NATIONAL INSTITUTE OF TECHNOLOGY, TIRUCHIRAPPALLI 15

DEPARTMENT OF CHEMICAL ENGINEERING

CHEMICAL REACTION ENGINEERING LABORATORY MANUAL

Experiments Order
1) Adiabatic Reactor
2) Batch Reactor I
3) Batch Reactor II
4) Mixed Flow Reactor
5) Mixed Flow Reactor in Series
6) Plug Flow Reactor
7) Mixed Flow Reactor followed by Plug Flow Reactor
8) RTD Studies in a Plug Flow Reactor
9) RTD studies in a Mixed Flow Reactor

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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.

Tf T 2

dT KCA0e E RT

dt
TF T0

Where
TF Final Temperature (C)
T0 Initial Temperature (C)
K Rate constant
CA0 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)

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ln A

Model Graph:

TC

lnA

Slope = -E/R

Time (s)

1/T (k-1)

Model Calculation:
1) t =
2) T =
dT
3)

dt
4) (Tf T)2=
5) A

dT
10 3

=
dt (Tf T) 2

6) lnA =
1
7)
=
(T 273)
8) E= -slope x R=
Result and Inferences:

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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 + CH3COOC2H5

CH3COONa + C2H5OH

Theory:
For a second order reaction, the rate of reaction is as follows
dCA
KCA 2
dt
Integrating,
CA
CA
dCA
1
t
1
2
CA CA0
KCA
K
CA0

1 xA

KCA0 1 xA

Procedure:
500 ml of NaOH and 500 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 CH3COOC2H5=
Normality of CH3COOH=
Tabulation:
S.No.
1
2
3
4
5
6
7
8
9
10

Reaction
Volume of Naormality
Time (min) NaOH (ml) of NaOH (N)
5
10
15
20
25
30
35
40
45
50

CA
1/CA
-3
(mol/lit)10
(lit/mol)

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XA

XA
1 XA

Model Graph:
y

CA

kCA0

XA
1 - XA

CA0
0

x
t

Model Calculation:
NNaOH
1) CA0
=
2
moles of CH3COOH added moles of NaOH added
2) CA
=
Sample Volume
1
3)
=
CA
CA0 CA
4) XA
=
CA0
XA
5)

1 XA
Result:
Thus the experiment on batch reactor was performed. The value of K found from
graph.
1/CA vs t =
XA /(1-XA) vs t =

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BATCH REACTOR II
Aim:
To verify the order and to determine the rate constants for the reaction between nonequimolar quantity of NaOH and ethyl acetate in a batch reactor.
Reaction:
NaOH + CH3COOC2H5

CH3COONa + C2H5OH

Theory:
In a batch reactor, the composition of the components is uniform throughout at any
instant of time
XA
kXA
t CA0
(-rA)
0

for (A B) Products
- rA KCACB

m XA
1
ln
K(CB0 - CA0) m1 XA

Procedure:
400 ml of NaOH and 800 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 CH3COOC2H5=
Normality of CH3COOH=
Tabulation:
S.No. Reaction Volume of Naormality CA
CBo
Time (min) NaOH (ml) of NaOH (N) (mol/lit)10 -3 (mol/lit)
1
2
3
4
5
6
7
8
9
10

XA

m XA
ln

m(1 XA)

5
10
15
20
25
30
35
40
45
50

Model Graph:

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m XA

ln
m1 XA

Slope = K (CB0 CA0)

x
Time (min)

Model Calculation:
VNaOH NNaOH
1) CA0
=
Vtotal
N V A.A N V NaOH =
2) CA
Total Volume
VEA NEA
3) CB0
=
Vtotal
CB0
4) M
=
CA0
CA0 CA
5) XA
=
CA0
Slope
6) K
=
CB0 CA0
Result:
Thus the experiment on batch reactor II was performed. The value of k found the
graph is

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Department of Chemical Engineering

MIXED FLOW REACTOR

Aim: To study the performance of a mixed flow reactor using second order saponification
reaction.
Reaction:
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
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
CA0 CA
CA0 = CB0,
CA = CB,

KCA 2
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 CH3COOC2H5=
Normality of CH3COOH=
Flow rate of NaOH
Flow rate of CH3COOC2H5=
Reaction Rate Constant =
Table: 1
S.No.

Volume of Sample
(ml)

Burette Reading (ml)

Initial
Final

Concordant Value (ml)

Model Calculation:
V
1) =

V NCH3COOH V N NaOH
2) CA
Vtotal
CA0 CA
3) XAexp
CA0
2
4) XAtheo kTCA01 XA
Result:
Thus the experiment of mixed flow reactor is studied and the conversion is found to be:
XATheo:
XAExp:
--------------Department of Chemical Engineering

MIXED FLOW REACTOR IN SERIES

Aim: To study the performance of a mixed flow reactor in series, using second order
saponification.
Reaction:
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
rA = KCACB = KCA2
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.
CA0 = CB0,
CA = CB ,
1 CA0 C2A
KCA1
CA1 CA2
2
KCA2 2
X A 2
KCA0 1-XA
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 CH3COOC2H5=
Normality of CH3COOH=
Flow rate of NaOH
Flow rate of CH3COOC2H5=
Reaction Rate Constant =
Table: 1
S.No.

Volume of Sample

Burette Reading (ml)

Initial
Final

Concordant Value (ml)

Volume of Sample

Burette Reading (ml)

Initial
Final

Concordant Value (ml)

Table: 2
S.No.

