Abstract

In this experiment , the operation of saponificaton of NaOH and

Et(Ac) is carry out in Continuous Stirrer Tank Reactor (CSTR) 40 L. There
are three component

in this experiment to be measured which are

reaction rate, residence time and conversion of X. This experiment used

model BP 143 as the mechanism to run the reaction. The experiment start
to be measured by obtain adjustable flow rate which are 0.15, 0.20, 0.25
and 0.30. For each flow rate, 100 mL of the sample are collected at V12
that used in the back titration. Then, the stable conductivity is recorded
into a data for every 5min before collect the samples. In the back titration,
the samples that had been collected are titrated with NaOH for
saponification reaction until it change colour from colourless into light
pink. Then, the amount of NaOH titrated were recorded.After experiment
compeleted , the data obtain can be used to plot graph.The graph is used
to see the effect of residence time on conversion of X.The graph show the
residence time is inversely proportional to the conversion which do not
follow the theory due to some error occur in this experiment. . For the
reaction rate, the data show the decreasing over the period of conversion.
This also not follow the theory whereby as the conversion increase the
rate of reaction will increase.

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products are continuously added and withdrawn.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 plugflow reactors. Analysis of selected combinations of these reactor types can
be useful in quantitatively evaluating more complex gas-, liquid-, and
solid-flow behaviors.
Furthermore, the continuous stirred tank reactor (CSTR) which is
also known as vat-or back-mix reactor and this kind of model used to
estimate the key unit operation variables when using a continuous
agitated-tank reactor to reach a specified output. This reactor can be used
for all fluids, gases and slurries. In a perfectly mixed reactor, thus the
output composition is identical to the composition of the materials inside
the reactor which is a function of residence time and rate of reaction that
had been considered in this experiment.
The unit used in this experiment, which is SOLTEQ-QVF Continuous
Stirred Tank Reactor (Model: BP 143), The unit conducted a saponification
reaction by using ethyl acetate and sodium hydroxide . The model also
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 saponification process between th2
compounds produced sodium acetate in a batch and the continuous
stirred tank reactor evaluate the rate data needed to design a production
scale reactor.

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

Theory
Rate of Reaction and Rate Law
Rate of reaction is the number of mol A reacting per unit time per unit
volume.It also defined as the rate of disappearance of reactants or the
rate of formation of products. When a chemical reaction is said to occur, a
reactant (or several) diminishes and a product(or several) produced. This
is what constitutes a chemical reaction.
aA+ bB cC +dD

where A and B represent reactants while C and D represent products. In

this reaction, A and B is being diminished and C and D is being produced.
Rate of reaction, concerns itself with how fast the reactants diminish or

how fast the product is formed. Rate of reaction of each species

corresponds respectively to their stoichiometric coefficient. As such :
r A r B r C r D
=
= =
a
b
c d
The negative sign indicates reactants.
The Equation for rA is :
r A=k C A C B
Conversion
Using the equation shown in Equation 1.1 and taking species A as the
basis of calculation, the reaction expression can be divided through by the
stoichiometric coefficient of species A, in order to arrange the reaction
expression in the form:
a A+

b
a B

p
a P+

q
a Q

The expression has now put every quantity on a per mole of A basis.
A convenient way to quantity how far the reaction has progressed, or how
many moles of products are formed for every mole of A consumed; is to
define a parameter called conversion. The conversion XA is the number of
moles of A that have reacted per mole of A fed to the system.
X A=

moles of A reacted
moles o f A fed

To perform a mole balance on any system, the system boundaries must

first be specified. The volume enclosed by these boundaries is referred to
as the system volume. We shall perform a mole balance on species j in a

system volume, where species j represents the particular chemical species

of interest, such as water or NaOH.

Continuous Stirred Tank Reactors (CSTR)

CSTR runs at steady state with continuous flow of reactants and products;
the feed assumes a uniform composition throughout the reactor, exit
stream has the same composition as in the tank.

