UNIVERSITI TEKNOLOGI MARA

FAKULTY OF CHEMICAL ENGINEERING

PROCESS ENGINEERING LABORATORY 2 (CPE553)
NAME

MOHAMAD AZRUL SOFI BIN MOHD TAHAR

(2013982991)
EH2414 (GROUP1)
LAB 3 : CSTR 40L

GROUP
:
EXPERIM
:
ENT
DATE
: 2 OCTOBER 2015
PROG/CO
: EH241
DE
SUBMIT
: MDM LIM YING PEI
TO
N
Title
o
1 Abstract
2 Introduction
3 Objectives
4 Theory
5 Procedures/Methodology
6 Apparatus
7 Results
8 Calculation
9 Discussion
10 Conclusion
11 Recommendations
12 References
13 Appendices
TOTAL

Allocated
Marks (%)
5
5
5
5
10
5
10
10
20
10
5
5
5
100

Marks

Remarks:

Checked by:

Rechecked by:

Date:

Date:

ABSTRACT
The conversion of reactant into product is very important in the chemical process. Reactors is
used to convert the reactant into product. Reactors are very important in chemical processes.
Furthermore the design of the reactors will determine the result of the product and it is very
important to the success of the production. Meanwhile, in this experiment sodium hydroxide and
ethyl acetate react in continuous stirred tank reactor. They are fed into the reactor at equimolar
flowrate. The conversion achieve at different retention time is determined by measured the
conductivity value of outlet stream. At the lowest flowrate, the retention time is highest. So the
result shows that the conversion is increased as the residence time increases.
Our objectives in this experiment are to carry out the saponification reaction between sodium
hydroxide and ethyl acetate in plug flow reactor, to determine the reaction rate constant and the
rate of reaction of the saponification process. First of all, the equipment is set up before started
the experiment. From the result, the rate of reaction and the value of reaction rate constant is
calculated. At 0.10 L/min flowrate is 60.00 M-1s-1, for the 0.15 L/min reaction rate constant is
34.28 M-1s-1, for the 0.20 L/min reaction rate constant is 31.94 M-1s-1, for the 0.25 L/min reaction
rate constant is 29.44 M-1s-1, and for the 0.30 L/min reaction rate constant is 27.00 M-1s-1.
However, we also can to determine the rate of reaction for this process. After that, we are
plotted a graph of conversion factor against residence time. From the graph plotted, the
conversion factor is directly proportional to the residence time. The conversion factor increases
so the residence time also increases.

INTRODUCTION
In a continuous-flow stirred-tank reactor (CSTR), reactants and products are continuously
added and withdrawn. In practice, mechanical or hydraulic agitation is required to achieve
uniform composition and temperature, a choice strongly influenced by process considerations.
The CSTR is the idealized opposite of the well-stirred batch and tubular plug-flow reactors.
Analysis of selected combinations of these reactor types can be useful in quantitatively
evaluating more complex gas-, liquid-, and solid-flow behaviors.
Because the compositions of mixtures leaving a CSTR are those within the reactor, the reaction
driving forces, usually the reactant concentrations, are necessarily low. Therefore, except for
reaction orders zero- and negative, a CSTR requires the largest volume of the reactor types to
obtain desired conversions. However, the low driving force makes possible better control of
rapid exothermic and endothermic reactions. When high conversions of reactants are needed,
several CSTRs in series can be used. Equally good results can be obtained by dividing a single
vessel into compartments while minimizing back-mixing and short-circuiting. The larger the
number of CSTR stages, the closer the performance approaches that of a tubular plug-flow
reactor.
Continuous-flow stirred-tank reactors in series are simpler and easier to design for isothermal
operation than are tubular reactors. Reactions with narrow operating temperature ranges or
those requiring close control of reactant concentrations for optimum selectivity benefit from
series arrangements. If severe heat-transfer requirements are imposed, heating or cooling
zones can be incorporated within or external to the CSTR. For example, impellers or centrally
mounted draft tubes circulate liquid upward, then downward through vertical heat-exchanger
tubes. In a similar fashion, reactor contents can be recycled through external heat exchangers.
By studying the saponification reaction of ethyl acetate and sodium hydroxide to form
sodium acetate in a batch and in a continuous stirred tank reactor, we can evaluate the rate
data needed to design a production scale reactor.
A stirred tank reactor (STR) may be operated either as a batch reactor or as a steady
state flow reactor (CSTR). The key or main feature of this reactor is that mixing is complete so
that properties such as temperature and concentration of the reaction mixture are uniform in all

