Mycstr40l (Repaired)

1
TABLE CONTENTS

NO TITLE PAGE
1.0 Abstract 2
2.0 Introduction 3
3.0 Aims/Objectives 3
4.0 Theory 4-8
5.0 Apparatus 9
6.0 Experimental Procedure 10-12
7.0 Results 13-15
8.0 Sample Calculations 16-25
9.0 Discussion 26
10.0 Conclusion 27
11.0 Recommendation 27
12.0 References 28
13.0 Appendices 29
2

ABSTRACT

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 the
apparatus will run without any disturbance. After the methodology of 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. For this experiment, the feed flow rates were adjusted in increasing order. For
each flow rate, 50 mL sample was taken to be used in the back titration procedure. In back
titration, the 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. Two graphs were plotted. From the calibration curve
we can see that the conductivity inversely proportional to the conversion. This shows that there is
a negative slope obtained from the line which is -0.114. This slope can be seen through the trend
line. The y axis intercept when x=0, where the value for conductivity is 9.748 where the second
graph, the conversion is inversely propotional to the residence time. As the residence time
increase, the conversion will decrease. This showed that the objectives were successfully
achieved. More details can be viewed in the result.

3

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and withdrawn.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.
The continuous stirred tank reactor (model BP 143) unit is suitable for student experiments on
continuous chemical reactions. The unit consists of jacketed reaction fitted in the agitator and
condenser. The unit comes complete with vessels for raw materials and product, feed pumps, and
thermostat.

OBJECTIVE

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

4

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.

Ideal stirred-tank reactor
A stirred- tank reactor (STR) may be operated either as a batch reactor or as a steady-
state flow reactor. The reactor can completely mix where the temperature and concentration of
the reaction mixture are uniform in all parts of the vessel.
The conservation principle requires that the mass of species A in an element of reactor
volume V obey the following statement:

Rate of A Rate of A Rate of A Rate of A
Into _ out of + produced = accumulated ...(1)
volume volume within volume within volume
element element element element

Batch stirred-tank reactor (BSTR)
In batch reactions, there are no feeds or exit streams and therefore equation (1) can be simplified
into:
Rate of A Rate of A
produced = accumulated (2)
within volume within volume
element element

The rate of reaction of component A is defined as:

reaction by
A
A
dt
dN
V
r
|
.
|
\
|
=
1
.(3)

5

When A is a reaction product, the rate is positive while when reactant is consumed, the rate is
negative. Rearranging equation (3);
( )
dt
dX
N V r
A
AO A
= .(4)

Integrate equation (4);

( )
}

=
V r
dX
N t
A
A
AO
(5)
where t is the time required to achieve a conversion X
A
for either isothermal or non-isothermal
operation.

Steady state mixed flow reactor

Figure 1: Components of mixed flow

From figure 1, if F
A0
= v
0
C
A0
is the molar feed rate of the component A to the reactor, then
considering the reactor as a whole we have,
Input of A (moles/time) = F
A0
(1 X
A0
) = F
A0

Output of A (moles/time) = F
A
= F
A0
(1 X
A
)
Disappearance of A by reaction (moles/time) = (-r
A
)V
Replacing equation (1) with mathematical formula above,

F
A0
X
A
= (-r
A
)V ...(6)

Which on arranging, will form the performance equation for mixed flow reactors,

A
A
AO AO
r
X
C F
V
A
= =
t

6

A
A AO
AO
AO
O
r
X C
F
VC
v
V
s
= = = =
1
t (7)

In mixed flow reactors, X
A
= X
AF
and C
A
= C
AF
. In a constant density system,
X
A
= 1 (C
A
/C
A0
)

The performance equation can be rewritten in terms of concentration, or

) (
A AO
A AO
A
A
AO
r C
C C
r
X
F
V
=
) (
A
A AO
r
X C
v
V
= = t (8)
Reaction Rate in Mixed Reactor

First order reaction (Unimolecular Type)
A Product
Suppose the reaction rate is the following type:
A
A
A
kC
dt
dC
r = = ..(9)
kt
C
C
A
A
=
0
ln .(10)

Plot of ln(C
A
/C
A0
) versus t will produce a straight line with a slope equals to rate constant, k

Figure 2: Plot of ln(C
A
/C
A0
) versus time

-ln C
A0
C
A

t
Slope = k
7

Irreversible Second-order Reaction (Bimolecular Type)
A + B Products
The rate equation can be written as:

B A
B A
A
C kC
dt
dC
dt
dC
r = = = .(11)

Plot of ln (C
B
/C
A
) versus t (time) will produce a straight line with slope equals (C
B0
C
A0
)k.

Figure 3 : Plot of ln (C
B
/C
A
) versus t

For second order reaction with equal initial concentrations of A and B, the rate equation can be
written based on only one component:

2 2 2
) 1 (
A AO A
A
A
X kC kC
dt
dC
r = = = .(12)

A plot of 1 / C
A
versus t will produce a straight line with slope equals to k.

