Chemical Reaction Engineering

Laboratory
CH8611

Department of Chemical Engineering

A.C.Tech, Anna University.
 Content
Ex. No Date Experiment Marks Initials
Diagram:

Batch Reactor
 Ex. No:
Date:

Kinetic Study of Batch Reactor

Aim:
To study the kinetics of batch reactor by determining the rate as well as rate constant of
the given reaction.

Theory:
A typical batch reactor consists of a tank, integral heating/ cooling system and
agitator. These vessels may vary in size from less than 1liter ton to more than 15,000
liters.

They are usually fabricated in steel, stainless steel or exotic alloy liquids and
solids are usually charged via connections in top cover of the reactor. Vapors and gases
also discharge through connections in top.

Liquids are usually discharged in the bottom. The advantages of batch reactor lie
with versatility. A single vessel can carry out a sequence of different reactions without the
need to break the containment. A batch reactor has no input to output when the reaction
occurs.( FA0 = FA=0 )

Observation:
S.No Time Volume of sample collected Volume of NaOH consumed
Unit (min) (ml) (ml)

Calculation:
S.No Time CA XA -ln(1-XA) XA / ( 1-XA) k1 k2
Unit (min) (mol/lit) - - - (min-1) (mol-1.lit.min-1)

Formulae:
1. Design equation for batch reactor:

n
2. Differential method of analysis: - = k CA

1-n 1-n
3. Integral method of analysis: CA – CA0 = (n-1) k t

Order 1: ln ( CA0 / CA) = k1t (or) -ln (1- XA ) = k1 t

Order 2: (1/ CA)- (1/ CAO) = k2t (or) XA / ( 1- XA ) = k2 t

Apparatus Required:
Measuring cylinder, burette, conical flask, beaker, stirrer.

Procedure:
Model Calculation:
1. VHClx NHCl= VNaOHx NNaOH

VHCl= (VNaOHx NNaOH) / NHCl

2. HCl consumed= 10 – HCl not consumed

=

3. CA = ( HCl consumed x NHCl ) / ( Volume of sample)

CA =
4. CAO =

5. Conversion, XA = 1- (CA / CA0 )

=
 XA=

6. For first order,

-ln (1- XA ) = k1 t

k1 = [-ln ( 1 – XA ) ] / t

k1 =
7. For second order,

XA / ( 1- XA ) =k2 t

k2= XA / [ ( 1 – XA ) t ]

k2 =

Inference:
The order of the system is observed to be ______________ order as the theoretical and
analytical values of k are similar. The regression value ( R2) is observed as

kavg (theoretical) =

k avg (analytical) =

Error (%) =

Possible errors are due to :

● Errors in end point detection

● Calculation approximation

● Instrumental errors
Result:
Thus the rate constant (k) for the first and the second order reaction have been

determined to be:

Analytical: k1 = k2 =

Theoretical: k1 = k2 =

Diagram:

Sonochemical Reactor
 Ex. No:
Date:

Kinetic Study of Sonochemical Reactor

Aim:
To determine the kinetics of hydrolysis of an ester in a sonochemical batch reactor
by integral method of analysis.

Theory:
Sonochemical reactor is one of the batch reactors. Here, instead of stirrers, we use
solid vibration. It is used in small scale industries and in simple reactions for laboratory
purposes. There are many designs for sonochemical reactors called the cavitation reactors.
Practically acceptable law of alternating of amplitude wave is described. Thus, the more
effective sonochemical reactors have symmetric acoustic cell.

The quality of product is very poor, that is the product’s specifications varies
widely with different batches. The time consumption is also higher compared to PFR and
CSTR.
The reactor should be maintained properly. After every batch, it should be washed
thoroughly, otherwise, the product obtained is poor in quality. The cost of operation for a
single reaction is high, hence it is not efficient compared to other reactors.

Sonochemical reactors are used in production of fuels, food and pharmaceutical

industries.