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Model Calculation:
VCH3COOH NCH3COOH
NNaOH
VNaOH
At steady state in Reactor I

CA1

V NCH COOH V N NaOH

3

Volume
CA0 CA1
XA1
CA0
At steady state in Reactor II
CA2
XA2

V NCH COOH V N NaOH

3

CA0 CA2
CA0

Volume

Theoretical conversion:
Reactor I:

V1

XA1
2
KCA01-XA

Reactor II:

V2

2 XA2 - XA1 2
KCA0 1-XA
2

Result:
Thus the experiment of mixed flow reactor in series is studied and the conversion is
found to be:
Reactor 1
XA,Theo :
XA,Exp :
Reactor 2
XA,Theo :
XA,Exp :
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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 + CH3COOC2H5 CH3COONa + C2H5OH
CA

dCA
1 1 CA

2
CA CA0
KCA
K
CA0

1 xA

KCA0 1 xA
KC A 0
XA
1 KC A 0
t

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 CH3COOC2H5 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 CH3COOC2H5=
Normality of CH3COOH=
Flow rate of NaOH
Flow rate of CH3COOC2H5=
Reaction Rate Constant =
Tabulation:
S.No Reactor volume Space time
(ml)
(min)

Titrant
volume (ml)

CA (N)
10 3

XA (%) XA (%)
(expt.) (theo)

Model Graph:
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11

y
Theoretical
Experimental
XA

0
Time
Model Calculation:
1)
2)
3)
4)
5)

Initial Concentration= NNaOH/2

V
V0
V NCH3COOH V N NaOH
CA
Volume
CA
XAexp 1
CA0
KCA0
XAtheo
1 KCA0

Result:
Thus the performance of plug flow reactor under constant flow rate is studied and
necessary graphs are drawn.

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Department of Chemical Engineering

12

MIXED FLOW FOLLOWED BY PLUG FLOW REACTOR

Aim: To study the performance of a mixed flow followed by plug flow reactor using second
order saponification reaction.
Reaction:
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
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
CA0 = CB0,
CA = CB,
1 V1
1 CA0 C2A1
V
KCA1
Whereas in plug flow the concentration of the reactants are changing along with length and
hence the with residence time as volume of the reactor changing with the length for give a
flow rates of reactants

V2
KCA02
; XAtheo
V
1 2KCA0

Experimental Setup:
It consists of a 1000ml flask attached with stirrer and transparent tube provided with
glass beads ( = 0.04) sampling can be done at different points all along the length of the
tube.
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
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 CH3COOC2H5=
Normality of CH3COOH=
Flow rate of NaOH
Flow rate of CH3COOC2H5=
Reaction Rate Constant =
S.No Reactor volume Space time
(ml)
(min)

Titrant
volume (ml)

CA (N)
10 3

XA (%) XA (%)
(expt.) (theo)

Model Calculation:
VCH3COOH NCH3COOH
NNaOH
VNaOH
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13

At steady state in Reactor I

CA1

V NCH COOH V N NaOH

3

Volume

CA0 CA1
CA0
At steady state in Reactor II
XA1

CA2

V NCH COOH V N NaOH

3

CA0 CA2
XA2
CA0

Volume

Theoretical conversion:
Reactor I:

V1
V

XA1
2
KCA01-XA

Reactor II:

V2
V
KCA02
4) XAtheo
1 2KCA0
2

y
Theoretical
Experimental
XA

x
Time

Result:
Thus the performance of mixed flow followed by plug flow reactor under constant flow
rate is studied and necessary graphs are drawn.

---------Department of Chemical Engineering

14

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.
Standard Data:
Normality of CH3COOH =
Flow rate of Water
=
Normality of NaOH (Nmax)
Formulae:
1) t tiEiti

2) 2 ti 2 Eiti t
2
3) 0 2 2
t
D
0 2

4)
UL
2
1
5) 0 2
N
where,
t mean residence time
2 variance
ti = time interval
D
Dispersion number
UL
Tabulation:
Time
VCH3COOH
(min)
(ml)

NNaOH

NNaOH
Nmax

Ei

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dF
dt

Eiti

Eiti2

15

Model Graph:
y

x
t

t
Model Calculation:
1) 1 NNaOH
=
N
2) F
Nmax
3) F = y (t)
dF
4) E
dt
5) t tiEiti
6) 2 ti 2 Eiti t
2
7) 0 2 2
t
D
0 2

8)
UL
2
1
9) 0 2
N

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

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16

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 CH3COOH =
Flow rate of Water
=
Normality of NaOH (Nmax)
Formulae:
1) t tiEiti

2) 2 ti 2 Eiti t
2
3) 0 2 2
t
D
0 2

4)
UL
2
1
5) 0 2
N
where,
t mean residence time
2 variance
ti = time interval
D
Dispersion number
UL

Tabulation:
Time
VCH3COOH
(min)
(ml)

NNaOH

NNaOH
Nmax

Ei

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dF
dt

Eiti

Eiti2

17

Model Graph:
y

x
t

t
y

Model Calculation:
N
1) F
Nmax
2) F = y (t)
dF
3) E
dt
4) t tiEiti
5) 2 ti 2 Eiti t
2
6) 0 2 2
t
D
0 2

7)
UL
2
1
8) 0 2
N

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