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

APPARATUS

Continuous stirred tank reaction (Model: BP143)

0.1M sodium hydroxide, NaOH
0.1M sodium acetate, Et(Ac)
0.25 hydrochloric acid, HCl
De-ionized water,H2O
Burette
Retort stand
Conical flask
pH indicator
Measuring cylinder

PROCEDURE
General Start-up Procedure
1 The following solutions were prepared:

i 40 L of sodium hydroxide, NaOH (0.1M)

ii 40 L of ethyl acetate, Et (Ac) (0.1M)
iii 1 L of hydrochloric acid, HCl (0.25M), for quenching
2 All valves were initially closed.
3 The feed vessels were charged as follows:
i The charge port caps for vessels B1 and B2 were opened.
ii The NaOH solution was carefully poured into vessel B1, and
the Et (Ac) solution was poured into vessel B2.
iii The charge port caps for both vessels were closed.
4 The power for the control panel was turned on.
5 Sufficient water in thermostat T1 was checked. Refill as necessary.
6 The overflow tube was adjusted to give a working volume of 10 L in
the reactor R1.
7 Valves V2, V3, V7, V8 and V11 were opened.
8 The unit was ready for experiment.
General shutdown procedure.
1 The cooling water valve V13 was kept open to allow the cooling
water to continue flowing.
2 Pumps P1 and pump 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 valve 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.

Preparation of Calibration Curve for Conversion vs. Conductivity

1 The following solutions were prepared:
i 1 L of sodium hydroxide, NaOH (0.10M)
ii 1 L of sodium acetate, Et (Ac) (0.10M)

iii 1 L of deionised water, H20

2 The conductivity and NaOH concentration for each value were
determined by mixing the following solutions into 100 mL of
deionised water:
i.
ii

0% conversion : 100 mL NaOH

25%
: 75 mL NaOH + 25 mL Et (Ac)

. conversion
iii 50%

: 50 mL NaOH + 50 mL Et (Ac)

. conversion
iv 75%

: 25 mL NaOH + 75 mL Et (Ac)

. conversion
v. 100%

: 100 mL Et (Ac)

conversion

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.

Result
Flow

Flow

Total

Q,Co

Nao

Conve

Resi

Reactio

Reactio

Tim

rate

rate

flow

nduc

rsion

denc

n rate

n rate

e(

of

of

rate

tivity

titrat

consta

min

NaO

of

(ms)

ed(M

time

nt k

et(ac

solut

l)

(L/mi

(L/mi

ion

n)
0.10

n)
0.10

V0
0.2

3.51

24.6

98.4

100

768.75

4.92 x

10

0.15

0.15

0.3

3.17

25.6

98.00

66.6

734.87

10 -4
7.35 x

15

0.20

0.20

0.4

2.83

26.0

96.00

67
50.0

240

10 -4
9.6 x

99.64

00
16.6

185.95

10 -4
8.8 x

99.64

67
16.6

7
160.99

10 -4
9.8 x

20
25

0.25
2.30

0.25
0.30

0.5
0.6

2,64
2.52

25.9
25.9

67

10

-4

TABLE 1

conversion X VS residence time

100
99
98
Conversion X

97
96
95
94
19.64

19.64

50
Residence time

Graph 1

66.667000000000002

100

Conversio
n
0
25%
50%
75%
`100%

Solution mixture
0.1M
0.1M

H20

NaoH
100ml

100m 0.0500

NaoH(Ac)
-

75 ml
50ml
25ml
-

25ml
50ml
75ml
100ml

Concentration Conductivity(ms

l
100ml
100ml
100ml
100ml
Table 2

of NaoH(M)

/cm)
10.7

0.0375
0.0250
0.0125
0.0000

9.7
7.5
5.6
4.0

conversion vs conversion X
30
25
f(x) = 0.22x + 1.25
R = 0.9

20
CONDUCTIVITY

15
10
5
0
0

20

40

60

CONVERSION X

Graph 2

80

100

120

SAMPLE CALCULATION:
F0 =0.1L/min
Known quantities:
Volume of sample, Vs = 50 mL
Concentration of NaOH in the feed vessel, CNaOH,f = 0.1 mol/L
Volume of HCL for quenching, VHCl,s = 10 mL
Concentration of HCl in standard solution, CHCls = 0.25 mol/L
Volume of titrated NaOH, V1= 9.8 mL
Concentration of NaOH used for titration, CNaOHs = 0.1 mol/L

i-

Concentration of NaOH that entering the reactor, CNaOH0.

