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ChE 391: Chemical Engineering Laboratory I

Title of Experiment
(Experiment No. 8) (Sequence No. 3)

Date of Experiment:

(Regular/Make-up)

Regular

Date of Report Submission:


02/02/2012
(Any revision sought: Yes/No
If yes, state reasons for make-up:

(Regular/Make-up)

Regular

Group No.:
Batch:
1. Smriti Agrawal
2. Mounica Bodapudi
3. Lavanya
4. Nidhi Rajwania

Name of TA:

If make-up, state reasons:

19/01/2012
-

6
Thursday
Y9587
Y9175
Y9368
Y9306

Shilpi Saxena

Marks: ______________

I/C
Prof. P. K. Bhattacharya
Dr. Sri Sivakumar

Department of Chemical Engineering


Indian Institute of Technology Kanpur

Content
1.
2.
3.
4.
5.
6.
7.
8.
9.

Introduction
Objective
Theory
Keywords
Procedure
Observation
Calculation
Discussion
Error analysis

Page no.
3
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3
6
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Continuous Stirred Tank Reactor


Introduction
In a continuous-flow stirred-tank reactor (CSTR), reactants and
products are continuously added and withdrawn. The low driving
force makes possible better control of rapid exothermic and
endothermic reactions. Analysis of a CSTR helps in determining
the kinetics of a chemical reaction, i.e. rate law of the reaction.
Depending on the conversion, selectivity and yield required,
various reaction variables
such as temperature, concentration of the reactants etc. can be
controlled with the proper knowledge of the rate law. The CSTR
configuration is widely used in industrial applications and in
wastewater treatment units (i.e. activated sludge reactors).

OBJECTIVE
To determine the reaction rate of the saponification reaction
at ambient conditions and determine the reaction rate
constant for it
To verify the order of the reaction

Keywords
CSTR, reaction rate constant, order of reaction

Relevant Reaction
NaOH + CH3COOC2H5

CH3COONa + C2H5OH

Theory and Formulae


Residence time is expressed as and =VR/VO, min, where
VR = Reactor volume (volume of fluid in the reactor), in litres, and
VO =Volumetric feed rate (Feed rate of Reactant A + Reactant B),
in LPM.
The design equation for the mixed flow reactor at steady state is:
=VR/VO = CAO*XA/ (-rA) = (CAO- CA)/ (-rA)
XA and rA are evaluated at exit stream conditions, which are the
same as the conditions within the reactor in a perfectly mixed
CSTR. [1]
3

For a second order reaction:


A+B

C+D

With CAO = CBO and under constant volume condition rate (for a
second order reaction) can be
represented as
-rA = -dCA/dt = KCA2
=VR/VO = CAO*XA/ (-rA) = (CAO- CA)/ (-rA) =(CAO- CA)/ KCA2
(1)
Degree of conversion,
XA = (CAO- CA)/CAO
(2)
and
rate of reaction,
-rA = CAO*XA/ , g mol/ L min
(3)
the rate constant,
K = (CAO- CA)/ CA2, L/g mol min
(4)
For nth order reaction,
-rA =K CAn
log(-rA) = log K + n*logCA
The order of the reaction, n, can be obtained from a plot of log (rA) vs. log CA, that yields a straight line with slope = n, and
intercept (at CA = 1 or at log CA = 0) shall give the value of log(K).
Also, a plot of vs. XA/(1-XA)2 shall yield a straight line for an
assumed second order reaction with slope = 1/(KC AO). From this
slope, rate constant K can be obtained. [2]

APPARATUS REQUIRED
1) Electricity supply: single phase, 220 VAC, 50 Hz, 5-15 Amp
socket with earth connection
2) Distilled water (to prepare solution)
3) Drain required
4) 5 conical flasks
5) Measuring cylinder
6) 2 stopwatches
7) Burette

8)

Chemicals:
NaOH pellets
N/10 HCl
Ethyl acetate
Indicator(phenolphthalein)

