NATIONAL INSTITUTE OF TECHNOLOGY, TIRUCHIRAPPALLI 15

DEPARTMENT OF CHEMICAL ENGINEERING

CHEMICAL REACTION ENGINEERING LABORATORY MANUAL
ADIABATIC REACTOR
Aim:
To study the effect of temperature on the rate of reaction between hydrogen peroxide and
sodium thiosulphate under adiabatic reaction conditions and to determine the activation energy
of the reaction.
Theory:
The effect of temperature on the reaction mixture consisting of hydrogen peroxide and
sodium thiosulphate when the reaction is carried out under adiabatic conditions, it can be
observed and correlation with the reaction rate is given. As the exothermic reaction proceeds,
the temperature increases and becomes constant. The rate of the reaction and temperature are
correlated to various temperatures.
Where
T
F
Final Temperature (C)
T
0
Initial Temperature (C)
K Rate constant
C
A0
Initial concentration (moles/ litre)
A graph is drawn between lnA Vs.1/T and the slope is equated to -E/R.
Procedure:
Take 30 ml of hydrogen peroxide in a beaker and dilute it into 300 ml by using distilled
water and pour it into the reactor, 300 ml of sodium thiosulphate solution will also be added in
the reactor. Due to exothermic reaction, the temperature of reaction mixture starts increasing,
the rise in temperature is noted at different time intervals as the reaction proceeds.
Tabulation:
Time
(sec)
Temperature
(C)
dT/dt (Ts T)
2
1/(T+273)
(k
-1
)
A ln A
Department of Chemical Engineering 2
( )
0 F
RT E
A0
2
f
T T
KC
dt
dT
T T
1 e

Model Graph:
Model Calculation:
1) t =
2) T =
3)
dt
dT
4) (T
f
T)
2
5)
2
f T) (T
1
dt
dT
A

6) lnA =
7)
273) (T
1
+
=
8) Slope= -E/R
9) E=
Result and Inferences:
--------------
Department of Chemical Engineering
Slope = -E/R
1/T (k
-1
)
x 0
l
n
A
TC
Time (s)
3
BATCH REACTOR -1
Aim:
To verify the order and to determine the rate constants for the reaction between equimolar
quantity of NaOH and ethyl acetate in a batch reactor.
Reaction:
NaOH + CH
3
COOC
2
H
5
CH
3
COONa + C
2
H
5
OH
Theory:
For a second order reaction, the rate of reaction is as follows
2
A
A
KC
dt
dC

Integrating,
[ ]

,
_

A
A
A
C
C A
C
CA
A
A
x 1
x
KC
1
t
C
1
K
1
KC
dC
t
0
A
A0
A
0
2
Procedure:
50 ml of NaOH and 50 ml of ethyl acetate are taken in the batch reactor with the starting
and stop water. Then each 10 ml of the reaction mixture is taken every 5 minutes the reaction is
arrested by adding acetic acid to the sample. The reaction mixture is titrated against sodium
hydroxide of known normality and its concentration found. Samples are taken up to 50 minutes
and the concentration of the reactor is found.
Standard Data:
Normality of NaOH :
Normality of Acitic Acid:
Normality of Ethyl acetate:
Tabulation:
S.No. Reaction
Time (min)
Volume of
CH
3
COOH(ml)
Volume of
NaOH (ml)
C
A
(mol/lit)
1/C
A
(lit/mol)
X
A
A
A
X 1
X

1 5
2 10
3 15
4 20
5 25
6 30
7 35
8 40
9 45
10 50
Department of Chemical Engineering 4
Model Graph:
Model Calculation:
1)
2
N
C
NaOH
0
A

2)
Volume Sample
added NaOH of moles added COOH CH of moles
C
3
A

3)
A C
1
4)
0
0
A
A A
A
C
C C
X

5)
A
A
X 1
X
Result:
Thus the experiment on batch reactor was performed. The order of the reaction was
verified and the value of K found from graph.
K=-----------------------(1/C
A
vs time graph)
K=----------------------- (X
A
/(1-X
A
) vs time graph)
**********
BATCH REACTOR II
Department of Chemical Engineering
t
k
A C
1
0 A C
1
0
x
t
x
0
kC
A0
y
y
A
A
X - 1
X
5
Aim:
To verify the order and to determine the rate constants for the reaction between non-
equimolar quantity of NaOH and ethyl acetate in a batch reactor.
Reaction:
NaOH + CH
3
COOC
2
H
5
CH
3
COONa + C
2
H
5
OH
Theory:
In a batch reactor, the composition of the components is uniform throughout at any
instant of time
( )
( )
1
]
1

