which is 90.4% gives the
lowest conductivity value of 2.37 mS/cm. The decrease in the ionic activity of a solution in term
of its capacity to transmit current is the reason why the value of conductivity is decreasing. The
conductivity increases as the concentration of ions increases when the electric current is
transported by the ions. Thus, the ionic activity is higher in the higher conversion of NaOH. This
is possibly because of the agitation in CSTR which making the ionic activity still going on in the
solution even after the conversion.
Besides that, based on the result, when flowrate is low, the conversion value is higher. This is due
to that when flowrate is low, it helps to escalate the reaction more in the CSTR as conversion
value is higher when flowrate is lower. The reactants have a lot of time to make contact with
each other before exiting the outlet when the flow rate is low. Thus, the lower the flow rate will
helps the conversion to increase the contact between the reactant. As for the reaction rate of the
reaction,-rA from the result achieved, it shows that rate of reaction is increased as the rate
constant, k is decreasing.

15

Saponification reaction of ethyl acetate (Et(Ac)) and sodium hydroxide (NaOH) have been
carried out to study the effect of conversion on residence time. The reaction is carried out using
equimolar feeds of Et(Ac) and NaOH solutions with the same initial concentrations to ensures
that both concentrations are similar throughout the reaction. The flow rate is then varied from 0.1
L/min to 3.0 L/min for both feeds in order to give variation in the residence time. Then, the
residence time is determined and calculated from this equation:
=
Residence Time,

Reactor volume ( L ) ,V
L
Total flow rate
, v0
min

( )

Conversion VS Residence Time

98
96
94
Conversion (%)

92
90
88
86
10 20 30 40 50 60
Residence Time (min)

Graph 1 Conversion VS Residence Time

The results obtained from the experiment are shown in the graph above. From the graph, we can
see that the conversion is increase proportionally with residence time where the percentage of
conversion of NaOH is increasing with the increase of residence time. The highest conversion of
NaOH shown when the residence is 50 min, where the conversion is 95.6%. Then as the total
flow rate provided for the system is increased, the residence time is decreased and that makes the
conversion of NaOH to decrease as well. When the residence time is 16.6667 min, the
conversion is decreasing to 90.4% which is the lowest conversion obtained from this experiment.
16

Residence time was defined as the length of time the fluid would stay in the reactor while
conversion is a property that shows how much of the reaction has taken place. The longer the
reactants would stay in the reactor, more products would be formed. The data mainly shows that
the longer the residence time, the percentage of conversion increases and this obey the expected
result where the longer time left in the reactor, more reaction occurs between NaOH and Et(Ac).

17

1.10

Conclusion

As a conclusion, the objective of this experiment is successfully achieved. Saponification

reaction between NaOH and Et(Ac) was obtained in the reactor. By using a continuous stirred
tank reactor, these two substances were flowed into the reactor and mixed together for a certain
period of time to complete the saponification process. Both reaction rate constant and effect of
residence time on the conversion was also determined. Graph of residence time vs conversion
was plotted based on the result obtained. The relationship between residence time and conversion
was successfully studied and graphed in graph 1, residence time VS conversion. By analysing the
graph, it can be concluded that, conversion is increase proportionally with residence time where
it shows that the longer the residence time, the greater the percentage of conversion. This is due
to the longer the reactants stay in the reactor, more products would be formed. From the data
obtained also it can be concluded that the reaction rate constant is depend on the flow rate in the
continuous stirred tank reactor where, as the flow rate decrease, the reaction rate constant
increased.

18

1.11 Recommendations
In my point of view, there are a few recommendations and precautions that have to be considered
during the experiments in order to get an accurate value and readings of data. Firstly, before
carry out the experiment, make sure that the reactor does not have any leaks and valve is closed
and opened as needed, controlled the valve carefully and slowly when adjusting the flow rate to
obtain 0.10 L/min. This is to make sure that the flow rate is stabilized and the experiment will
run smoothly. Other than that, before started the experiment, make sure that all valves are
properly open to carry out the experiment. Make sure to perform general start-up and shut down
procedure so that the equipment will run smoothly and is in the best shape to operate.
Besides that, each flow rates of the feed also should be constantly monitored so that it remains
constant throughout the reaction to prevent any changes that can affect the result. It is
recommended to run several trials on the reactor to get more accurate results by taking the
average value from each different molar rate.
In order to avoid from any contaminants into the sample, the titration should be done as soon as
possible after taking the sample. Be extra careful when carry out the titration where the titration
should be stop as soon as the indicator turn into pale pink color. The excess drop of NaOH from
titration can effect on the solution color hence effect the calculations and the result.

19

1.12

Reference

Dey, D., Herzog, A., & Srinivasan, V. (2007). Tracer Studies In A Plug Flow Reactor. 143.
Fogler, H. S. (2014). Elements of Chemical Reaction Engineering (4th ed.). London:
Pearson Education.
Green, D., & Perry, R. (1987). Perry's Chemical Engineer's Handbook. McGraw Hill.
K.G.Denbigh, & J.C.R.Turner. (1984). Chemical Reactor Theory: An Introduction.
Briston: Cambridge University Press.
Levenspiel, O. (1999). Chemical Reaction Engineering. John Wiley.
Mann, U. (2009). Principles Of Chemical Reactor Analysis And Design (2nd ed.). New
Jersey: A John Wiley & Sons, Inc.
Nanda, S., & M.Pharm. (2008). Reactors and Fundamentals of Reactors Design for
Chemical Reaction . PHARMACEUTICAL ENGINEERING , 1-22.
Schmidt, & Lanny, D. (1998). The Engineering of Chemical Reactions. New York:
Oxford University Press.
Smith, J. (1981). Chemical Engineer Kinetics. McGraw Hill.
Winterbottom, J., & King, M. (1999). Reactor Design for Chemical Engineers. United
Kingdom: Stanley Thornes Ltd.

20

1.13 Appendix

21

22

Advantages of CSTR:

It is possible to maintain this reactor at isothermal conditions for high heat of reaction.

It is quite easy to maintain good temperature control with this reactor.

Due to large volume, it provides a long residence time.

It also has low cost of construction.

Disadvantages:

It is not recommended for high pressure reactions because of cost consideration. For high
pressure reactions it requires complex sealing arrangements for the agitator which
increase the initial as well as maintenance cost.

Conversion of these reactors is low due to this they are not preferred.

These reactors are not suited for high heat effect since availability of both heat transfer
coefficient and heat transfer per unit area is low.

Applications:

These reactors are normally employed on commercial scale mainly for liquid phase
reaction at low or medium pressure.
23

It is commonly used in industrial processing of homogeneous reactions (only liquid

phase) and usually used in series

UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA
CHEMICAL ENGINEERING LABORATORY iii (CHE 574)
NAME
: NUR IZZATI BINTI AHMAD TARHIZI (2014233914)
GROUP
: EH220 4A
EXPERIM
: CONTINUOUS STIRRED TANK REACTOR 40L
ENT
DATE
: 29 MARCH 2016
PROG/CO
: EH220
DE
SUBMIT
: MADAM NURHASHIMAH BINTI ALIAS
TO
MISS SITI KHATIJAH BINTI JAMALUDIN
N
Title
Allocated
Marks
o
Marks (%)
1 Abstract
5
2 Introduction
5
3 Objectives
5
4 Theory
5
5 Procedures/Methodology
10
6 Apparatus
5
7 Results
10
8 Calculation
10
9 Discussion
20
10 Conclusion
10
11 Recommendations
5
12 References
5
24

13 Appendices
TOTAL

5
100

Remarks:

Checked by:

Rechecked by:

Date:

Date:

25