CNaOHo = CNaOHf
= (0.1)
= 0.05 mol/L

ii-

Volume of unreacted quenching HCl,V2

V2 = (CNaOHs / CHCls) x V1

= (0.1/0.25) x 24.6
= 9.84 mL
iii-

Volume of HCl reacted with NaOHin sample, V3

V3 = VHCls V2
= 10 9.84
= 0.16

iv-

Moles of HCl reacted with NaOH in sample, n1

n1 = (CHCls x V3) / 1000
= 0.25 x 0.16/1000
= 0.00004 mol

v-

Moles of unreacted NaOH in sample, n2

n2 = n1
= 0.00004 mol

vi-

Concentration of unreacted NaOH in the reactor, CNaOH

CNaOH = n2/Vs x 1000
= 0.0004/50 x 1000
= 0.0008 mol/L

vii-

Conversion of NaOH in the reactor, X

X = (1- CNaOH / CNaOHo) x 100%
= (1 0.0008/0.05) x 100%
= 98.4 %

viii-

i
k

Residence time,
= VCSTR / Fo
= 10 / 0.10

Reaction rate constant, k

=

( C A C A )
0

C 2A
=

( 0.050.0008 )
2
100 0.OOO 8

ii
r A

Rate of reaction,

768.75 M min

r A
=

kC 2A

768.75 0.0008

4.92 104 mol / L. min

Discussion
This experiment was conducted to achieve three main adjectives
which are to carry out saponification reaction between NaOH and Et (Ac)
in a CSTR, to determine the effect of the residence time onto the reaction
extent of conversion and to determine the reaction rate constant.
From the data obtain from the experiment, a graph can be plotted to
achieve the objective. The first graph plotted to see the effect of
residence time towards reaction extent of conversion. The graph shows
decreasing conversion of X as the residence time increase. Residence time
can be defined as average amount of time that a particle spends in a
particular system. Its mean that the more time the particle spend in the
system the lesser conversion of X into product. It is suppose the result to
be the conversion X directly proportional to residence time. This is
because the more time the particle in the system the more potential
collision can occur among each particle to achieve activation energy.
Thus, more reactant can be converted into product.The reaction rate also
will increase as the conversion increase.
The second graph is plotted for calibration curve which is a method
general method for determining the concentration of a substance in an
unknown sample by comparing the unknown to a set of standard samples
of known concentration. Based on the graph,it show that the conversion is
increase as the conductivity increase. This shows that there is a positive
slope obtained from the line which is 0.2151.
Saponification is the process to make a soap. Saponification is a
continuous reaction. In this experiment, the reaction of saponification is
quench with hydrochloride acid to stop the reaction. The reaction rapidly

react in increasing of temperature. Back titration is done to investigate if

the reaction is stop.

Conclusion
The objective of this experiment

is to determine

the effect of

residence time on the reaction extent of conversion.Based on the theory,

the result

should be conversion and residence time was directly

proportional.But in this experiment, the result slightly different from the

theory due to some error that occur in this experiment. For the reaction
rate, the data show the decreasing over the period of conversion. This not
follow the theory whereby as the conversion increase the rate of reaction
will increase.

RECOMMENDATION
-The samples need to immediately quench with hydrochloride acid (HCl) to
stop the reaction. The reaction still occurred as long as no quenching is
done. The recommendation is store the HCl near to the sample so it can
immediately quench.
-Immediately stop the titration after the colour turns light pink. The long
titration may cause error to the calculation which the flow rate of NaOH
could be more than the initial.

-During titration, the indicator must be put to HCl then followed by

sample.

REFERENCES
-Fogler, H.S (2006). Elements of Chemical Reaction Engineering (3rd
Edition). Prentice Hall.
-Levenspiel, O. (1999). Chemical Reaction Engineering (3rd Edition). John
Wiley.
-

Continuous

Stirrer

Tank

Reactor

(CSTR)

(Retrieved

http://www.konferenslund.se/p/L16.pdf on 18th October 2013)

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