A
A
A0 B0
B A A
0
A
A
A
X 1 M
X M
ln
) C - KC
1
C KC r -
Products B) (A for
) (-r
kX
C t
XA
0
Procedure:
200 ml of NaOH and 400 ml of ethyl acetate of known concentration are taken in the
reactor. Samples (10ml) are drawn for every 5 minutes from the reactor up to 50 minutes. The
concentration of reactants in the sample is found out by adding 10 ml of acetic acid and
titrating against sodium hydroxide.
Standard Data:
Normality of NaOH :
Normality of Acitic Acid:
Normality of Ethyl acetate:
Tabulation:
S.No. Reaction
Time
(min)
Volume of
CH
3
COOH
(ml)
Volume
of NaOH
(ml)
C
A
(mol/lit)
X
A
M
1
]
1

) X M(1
X M
ln
A
A
1 5
2 10
3 15
4 20
5 25
6 30
7 35
8 40
9 45
10 50
Model Graph:
Department of Chemical Engineering 6
Model Calculation:
1)
total
NaOH NaOH
A
V
N V
C
0

2)
Volume Sample
added NaOH of moles added COOH CH of moles
C
3
A

3)
total
EA EA
B
V
N V
C 0

4)
0
0
A
B
C
C
M
5)
0
0
A
A A
A
C
C C
X

6)
0 0
A B C C
Slope
K

Result:
Thus the experiment on batch reactor II was performed. The order of the reaction was
verified and the value of k found the graph is
K =
**********
Department of Chemical Engineering
Time (min)
x
0
Slope = K (C
B0
C
A0
)
y
( )

,
_

A
A
X 1 M
X M
ln
7
MIXED FLOW REACTOR
Aim: To study the performance of a mixed flow reactor using second order saponification
reaction.
Reaction:
NaOH + CH
3
COOC
2
H
5
CH
3
COONa + C
2
H
5
OH
Theory:
In a mixed flow reactor, properties of the reaction mixture are uniform. Thus for
example, concentration of the reactants at inlet of the second order reaction and outlet
concentration of the reactants remain the same. The design equation for reaction
C
A0
= C
B0
, C
A
= C
B
,
2
A
A A
KC
C C
T
0

Experimental Setup:
It consists of a 500ml flask with a flow steam. This is attached with the flow meter for
setting the flow rate.
Procedure:
The residence time of the reactor is adjusted by adjusting of reactants the flow rate and
keeping the reactor volume constant. When steady state is reached a sample is collected. Excess
acetic acid is added to the sample in order to arrest the reaction. Thus moles of unreacted
reactants and hence the conversion can be found.
Standard Data:
Normality of NaOH :
Normality of Acitic Acid:
Normality of Ethyl acetate:
Flow rate of NaOH =
Flow rate of Ethylacetate =
Tabulation
S.No Sample
Volume (ml)
Burette Reading(ml) Volume of NaOH
consumed (ml)
Initial Final
Model Calculation:
1.
2
N
C
NaOH
A
0

2.
( ) ( ) [ ]
total
NaOH COOH CH
A
V
N V N V
C
3

3.
0
0
A
A A
Aexp
C
C C
X

4. ( )
2
A A Atheo X 1 C k X
0

Result:
Thus the experiment of mixed flow reactor is studied and the conversion is found to be:
Theoretically (X
Atheo
):
Experimentally (X
Aexp
):
**********
Department of Chemical Engineering 8
kC
A0
A
A
X - 1
X
MIXED FLOW REACTOR IN SERIES
Aim: To study the performance of a mixed flow reactor in series, using second order
saponification.
Reaction:
NaOH + CH
3
COOC
2
H
5
CH
3
COONa + C
2
H
5
OH
r
A
= KC
A
C
B
= KC
A
2
Theory:
In a mixed flow reactor, properties of the reaction mixture are uniform. Thus we have
the equimolar concentration of reactant at inlet for the second order reaction. The outlet
concentration will hence be the same.
C
A0
= C
B0
, C
A
= C
B
,
2
A1
A A
1
KC
C C 0