-ln C
B
C
A

t
slope = (C
B0
-C
A0
)k
Intercept = ln C
B0
/C
A0

8

Figure 4: Plot of 1/C
A
versus t

1/C
A

t
slope = k
Intercept = 1/C
A0

9

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,H
2
O
- Burette
- Retort stand
- Conical flask
- pH indicator
- Measuring cylinder

10

PROCEDURE

General Start-Up Procedures

1. Prepare the following solutions:
a) 20 L of sodium hydroxide, NaOH (0.1M)
b) 20 L of ethyl acetate, Et(Ac) (0.1M)
c) 1 L of hydrochloric acid, HCL (0.25M), for quenching

2. Ensure that all valves are initially closed.

3. Charge the feed vessels as follows:
a) Open the charge port caps for vessels B1 and B2.
b) Carefully pour the NaOH solution into vessel B1 and the Et(Ac) solution into vessel B2.
c) Close the charge port caps for both vessels.

4. Turn on the power for the control panel.

5. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.

6. Open cooling water valve V13 and let the cooling water flow through the condenser W1.
(Only for Experiment 2)

7. Adjust the overflow tube to give a working volume of 10 L in the reactor R1.

8. Open valves V2, V3, V7, V8 and V11.

9. The unit is now ready for experiment.

General Shut-Down Procedures
11

1. Keep the cooling water valve V13 open to allow the cooling water to continue flowing.

2. Switch off both pumps P1 and P2. Switch off stirrer M1.

3. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool down to room
temperature.

4. Close cooling water valve V13.

5. Close valves V2, V3, V7 and V8. Open valves V4, V9 and V12 to drain any liquid from
the unit.

6. Turn off the power for the control panel.

EXPERIMENT PROCEDURES

1. Perform the general start-up procedures as in Section 4.1.

2. Switch on both pumps P1 and P2 simultaneously and open valves V5 and V10 to obtain
the highest possible flow rate into the reactor.

3. Let the reactor fill up with both the solution until it is just about to overflow.

4. Readjust the valves V5 and V10 to give a flow rate of about 0.1 L/min. Make sure that
both flow rates are the same. Record the flow rate.

5. Switch on the stirrer M1 and set the speed to about 200 rpm.

6. Start monitoring the conductivity value at QI-401until it does not change over time. This is
12

to ensure that the reactor has reached steady state.

7. Record the steady state conductivity value and find the concentration of NaOH in the
reactor and extent of conversion from the calibration curve.

8. Open sampling valve V12 and collect a 50 mL sample. Carry out a back titration
procedure to manually determine the concentration of NaOH in the reactor and extent of
conversion (Section 5.2).

9. Repeat the experiment (steps 5 to 9) for different residence times by adjusting the feed
flow rates of NaOH and Et(Ac) to about 0.15, 0.20, 0.25 and 0.30 L/min. Make sure that
both flow rates are the same.

13

RESULT

TABLE FOR PREPARATION OF CALIBRATION CURVE

y = -0.114x + 9.748
R = 0.7334
-4
-2
0
2
4
6
8
10
12
14
0 20 40 60 80 100 120
c
o
n
d
u
c
t
i
v
i
t
y

(
M
s
/
c
m
)

conversion (%)
conductivity vs conversion
Conversion

Solution
mixture

Concentration Conductivity

0.1 M NaOH 0.1 M Et(Ac) H
2
O of NaOH (Ms/cm)
0% 100ml - 100ml 0.0500
13.18
25% 75ml 25ml 100ml 0.0375
3.33
50% 50ml 50ml 100ml 0.0250
2.54
75% 25ml 75ml 100ml 0.0125
1.20
100% - 100ml 100ml 0.0000
0.00
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TABLE FOR EXPERIMENT 1.

Reactor volume: 10 L
Concentration of NaOH in feed vessel = 0.1 M
Concentration of Et( Ac) in feed vessel = 0.1 M

Flow
rate of
NaOH
(ml/min)
Flow
rate of
Et, Ac
(ml/min)
Total
flow
rate of
solution
F
o

(ml/min)
Residence
Time,
(min)
Conductivity
(ms/cm)
Exit
concentration
Of NaOH,
C
NaOH
(M)
Conversion,
X (%)
0.10 0.10 0.20 50.0 1.29 0.0072 85.6
0.15 0.15 0.30 33.3 1.27 0.0060 88.0
0.20 0.20 0.40 25.0 1.26 0.0056 88.8
0.25 0.25 0.50 20.0 1.25 0.0050 90.0
0.30 0.30 0.60 18.7 1.24 0.0028 94.4

Data collected from the back-titration process
No

Flow rate (mL/ min) Volume of 0.25 M
HCl (mL)
Volume of 0.10 M
NaOH(mL)
NaOH Et (Ac)
1 0.10 0.10 10.0 21.40
2 0.15 0.15 10.0 22.00
3 0.20 0.20 10.0 22.20
4 0.25 0.25 10.0 22.50
5 0.30 0.30 10.0 23.60