parts of the vessel. Material balance of a general chemical reaction described below.The
conservation principle requires that the mass of species A in an element of reactor volume dV
obeys the following statement:
(Rate of A into volume element) - (rate of A out of volume element) + (rate of A produced within
volume element) = (rate of A accumulated within vol. element)

THEORY
A mathematical model to predict ideal transient concentration in a CSTR is developed by using
principles of a simple material balance. From the material balance, the ideal residence time
distribution is derived. In order to create the experimental model, a negative step input method
is utilized. This process is used instead of the positive step method due to the difficulty of
keeping an initial tracer concentration in the feed stream.

General Mole Balance Equation

Assumptions

1) Steady state therefore

2) Well mixed therefore rA is the same throughout the reactor

Rearranging the generation

In terms of conversion

The reaction to be studied is the saponification reaction of ethyl acetate Et(Ac) and sodium
hydroxide NaOH. Since this is a second order of reaction, the rate of reaction depends on both
of these reactants. The reaction will be carried out using equimolar feeds of both the reactants
with same initial concentrations. The reaction equation is;
NaOH + Et (Ac) Na(Ac) + EtOH
or
A

C +

For a second order equimolar reaction with the same initial concentration (CAO = CBo), the rate
law is;

r a=k C A C B=k C 2A

r A=

V CSTR
FA 0 X

Thus, the volume of the reactor is ;

Ao C A
C

F0
F X
V CSTR = A 0 2 =
k CA

For equimolar feed rate, the reaction constant is ;

Ao C A
C

k =
The residence time of a chemical reactor or vessel is a description of the time that different fluid
elements spend inside the reactor is given by;

Residencetime , =

V CSTR
F0

This equation gives the concentration of species i in the outlet stream at any time t. The
residence-time distribution function, E(t), is given:

By substituting this equation

into above equation and solving, we obtain the following expression which describes the
amount of time a tracer spends in the reactor:

The ideal cumulative concentration distribution, F(t), is also practical when evaluating the
residence time distribution, providing the percent of material that has a RTD of time t or less

By definition, E(t) = -dF(t)/dt for a negative step input. Therefore, by differentiating Eq. 6, we
obtain the residence-time distribution function for a non-ideal CSTR.

OBJECTIVES
1. To carry out a saponification reaction between sodium hydroxide,NaOH and ethyl
acetate Et(Ac) in a CSTR
2. To determine the reaction rate constant of sodium hydroxide,NaOH and ethyl acetate
Et(Ac)
3. To determine the effect of residence time on the conversion in a CSTR.

APPARATUS
1. A laboratory scale of Continuous Stirred Tank Reactor 40litre
2. A conductivity meter
3. 50 mL Beakers
4. 250 mL Conical Flasks
5. A burette
6. A retort stand.
7. Sodium Hydroxide
8. Ethyl acetate
9. Hydrochloric acid
10. Phenolphtalein
11. Deionized water