2
A2
A2 A1
2
KC
C C

( )
2
A A0
A
X - 1 KC
X

Procedure:
The residence time of the reactor is adjusted by setting the flow rate of reactants and
keeping the reactor volume constant. When steady state is reached a sample is collected and
excess acetic acid is used to arrest the reaction. Thus moles of unreacted reactants and the
conversion can be found.
Standard Data:
Normality of NaOH :
Normality of Acitic Acid:
Normality of Ethyl acetate:
Flow rate of NaOH =
Flow rate of Ethylacetate =
Tabulation
For Reactor-I
S.No Sample
Volume (ml)
Burette Reading(ml) Volume of NaOH
consumed (ml)
Initial Final
For Reactor-II
S.No Sample
Volume (ml)
Burette Reading(ml) Volume of NaOH
consumed (ml)
Initial Final
Model Calculation:
NaOH
COOH CH COOH CH
NaOH
V
N V
N
3 3

Department of Chemical Engineering 9

At steady state in Reactor I
( ) ( ) [ ]
Volume
N V N V
C
NaOH COOH CH
A
3
1

0
1 0
1
A
A A
A
C
C C
X

At steady state in Reactor II

( ) ( ) [ ]
Volume
N V N V
C
NaOH COOH CH
A
3
2

0
2 0
2
A
A A
A
C
C C
X

Theoretical conversion:
Reactor I:
V
V1
1
( )
2
1
A A0
A
1
X - 1 KC
X

Reactor II:
V
V2
2
( )
2
1 2
A A0
A A
2
X - 1 KC
X - X

Result:
Thus the experiment of mixed flow reactor in series is studied and the conversion is
found to be:
For Reactor-I
Theoretically :
Experimentally :
For Reactor-I
Theoretically :
Experimentally :
**********
Department of Chemical Engineering 10
PLUG FLOW REACTOR
Aim:
To study the performance of the plug flow reactor for the second order reaction of
saponification of ethyl acetate.
Reaction:
NaOH + CH
3
COOC
2
H
5
CH
3
COONa + C
2
H
5
OH
Experimental setup:
It consists of a transparent tube provided with glass beads ( = 0.04) sampling can be
done at different points all along the length of the tube.
Procedure:
NaOH and CH
3
COOC
2
H
5
solution of equal flow rate is allowed to enter at a constant
flow rate until steady state is reached. When the inlet flow rate equals the outlet flow rate, the
steady state is said to be attained. Samples are collected at different position, acetic acid is
added to arrest the reaction. The concentration of unreacted NaOH and conversion in the
mixture is noted.
Standard Data:
Normality of NaOH :
Normality of Acitic Acid:
Normality of Ethyl acetate:
Flow rate of NaOH =
Flow rate of Ethylacetate =
Tabulation:
S.No Sample
Volume (ml)
Burette Reading(ml) Volume of NaOH
consumed (ml)
Initial Final
S.No Reactor volume
(ml)
Space time
(min)
Titrant
volume (ml)
C
A
(N)

X
A
(%)
(expt.)
X
A
(%)
(theo)
Department of Chemical Engineering 11
Model Graph:
Model Calculation:
1. C
Ao
= N
NaOH
/2
2.

V

3.
( ) ( ) [ ]
Volume
N V N V
C
NaOH COOH CH
A
3

4.
0 A
A
Aexp
C
C
1 X
5.
0
0
A
A
Atheo
KC 1
C K
X

Result:
Thus the performance of plug flow reactor under constant flow rate is studied and
necessary graphs are drawn.
**********
Department of Chemical Engineering
Theoretical
Experimental
X
A
x
0
y
Time(min)
12
RTD STUDIES IN A PLUG FLOW REACTOR
Aim:
To study the behavior of a plug flow reactor by RTD studies.
Theory:
Elements of fluid taking different routes through the reactor may take different lengths of
time to pass through the vessel. The distribution of these times for the stream of fluid leaving
the vessel is called the exit age distribution E, or the residence time distribution (RTD) of the
fluid. From E mean residence time, flow pattern, model parameters can be evaluated.
Procedure:
In a plug flow reactor, a tube packed with particles is used. To start with reactor is filled
with 0.05N of NaOH Water flow is allowed from a water tank above the reactor. The variation
of concentration of sodium hydroxide in the each taping point is noted. The dispersion number
is obtained from the graph.
Formulae:
1) ( ) ti E t t i i
2)
2
i i
2
i
2
t t E t
3)
N
1
t

2
2
0
2

where,
time residence mean t
variance
2

t
i
= time interval
number Dispersion
UL
D

Standard data:
Normality of NaOH
Normality of Acitic Acid;
Flow rate of water
Tabulation:
Time
(min)
V
NaOH
(ml)
V
CH3COOH
(ml)
N
NaOH
max
NaOH
N
N
F
dt
dF
Ei
E
i
t
i
E
i
t
i
2
Department of Chemical Engineering 13
Model Graph:
Model Calculation:
1.
NaOH
COOH CH COOH CH
NaOH
V
N V
N
3 3