Formulae:
1. Design equation for batch reactor:

2. Differential method of analysis: - = k CAn

3. Integral method of analysis: CA1-n– CA01-n= (n-1) k t

Order 1: ln ( CA0 / CA) = k1t

Order 2: (1/ CA)- (1/ CA0) = k2t

Apparatus Required:
Sonicator, measuring cylinder, beaker,conical flask, burette.
Observation:
S.No Time Volume of sample Volume of NaOH Consumed
collected
Unit (min) (ml) (ml)

Calculation:
S.No Time Conc. of ln[CA0/CA] (1/CA)-(1/CAO) k1 k2
NaOH
Unit (min) (mol/lit) - (lit/mol) (min-1) (min-1.lit.mol-1)
Procedure:
Model calculation:
1. VHClx NHCl= VNaOHx NNaOH

VHCl= (VNaOHx NNaOH) / NHCl

VHCl =

2. HCl consumed = 10 – HCl not consumed

=
HCl consumed =

3. CA = ( HCl consumed x NHCl ) / ( Volume of sample)

CA =

4. CAO =

5. ln [ CAO / CA ] =

6. (1/ CA) - ( 1/ CAO ) =

7. k1 = [ln ( CAO / CA )] / t
=

k1 =

8. k2 = [(1/CA) – (1/ CAO)] / t

k2 =
Inference:
The order of the system is observed to be ______________ order as the theoretical and
analytical values of k are similar. The regression value ( R2) is observed as

kavg (theoretical) =

k avg (analytical) =

Error (%) =

Possible errors are due to :

● Errors in end point detection

● Calculation approximation

● Improper standardization of solutions

Result:
Thus the rate constant (k) for the first and second order reaction have been

determined to be:

Analytical: k1 = k2 =

Theoretical: k1 = k2 =
Diagram:

Plug Flow Reactor

Ex. No:
Date :
 Kinetic Study of Plug Flow Reactor
Aim:
To determine the rate constant for the reaction between equi-molar NaOH and
ethyl acetate in a given plug flow reactor.

Theory:
Plug flow reactor, sometimes called continuous tubular reactor (CTR) or piston
flow reactor, is a model used to describe chemical reaction in continuous flowing system
of cylindrical geometry. Fluid going through PFR may be modeled as flowing through the
reactor as a series of infinitely thin coherent plugs traveling in the axial direction with each
plug having a different composition from the ones before and after it. Key assumption is
that as a fluid flows through the PFR, the fluid is perfectly mixed in the radial direction
but not in the axial direction.

PFR has a high volumetric unit conversion run for any period of time without
maintenance. Heat transfer rate can be determined by using thinner or thicker tubes in
parallel.

Formulae:
1. Residence time, τ = V / v0

V – volume of reactor ( m3 )

v0– volumetric flow rate ( m3 / sec )

2. XA = ( CAO – CA ) / CA0

Apparatus Required:
Measuring cylinder, burette, conical flask, beaker,stirrer.

Observation :
S.No Volumetric Volumetric Total Volume Volume of Volume
flow rate of flow rate of flow rate of reactor of NaOH
NaOH CH3COOC2H sample Ʈ CA
5
collected
Unit (LPH) (LPH) (LPH) (ml) 3 (ml) (sec) (mol/lit)
(m )

Calculation :
S.No XA -ln(1-XA) XA/ ( 1-XA) k1 k2
Unit - - - (min-1) (mol-1.lit.min-1)

Procedure:
Design Parameters:
 1. Diameter of pipe = 1.5 cm

2. Diameter of reactor = 22.5 cm

3. Volume of reactor = No. of turns x cross- sectional area x circumference

= 9 x π [ ( 1.5 x 10-2 ) / 2 ]2 x 2 x π x [ (22.5 x 10-2 ) / 2 ]

= 0.00124 m3

Model Calculation:
1. VHClx NHCl= VNaOHx NNaOH

VHCl= (VNaOHx NNaOH) / NHCl

=

2. HCl consumed = 10 – HCl not consumed

=

3. CA = ( HCl consumed x NHCl ) / ( Volume of sample)

4. XA = 1- ( CA / CA0 )
=

5. τ= V / v 0

6. k1 = -ln ( 1- XA) /τ

7. k2 = XA / [ ( 1- XA ) CA0τ ]

Inference:
 The system follows ____________ order as the theoretical and analytical values of

rate constant are the same.

k avg ( theoretical) =

k avg (analytical) =

Error ( % ) =

Possible errors are due to:

● End point detections

● Improper standardization of solution

● Instrumental fault

Result:
Thus the rate constant (k) of the given reaction for first and second order have been

determined to be:

Analytical: k1 = k2=

Theoretical: k1 = k2 =

Diagram:
Batch reactor

Ex. No:
Date:
Kinetic Study of Non-Equimolar Batch Reactor
Aim:
To study the kinetics and hence determine the rate constant of given reaction between
non-equimolar concentration of NaOH and ethyl acetate in a batch reactor.