PROCEDURE
a) Preparation of Calibration Curve
1. 1 liter of sodium acetate, Na(Ac) 0.1M and 1 liter of sodium hydroxide, NaOH 0.1M are
prepared.
2. The following list of solution are mixed together into 100mL of deionised water to
determine the conductivity and NaOH concentration for each conversion values.
a) 0% conversion
: 100mL NaOH
b) 25% conversion : 75mL NaOH + 25mL Na(Ac)
c) 50% conversion : 50mL NaOH + 50mL Na(Ac)
d) 75% conversion : 25mL NaOH + 75mL Na(Ac)
e) 100%conversion : 100 mL Na(Ac)
3. The value of conductivity for each conversion is recorded.
4. The graph of the calibration curve of conductivity versus conversion is plotted. The slope
and y-axis intercept is determined.

b) Back Titration Procedures for manual Conversion Determination

1. 0.1M NaOH solution is filled into a burette.
2. 0.25M HCl is measured at 10mL in a flask.
3. From the experiment, a 50mL sample is obtained and immediately added to the HCl in
the flask to quench the saponification reaction.
4. Then, a few drops of phenolphtalein were fadded into the mixture
5. The mixture is titrated with NaOH solution from the burette until the mixture was
neutralized. The amount of NaOH titrated recorded.

c) Effect of Residence Time on the Reaction in a CSTR

1. General start-up procedures is performed.
2. Pumps P1 and P2 are switched on simulteneously and the valves V5 and V10 are
opened to obtain the hishest possible flow rate into reactor.
3. The NaOH and Et(Ac) solutions were allowed to enter the reactor until it is just about to
overflow.
4. For the valves V5 and V10 are readjusted to give a flowrate about 0.1L/min.
5. The stirrer M1 were switched on and the speed were setted to about 200 rpm.
6. The conductivity value at (QI-401) is started to monitor until they did not change over the
time to ensure that the reactor reached the steady state.
7. The sampling valve V12 is opened and a 50mL sample collected. A back titration
procedure is carried out to manually determine the concentration of NaOH in the reactor
and extent of conversion.
8. The experiment is repeated from step 4 to 7 for different residence time by increasing
the feed flow rates of NaOH and Et (Ac) to about 0.15, 0.20, 0.25 and 0.30 ml/min. Make
sure that both was the same.

RESULTS
Reactor volume = 4L
Concentration of NaOH in feed vessel = 0.1M
Concentration of Et(Ac) in feed vessel = 0.1M

Temperature (C)
Flowrate of
NaOH, (mL/min)
Flowrate of
Et(Ac), (mL/min)

30.1

29.9

30.5

30.6

31.0

100

149

205

253

298

102

151

203

252

301

202

300

408

505

599

4.0

4.6

5.2

5.3

5.4

19.80

13.33

9.80

7.92

6.68

94.00

88.00

82.00

78.00

76.00

Total flow rate of

solutions, F0
(mL/min)
Conductivity,
(S/cm)
Residence time,
(min)
Conversion, X
(%)

Table 1 Effect of residence time tubular flow reactor

Solution mixtures
Conversion
%

0.1 M NaOH, mL

0.1 M Et(Ac), mL

H2O, mL

Concentration

Conductivity,

of NaO (M)