2. F=N/N
max
. =
3.
dt
dF
Ei
4. ( ) ti E t t i i
5.
2
i i
2
i
2
t t E t
6.
2
2
0
t

7.
2

UL
D
2
0

8.
N
1
2
0

Result:
Thus, the experiment of plug flow RTD was conducted and the dispersion number and N
were calculated.
**********
Department of Chemical Engineering
F E
y y
x x
t t
14
RTD STUDIES IN MIXED FLOW REACTOR
Aim:
To study the behavior of the mixed flow reactor through RTD studies.
Theory:
Elements of fluid taking different routes through the reactor may take different lengths of
time to pass through the vessel. The distribution of these times for the stream of fluid leaving
the vessel is called the exit age distribution E, or the residence time distribution (RTD) of the
fluid. From E mean residence time, flow pattern, model parameters can be evaluated.
Experimental setup and procedure:
Reactor consists of 500 ml beaker attached with stirrer. The flow of water is allowed
from a bottle packed above the level of the reactor. The concentration of NaOH in the exit
stream is determined in the samples collected at intervals the graphs are hence obtained.
Standard data:
Normality of NaOH
Normality of Acitic Acid;
Flow rate of water
Tabulation:
Time
(min)
V
NaOH
(ml)
V
CH3COOH
(ml)
N
NaOH
max
NaOH
N
N
F
dt
dF
Ei
E
i
t
i
E
i
t
i
2
Department of Chemical Engineering 15
Model Graph:
Model Calculation:
1.
NaOH
COOH CH COOH CH
NaOH
V
N V
N
3 3

2. F=N/N
max
. =
3.
dt
dF
Ei
4. ( ) ti E t t i i
5.
2
i i
2
i
2
t t E t
6.
2
2
0
t

7.
2

UL
D
2
0

8.
N
1
2
0

Result:
Thus, the experiment of mixed flow RTD was conducted and the dispersion number and
N were calculated.

**********
Department of Chemical Engineering
F C
y y
x x
t t
x x
y y
X
AP

X
AS

X
Ae

16
SEGREGATED FLOW REACTOR
Aim:
To calculate the performance of a tubular reactor as a segregated flow reactor for the
saponification of ethanol.
Reaction:
NaOH + CH
3
COOC
2
H
5
CH
3
COONa + C
2
H
5
OH
Theory:
In laminar flow in a tubular reactor, segregated flow occurs. The conversion is time
dependant as the element moves through the water. The conversion in each element of fluid
depends upon the residence time. Hence, to obtain average uniform conversion model equation
incorporating non ideal flow is used.
Procedure:
NaOH and ethyl alcohol at known concentrations are allowed to enter at a flow rate of
60 cc/min each into the reactors. Sufficient time is allowed to reach steady state. Samples are
collected drop by drop at different points. Concentration is found by the addition of acetic acid
and titration with NaOH.
From the volume and concentration of sample with NaOH, its concentration is found
out.
Formulae:
1)
q
V

2)
0
0
A
A A
Ae
C
C - C
X
3)
0 A
A0
AP
KC 1
KC
X

4)
1
1
]
1

,
_

+
0
0
0
2
1 ln
2
1
A
A
A A
C K
C K
C K X
seg

Standard Data:
Normality of NaOH :
Normality of Acitic Acid:
Normality of Ethyl acetate:
Flow rate of NaOH =
Flow rate of Ethylacetate =
Tabulation:
S.No Sample
Volume (ml)
Burette Reading(ml) Volume of NaOH
consumed (ml)
Initial Final
Department of Chemical Engineering
X
AP

X
AS

X
Ae

17
S.No Reactor
volume (ml)
Space
time
(min)
Titrant
volume
(ml)
C
A
(mol/lit) X
A(Plug)
X
A (Seg)
X
A(exp)
Model Calculation:
1. C
Ao
= N
NaOH
/2
2.

V

3.
( ) ( ) [ ]
Volume
N V N V
C
NaOH COOH CH
A
3

4.
0 A
A
Aexp
C
C
1 X
5.
0
0
A
A
Atheo
KC 1
C K
X

6.
1
1
]
1

,
_

+
0
0
0
2
1 ln
2
1
A
A
A A
C K
C K
C K X
seg

Model Graph:
Result:
Experiments were conducted in segregated flow and the conversions at various times were
calculated and graphs of conversion Vs time were drawn.
**********
Department of Chemical Engineering
X
AP

X
A
x
0
y
Time (min)
X
AS

X
Ae

18