Theory:
The experimental batch reactor is usually operated isothermally at constant
volume because it is easy to interpret the result of such runs. It is used as small scale set-
up and used whenever possible for obtaining homogeneous data. The starting point for all
design is the material balance expressed for any reactant or product over a small element of
volume. Reactants enter and leave while getting accumulated and disappeared by reaction
within the element. If the composition within the reactor is uniform, the accounting may be
made over the whole reactor. If the composition is not uniform, it must be made uniform
 over a differential element of volume and then integrated across the whole reactor for the
appropriate flow and concentration conditions.

NaOH + CH3COOC2H5 ------> CH3COONa+ C2H5OH

Rate equation for a second-order non-equimolar reaction,

-rA = k CA0 (1 – XA ) CB0( 1 – XB)

=k CA0 (1 – XA) ( CB0 – CA0 XA )

CA0 = k CA0( 1 – XA ) CA0 ( ΘB– XA) where ΘB = CB0 / CA0

=k CA0( 1 – XA) ( ΘB – XA)

d XA / [ (1- XA ) ( ΘB – XA) ] = k CA0dt

Integrating at limits, t=0 XA = 0

t=t XA = XB

ln [ ( ΘB– XA) / (1- XA) ΘB ] = k CA0 (ΘB– 1 ) t

Observation:
S.No Time Volume of sample collected Volume of NaOH consumed
Unit (min) (ml) (ml)
 Calculation:
S.No CA XA ln[1/ (1-XA)] XA/ ( 1- XA) k1 k2
Unit (mol/lit) - - - (min-1) (mol-1.lit.min-1)

Formulae:
1. Volume of HCl not consumed = ( titrated value x NNaOH) /NHCl

2. Conversion, XA = 1- ( CA/ CA0 )

3. For first order, k1 = -ln ( 1- XA) / t

4. k2 = XA / [ ( 1- XA ) CA0 t ]

Apparatus Required:
Measuring cylinder, burette, conical flask, beaker, stirrer.

Procedure:
Model Calculation:
1. VHClx NHCl= VNaOHx NNaOH

VHCl= (VNaOHx NNaOH) / NHCl

=

VHCl =

2. HCl consumed = 10 – HCl not consumed

=
HCl consumed =

3. CA = ( HCl consumed x NHCl ) / ( Volume of sample)

=
 CA =

4. CAO=

5. Conversion, XA = 1- (CA / CA0 )

XA =

6. For first order,

-ln (1- XA ) = k1 t

k1 = [-ln ( 1 – XA ) ] / t

7. For second order,

XA / ( 1- XA ) =k2 t

k2 = XA / [( 1 – XA ) t]

Inference:
The system follows ____________ order as the theoretical and analytical values of

rate constant are the same.

k avg ( theoretical) =

k avg (analytical) =

Error ( % ) =

Possible errors are due to:

● End point detection

● Approximation in calculation

● Instrumental error
Result:
Thus the rate constant (k) of the given reaction for first and second order have been

determined to be:

Analytical: k1 = k2 =

Theoretical: k1= k2=

Diagram:

Packed Bed Reactor

 Ex. No:
Date:

Kinetic Study of Packed Bed Reactor

Aim:
To determine the rate constant of the reaction between NaOH and ethyl acetate
using a packed bed reactor.

Theory:
The principle difference between reactor design calculations involving
homogeneous reactions and these involving fluid- solid heterogeneous reactions is that is
latter, reaction takes place on surface of catalyst. The reaction is based on mass of catalyst
rather than reaction volume. The reactor volume containing catalyst is of secondary
significance. The design equation is similar to that of PFR but, the volume is replaced with
weight of catalyst. As with PFR, PBR is assumed to have no radial gradient as concentration.