Quantity:
100 g
100 ml
200 ml
few drops

DESCRIPTION OF THE EXPERIMENTAL SET UP


The set-up has two sump tanks to which the NaOH and
CH3COOC2H5 solutions are fed. The reactant solutions from these
sump tanks are pumped to two overhead storage tanks. The
reactants are supplied to the CSTR from these storage tanks and
their flow rates are controlled by Rotameters. There is a stirrer in
the CSTR for proper mixing. Samples for analysis are collected
from the top outlet of the CSTR. The samples are analyzed by
titration with NaOH solution.
The simplified flow sheet for the experimental set up is :

EXPERIMENTAL PROCEDURE
1) Firstly, the reactant solutions to be used for the experiment
were prepared.
20 L of 0.1N NaOH solution by dissolving 80gm NaOH in 20L
water and
20 L of 0.1N CH3COOC2H5 solution by mixing 200.24 ml
CH3COOC2H5 in 20L water.
2) The respective tanks were filled with these solutions and the
motor was switched on to fill them into their respective overhead
tanks.
3) Equal volumetric flow rates of both NaOH and CH 3COOC2H5
were fed into the CSTR. The flow rates of the streams were
measured with the Rotameter.
4) When the liquid in the reactor reached a certain level (nearly
3/4th) it started overflowing and the volume of liquid inside it
became constant. It was at this instance that the stirrer of the
CSTR was switched on.
5) Next, the heater, provided on the set-up, was switched on and
a desired temperature was set on its digital controller.
6) An experimental measurement of the flow rate was made by
collecting the product stream in a measuring cylinder for a certain
time period, measured on a stopwatch. This flow rate was used to
make an estimate of the residence time for the reactor.
7) Once the desired temperature was reached, it was assured
that the reactor had reached steady state by allowing it to run
undisturbed for 10 minutes or the calculated residence time,
whichever was greater.

8) A 10ml sample of the product was taken from the outlet of the
CSTR and was added to20ml 0.1N HCl kept in a flask.
9) The solution left in the flask was titrated with 0.1N NaOH
which was added drop by drop from a burette, using
phenolphthalein as indicator. The volume of NaOH (V NaOH) required
for the complete neutralization of the leftover HCl was noted.
10) The steps 3 to 9 were repeated for different values of
temperatures and different flow rates for each value of
temperature.
11)The experiment was conducted at 40,50 and 600oC and the
flow rates used for each temperature were 7.5,12.5 and 15 LPH,
as measured by the Rotameter.