15

85.6
88
88.8
90
y = -0.1404x + 92.604
R = 0.9871
85
85.5
86
86.5
87
87.5
88
88.5
89
89.5
90
90.5
0 10 20 30 40 50 60
c
o
n
v
e
r
s
i
o
n

(
%
)

residence time (min)
conversion vs residence time
16

CALCULATION
1)

Known quantities
Volume of sample,
=
Concentration of NaOH in the feed vessel,
=
Volume of HCl for quenching,
=
Concentration of HCl in standard solution,
=
Volume of titrated NaOH,
=
Concentration of NaOH used for titration,
=

i. Concentration of NaOH entering the reactor,

=

ii. Volume of unreacted quenching HCl,

=

iii. Volume of HCl reacted with NaOH in sample,

=
=

iv. Moles of HCl reacted with NaOH in sample,
=
(
)
=
=

v. Moles of unreacted NaOH in sample,

=

vi. Concentration of unreacted NaOH in the reactor,

17

=
=

vii. Conversion of NaOH in the reactor,
=
(
)
=
(
)
=

viii. Residence time,
=

=

ix. Reaction rate constant,
=
(

x. Rate of reaction,

18

2)

Known quantities
Volume of sample,
=
=
=
=
=
=


=


=


=
=

=
(
)
=
=


=


19

=
=

=
(
)
=
(
)
=

=

=

=
(


20

3)

Known quantities
Volume of sample,
=
=
=
=
=
=


=


=


=
=

=
(
)
=
=


=


21

=
=

=
(
)
=
(
)
=

=

=

=
(


22

4)

Known quantities
Volume of sample,
=
=
=
=
=
=


=


=


=
=

=
(
)
=
=


=


23

=
=

=
(
)
=
(
)
=

=

=

=
(


24

5)

Known quantities
Volume of sample,
=
=
=
=
=
=


=


=


=
=

=
(
)
=
=


=


25

=
=

=
(
)
=
(
)
=

=

=

=
(


26

DISCUSSION

This experiment was conducted to achieve three adjectives; 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. We plotted two graphs
from this experiment which are the graph of conductivity vs conversion and the graph of
conversion vs residence time.

In this experiment, firstly, we had prepared the calibration curve to see the relationship between
conductivity and conversion of NaOH. The 0ml, 25ml, 50ml, 75ml and 100ml of acetate was
added to the 100ml, 75ml, 50ml, 25ml and 0ml of NaOH respectively by mixing with 100ml
deionised water to get 0%, 25%, 50%, 75% and 100% conversion. From the calibration curve we
can see that the conductivity inversely proportional to the conversion. This shows that there is a
negative slope obtained from the line which is -0.114. This slope can be seen through the trend
line. The y axis intercept when x=0, where the value for conductivity is 9.748.

After that we had carry out a saponification reaction between NaOH and Et in a CSTR. Firstly,
we perfomed the general start-up procedure then P1 and P2 was switched on simultaneously and
V5 and V10 was opened to obtain the highest possible flow rate into the reactor. The V5 and
V10 was readjusted to get different flowrate of NaOH and Et. Then, we recorded the
conductivity when the reading has reached the steady state and the sample had taken for titration.
For the second graph, the conversion is inversely propotional to the residence time. As the
residence time increase, the conversion will decrease.

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.

27

CONCLUSION

This experiment was conducted to achieve three adjectives; 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. We plotted two graphs
from this experiment which are the calibration curve of conductivity vs conversion and the graph
of conversion vs residence time. From the calibration curve we can see that the conductivity
inversely proportional to the conversion. This shows that there is a negative slope obtained from
the line which is -0.114. This slope can be seen through the trend line. The y axis intercept when
x=0, where the value for conductivity is 9.748. For the second graph, the conversion is inversely
propotional to the residence time. As the residence time increase, the conversion will decrease.
From the calculation we can see that the rate reaction constant is increase as the flowrate is
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.
- Always plug in all cables into appropriate sockets before switching on the main power on
the control panel. Inspect all cables for any damage to avoid electrical shock.
- Make sure that the stirrer assembly is secured properly. Avoid excessive load to the
electrical motor to prevent damage.
- Inspect the unit, including tubing and fittings, periodically for leakage and worn out.
- 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.
- Use white tile to see light pink while do titration.
28

REFFERENCES

1. Chemical Reaction Engineering, Third Edition, Octave Levenspiel, 1999 John Wiley &
Sons
2. http://en.wikipedia.org/wiki/Continuous_stirred-tank_reactor
3. http://www.engin.umich.edu/~cre/asyLearn/bits/cstr/
4. http://www.solution.com.my/pdf/BP143(A4).pdf

29

APPENDICES

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