For fluid-solid heterogeneous system,

Here, W is the weight of catalyst required to reduce the entering molar flow rate FA0
of species to flow rate FA .

Advantages:
● High conversion rate per unit weight of the catalyst.
● Easy to build more contact between reactant and catalyst than any other reactors.
● Low cost of construction and operation.
● Effective at high temperature.

Observation:
 S.No Flow rate Time Volume of NaOH Volume of sample
collected consumed
Unit (LPH) (sec) (ml) (ml)

Calculation:
S.No τ CA XA -ln ( 1 – XA ) XA / ( 1 – XA ) k1 k2

Unit (sec) (mol/lit) - - - - -1

(sec 1 ) ( mol .lit.sec-1 )
Formulae:
1. Design equation for packed bed reactor :

2. Differential method of analysis: - = k CAn

3. Integral method of analysis: CA1-n – CA01-n= (n-1) kτ

Order 1: ln ( CA0 / CA) = k1τ

Order 2: (1/ CA)- (1/ CA0) = k2τ

Apparatus Required:
Measuring cylinder, beaker, conical flask, burette, stirrer.

Procedure:
Design Parameters:

1. Radius of the reactor = 0.029 m

2
2. Volume of the reactor = πr h
3
= 0.00258 m

Model Calculation:
1. VHClx NHCl= VNaOHx NNaOH
VHCl= (VNaOHx NNaOH) / NHCl
=

VHCl =

2. HCl consumed = 10 – HCl not consumed

=
HCl consumed =

3. CA = ( HCl consumed x NHCl ) / ( Volume of sample)

CA =

4. CAO=

5. Conversion, XA = 1- (CA/ CA0 )

XA=

6. τ = V / v0

τ=
7. For first order,

-ln (1- XA) = k1τ

k1= [-ln ( 1 – XA) ] /τ

k1 =
8. For second order,

XA/ ( 1- XA) =k2τ

k2 = XA / [ ( 1 – XA ) τ ]

k2 =
Inference:
The system follows ____________ order as the theoretical and analytical values of

rate constant are the same.

k avg ( theoretical) =

k avg (analytical) =

Error ( % ) =

Possible errors are due to:

● End point detection

● Approximation in calculation

● Instrumental error

Result:
Thus the rate constant (k) of the given reaction for first and second order have been

determined to be:

Analytical: k1 = k2 =

Theoretical: k1 = k2 =
Diagram:

Different types of RTD analysis (non-chemical)

c (t) versus time

 Ex. No:
Date:

RTD Study of Packed Bed Reactor

Aim:
To study the non-ideality of packed bed reactor by carrying out the Residence Time
Distribution study and to determine the mean residence time.

Theory:
The PBR consists of a glass column packed with catalyst. Reactant are fed toe the
reactor through liquid distribution. The flow patter in real reactors do not confirm exactly to
those postulated for ideal PBR. The significant difference is noted between observed two
predicted results. These differences may rise from a number of sources from channeling of
fluid as it moves through a reaction vessel from longitudinal mixing caused by vertices and
turbulence from the presence of stagnant region within the reactors. By passing an inert –
tracer or short circuiting a portion of PBR, the RTD study is done.

Formulae:
1. c (t) = ( titer value x NNaOH ) / Volume of sample

2. Q = ∑ c (t) ∆t

3. E (t) = c (t) / Q

4. F (t) = ∑ E(t) ∆t

5. = ∑ [ t c(t) ∆t ] / ∑ [ c (t) ∆t ]

Apparatus Required:
Burette, injection, tracer, conical flask.

Reagents Used:
0.1 N HCl , dye, water, NaOH.