Observations:
T=16 oC
Rotamet
er
reading

Volume
in ml

t,Reside
nce time
in min

Initia Final
l
NaO
NaOH H

Differe
nce

57

Time in Flow
s
rate
in
l/min
14.44
0.24

7.5

9.08

10.0

37

6.10

0.36

5.9

12.5

44

5.72

0.461
5

5.41

41
58
63
55.4
3.0
20.0
37.0
55.0
72.5
1.0
18.0

58
75.2
80
72.4
19.5
36.5
55.0
72.5
89.5
18.0
35.3

17
17.2
17
17
16.5
16.5
18.0
17.5
17.0
17.0
17.3

Volume
in ml

Time in Flow
s
rate

Initia
l

Final
NaO

Differe
nce

T=28 oC
Rotamet
er

t,
Residen

reading
7.5

35

7.40

in
l/min
0.28

ce time
in min
7.58

NaOH H

10.0

47

7.00

0.40

5.33

12.5

51

6.37

0.48

4.47

Rotamet
er
reading

Volume
in ml

t,Reside
nce time
in min

Initia Final
l
NaO
NaOH H

Differe
nce

7.5

79

Time in Flow
s
rate
in
l/min
18.87
0.25

8.56

10.0

48

7.56

0.38

5.64

12.5

39

5.56

0.42

5.12

52.0
20.0
38.2
58.0
22.0
55.8
74.6
30.0
14.0
32.0
51.0
69.0

18.6
18.2
18.6
18.8
18.8
18.8
19.0
19.0
18.0
19.0
18.0
18.4

35.3
53.2
2.0
19.8
37.8
55.8
3.0
21.2
39.4
57.2
16.2
34.0

53.2
71.0
19.8
37.8
55.8
74.2
21.2
39.4
57.2
75.0
34.0
52.0

17.9
17.8
17.8
18.0
18.0
18.4
18.2
18.2
17.8
17.8
17.8
18.0

T=38 oC

70.6
38.2
56.8
76.8
38.8
74.6
93.6
49.0
32.0
51.0
69.0
87.4

SAMPLE CALCULATION
T= 150C
Flow rate = 7.5 LPH

Outlet Volumetric Flow Rate = 57 ml / 14.44 sec = 14.210 LPH


Residence Time = 2.15 li / 14.210 LPH = 9.078 min
Volume of HCl added = 20ml
Moles of HCl added = 20ml X 0.1006M = 2.012 mMol
NaOH from the burette consumed = 17.0 ml
Moles of NaOH consumed = 17.0ml X 0.1016M = 1.7272 mMol
Now, moles of NaOH in the sample taken = 2.012-1.7272 mMol = 0.2848
mMol
Therefore, exit concentration of NaOH, CA = 0.2848/10 = 0.028 M
Moreover, CA0=0.1*7.5/(7.5+7.5)=0.050 M

XA = (CAO- CA)/CAO = 0.43


XA/(1-XA)2 =1.33

In this manner,
and

is calculated for different cases and a graph between

is plotted for each temperature to obtain the K value from its

slope as discussed in the theory above.

CASE 1
T= 150C
NaO
H
(LPH
)
7.5
10.0
12.5

ETOAc (mi
(LPH)
n)
9.07
7.5 8
5.90
10.0
0
5.41
12.5
0

Buerette
Reading
(ml)
17.0

NaOH
consumed
(mMol)
1.73

CAO (M)

CA (M)

XA

0.050

0.028

0.43

1.32

16.5

1.68

0.050

0.033

0.33

0.73

17.0

1.73

0.050

0.028

0.43

1.32

`Residence Time vs

Slope= 1/K

= 2.197

K= 9.103
CASE 2
T= 28 0C
NaO
H
(LPH
)
7.5
10.0
12.5

ETOAc
(LPH)
7.5
10.0
12.5

(mi
n)
7.5
8
5.3
3
4.4
7

Buerette
Reading
(ml)

NaOH
consumed
(mMol)

18.4

1.81

CAO (M)

CA (M)

XA

0.050

0.014

0.71

8.79

18.2

1.86

0.050

0.016

0.67

6.35

17.8

1.83

0.050

0.020

0.59

3.58

Residence Time vs

10

CASE 3
T= 360C
NaO
H
(LPH
)
7.5
10.0
12.5

ETOAc
(LPH)
7.5
10.0
12.5

(mi
n)
8.5
6
5.6
4
5.1
2

Buerette
Reading
(ml)
18.8

NaOH
consumed
(mMol)
1.89

CAO (M)

CA (M)

XA

0.050

0.012

0.75

18.8

1.91

0.050

0.010

0.80

18.0

1.91

0.050

0.010

0.80

Residence Time vs

11

12.64
19.16
19.16

Slope= 1.729 = 1/K

K= 11.567
T
288
299
309

-1/T
-0.00347
-0.00334
-0.00324

K
9.103
10.219
11.567

Ln(K)
2.2308
2.3242
2.4481

Slope = Ea/R = 1013.8


Ea = 8428.74 Joules

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RESULT
(A)
Temperature

Value of K

(Kelvin)
288
299
309

9.103
10.219
11.567

(B) Ea = 8428.74 Joules


Discussion
The graph shows an increasing linear trend which is in accordance
with the equation.
Arrhenius eqn:

Logarithmic form:

Error analysis
1. Slope of the first graph comes out to be ve . This can be
due to the following errors:
Time lag in which solution was taken and the
titration was conducted. So, the reaction
continued and concentrations changed.
Titration was erroneous. The pink solution stability
and first appearance, or presence of some water
in the flask.
Dropper used may be of other chemical.

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