mS/cm

100

100

0.0500

7.4600

25

75

25

100

0.0375

1.9240

50

50

50

100

0.0250

0.7080

75

25

75

100

0.0125

0.0141

100

100

100

100

0.0000

0.0021

Table 2 Preparation of calibration curve

Graph of conversion X vs. temperature of reactor

31.2
31
30.8
30.6
30.4
30.2
Temperature
30
29.8
29.6
29.4
29.2
70

75

80

85

Conversion X

90

95

100

Graph of Conversion, X versus Residence time

25
20
15
Residence time

10
5
0
70

75

80

85

90

95

100

Conversion, X

DISCUSSION
To determine the conversion of the reaction of between sodium hydroxide (NaOH) and ethyl
acetate (Et(Ac)) at certain value of conductivity, the calibration curve is plotted. From the
calibration curve, the conductivity of the sodium hydroxide solution varied linearly with
concentration of sodium hydroxide. When the molar concentration of NaOH decreases, the
conductivity is decrease. Different value of conductivity will be given by both of them when
mixture of different of moles is used. Sodium hydroxide is used as a reactant while sodium
acetate is produced as a product from this mixture. Ethyl acetate and ethanol are not electric
conductor from that we can measured the concentration of unreacted NaOH that remains
solution that relate to conversion by used the conductivity of the mixture measurements.
Volumetric flowrate is affect to the residence time so this experiment is conduct in different
flowrate. When the volumetric flowrate is increase so the conversion is increases too.
Residence time is time that the fluid elements spend within reactor. More conversion reactant is
occurred when the time of the reactant spend in is longer. So the concentration of the reactant
will decrease and the concentration of product will increase. Fluid entering the reactor at time t

will exit the reactor at time t + , where is the residence time of the reactor. The velocity of fluid
moving inside the reactor is low at the low flowrate. The reactant will spend more time within the
reactor when the velocity of fluid is lower.
Furthermore, the electronic device on the reactor is used to determine the conversion based on
the conductivity value. Back titration procedure is used to determine the conversion manually.
From the calculation, the value of conversion that obtained is increase when the volumetric
flowrate decrease. This proved the theory form the calibration curve from the first experiment.
The experiment is successful conducted.
Unfortunately there are no calculations in this experiment due to the mistake with the instrument
itself during the experiment is conducted. For the titration part not done successful because of
the error in the reading of the samples obtained from the instrument.

CONCLUSION
From the experiment, the different volumetric flowrate is used and caused different conversion
in the reaction between NaOH and Et(Ac) which done in a continuous stirred tank reactor. As
the flowrate decreases, the reaction rate constant, k for the second order of reaction is
decreases. In order to achieve the objectives of the experiment, the continuous stirred tank
reactor is used. From the experiment, all the purposes are met and the results are recorded.
From the results, it shows that as for each flow rates decrease from 0.100 L/min to 0.298 L/min,
the conversion of sodium hydroxide decrease from 94.0 % to 76.0 %. Meanwhile for the graph
of conversion of sodium hydroxide versus residence time is plotted. It is shows that the
conversion of sodium hydroxide is directly proportional to the residence time. As the conversion
increase, the residence time increase as well. As all the purposes of this experiment is
achieved, this experiment is considered as a successful.

RECOMMENDATION
1. The general start-up must be done first to check the machine functining well.
2. Rinsed the burette with sodium hydroxide after rinsed using the distilled water to prevent
error.
3. Please make sure the solution that filled in the tank is correct solution and the amount is
also correct. Different substance reacts differently and lack of substance can damage
the apparatus.
4. Eye protection must be wear at all the time when handle with the sodium hydroxide.
Because sodium hydroxide is corrosive to flesh and can cause blindness.
5. The device needs to be well maintenance in order to avoid it from malfunctioning during
the experiment period like the one we are having in our session.
6. To get a better result, only one person is needed to take care of the opening and closing
of the valve and other person take care of the pump. This is because some valve
needed to be opened or closed simultaneously.

REFERENCES
1. Fogler, H. S., Elements of Chemical Reaction Engineering, 2

nd

edition, Prentice Hall,

1992, New Jersey.

2. Gilbert F.Froment and Kenneth B.Bischoff., Chemical Reactor Analysis and DesignJohn
Wiley & Sons, 2nd Edition, 1990.
3. Continuous Stirred Tank Reactor model, http://en.wikipedia.org/wiki/plug-flow-reactormodel, accessed in October 2011.
4. Levenspiel O. Chemical Reaction Engineering. John Wiley & Sons, NewYork, third
edition, 1999.
5. http://www.scribd.com/doc/74373588/cstr

APPENDICES

Time (min)

Weight of permeates (g)

Membrane 1

1
2
3
4
5
6
7
8
9
10

Membrane 2

Membrane 3

Membrane 4