Observation:
 S.No Time Volume of NaOH consumed
Unit (min) (ml)

Calculation:
S.No Time Volume of c(t) E (t) ∆t E (t) t E(t) F (t) t c(t)
NaOH
consumed
Unit (sec) (ml) - - - - - -

Procedure:
Model Calculation:
 1. c (t) = ( titer value x NNaOH) / Volume of sample

c (t)=

2. Q = ∑ c (t) ∆t

Q=

3. E (t) = c (t) / Q

E (t) =

4. F (t) = ∑ E(t) ∆t

F (t) =

5. = ∑ [ t c(t) ∆t ] / ∑ [ c (t) ∆t ]

Inference:
 RTD study was carried out in the packed bed reactor and the mean residence time was
determined to be:

(theoretical) =

(graphical) =

Error (%) =

Possible errors are due to errors in :

● Titration
● Normalization

● Tracer injection

Result:
RTD study was carried out in a packed bed reactor and the [ t E(t) versus time ]

graph was plotted.

( theoretical) =

(graphical) =

Diagram:
Different methods of RTD analysis (non-chemical)

c (t) versus time

Ex. No:
Date:
 RTD Study of Plug Flow Reactor
Aim:
To study the non-ideality of plug flow reactor by plotting curves for a positive
response to step input tracer experiment and also to determine mean residence time.

Theory:
Reactants are fed to the reactor through liquid distribution. The flow pattern in real
reactors do not confirm exactly to those postulated for ideal PFR. The significant difference
is noted between observed two predicted results. These differences may rise from a number
of sources from channeling of fluid as it moves through a reaction vessel from longitudinal
mixing caused by vertices and turbulence from the presence of stagnant region within the
reactors. By passing an inert – tracer or short circuiting a portion of PFR, the RTD study is
done.

Formulae:
1. c (t) = ( titer value x NNaOH ) / Volume of sample

2. Q = ∑ c (t) ∆t

3. E (t) = c (t) / Q

4.F(t) = ∑ E(t) ∆t

5. = ∑ [ t c(t) ∆t ] / ∑ [ c (t) ∆t ]

Apparatus Required:
Burette, injection, tracer, conical flask.

Reagents Used:
0.1 N HCl , dye, water, NaOH.

Observation:
 S.No Time Volume of NaOH consumed
Unit (min) (ml)

Calculation:
S.No Time Volume of c(t) E (t) ∆t E (t) t E(t) F (t) t c(t)
NaOH
consumed
Unit (sec) (ml) - - - - - -

Procedure:
Model Calculation:

1. c (t) = ( titer value x NNaOH) / Volume of sample

 =

c (t)=

2. Q = ∑ c (t) ∆t

Q=

3. E (t) = c (t) / Q

E (t) =

4. F (t) = ∑ E(t) ∆t

F (t) =

5. = ∑ [ t c(t) ∆t ] / ∑ [ c (t) ∆t ]

Inference:
RTD study was carried out in the plug flow reactor and the mean residence time was
determined to be:
(theoretical) =

(graphical) =

Error (%) =

Possible errors are due to errors in :

● Titration
● Normalization

● Tracer injection

Result:
RTD study was carried out in a plug flow reactor and the [ t E(t) versus time ] graph

was plotted.
( theoretical) =
( graphical)=

Diagram:
Continuous Stirred Tank Reactor

Ex. No:
Date:
 Kinetic Study of CSTR

Aim:
To determine the kinetics of hydrolysis of an ester in a mixed flow reactor by integral
method of analysis.

Theory:
Continuous flow reactors are always operated at steady state. It is also called as
back-mix reactor and is primarily used for liquid phase reactions. It is normally operated
at steady state and assumed to be perfectly mixed. There is no time dependence and
position dependence of temperature. Thus the temperature and concentration inside the
reactor and that in the exit stream are the same.

Formulae:
1. CA= ( VHCl x NHCl ) / VHCl of mixture

2. XA = ( CAO – CA) / CAO

3. k = XA / [ (1-XA)2CAO]

Apparatus Required:
Measuring cylinder, beaker, conical flask, burette, stirrer.

Observation:
S.No Time Volume of NaOH Flow rate
consumed
Unit (min) (ml) (LPH)
 Calculation:
S.No Volume Volume CA XA XA/(1- XA/[(1- Ʈ k1 k2
of HCl of HCl XA) XA)2CAO]
consumed unconsumed

Unit (ml) (ml) (mol/lit) - - (lit/mol) (sec) (sec-1) (mol-1.lit.sec-1)

Procedure:
Model Calculation:
1. VHClx NHCl= VNaOHx NNaOH
VHCl= (VNaOHx NNaOH) / NHCl
=

2. Volume of HCl consumed = 10 – volume of HCl not consumed

=
3. CA = ( VHCl x NHCl ) / Volume of sample
=
 4. XA= 1 - ( CA / CAO )

XA =

5. XA / ( 1 – XA ) =

6. XA / [ (1- XA )2CAO ] =

7. τ= V / v0
=

8. k1 = XA / [ ( 1 – XA )τ ]

k1 =

k2= XA / [ (1- XA )2 CAOτ ]

k2 =

Inference:
From the analytical and theoretical values of k, it is inferred that the system is
___________ order.

k avg (theoretical) =

k avg (analytical) =

Error (%) =

Errors might be due to :

● Instrumentation error
 ● Approximation of calculation

● Addition of excess indicator (phenolphthalein)

Result:
Thus, the rate constant values of the reaction for first and second order have been

determined to be:

Theoretical: k1= k2 =

Analytical: k1= k2=

Diagram:
 CSTR in Series

Ex. No:
Date:

Kinetic Study of CSTR in Series

Aim:
To determine the kinetics of CSTR in series and determine the rate constant for
the reaction between equi-molar NaOH and ethyl acetate in the given CSTR in series.

Theory:
The CSTRs ( in series) consist of agitated ,glass reactor vessels. The concentration
is kept uniform for each reactor and it is observed that there is a change in concentration of
fluids from one reactor to another. The CSTR has non-linear dynamics characteristics. It is
used to study the reaction mechanism as well as the dynamics of the reactor with various
types of inputs. CSTR is widely used in water treatment and chemical and biological
processes.

The ‘n’ number of CSTRs when used in series can be considered as a PFR. The
conversion is high and temperature can be easily maintained. On using a number of CSTRs
 in series rather than a large CSTR, reduces the total volume if reactor set-up required,
thereby reducing cost. Thus CSTR in series is preferable rather than a PFR or CSTR.

Formula:
1. CA = ( Volume of HCl consumed x NHCl )/ volume of sample

2. Conversion, XA = 1 - ( CA / CA0)

3. τ= V/ v0

4. For first order,

τ = XA / ( 1 - XA)
5. For second order,

τ= XA / [ ( 1 – XA)2 CA0]

Apparatus Required:
Measuring cylinder, beaker, conical flask, burette, stirrer.

Observation:
S.No Flow Rate Flow Rate of Time Volume of Volume of Volume of
of NaOH Ethyl acetate Tank 1 Tank 2 Tank 3
Unit (LPH) (LPH) (sec) (ml) (ml) (ml)

Calculation:
S.No Tank 1 Tank 1 Tank 2 Tank 2 Tank 3 Tank 3
k1 k2 k1 k2 k1 k2
Unit (min-1) (mol-1.lit.min-1) (min-1) (mol-1.lit.min-1) (min-1) (mol-1.lit.min-1)

Procedure:
Model Calculation:

1. VHClx NHCl= VNaOHx NNaOH

VHCl= (VNaOHx NNaOH) / NHCl
=

2. Volume of HCl consumed = 10 – volume of HCl not consumed

=
3. CA= ( VHCl x NHCl) / Volume of sample
=

CA=

4. XA = 1 - ( CA / CAO )

τ = V / v0
 =
5. XA / ( 1 – XA ) =

6. XA/ [ (1- XA )2CAO ] =

7. k1 = XA / [ ( 1 – XA ) τ]

k1 =

8. k2 = XA / [ (1- XA)2 CAOτ]

k2=

Inference:
From the analytical and theoretical values, we come to know that the system follows
_________________ order.

Error (%) for Tank 1 =

Error (%) for Tank 2 =

Error (%) for Tank 3 =

 Result:
The rate constant for the first and the second order have been determined theoretically
and graphically for the three tanks to be :

Tank 1 Tank 2 Tank 3

(Graphically ) k1
(Theoretically ) k1
(Graphically) k2
(Theoretically ) k2