Chemical Reaction Engineering

M.P.Shah, DDU, Nadiad Page 0

 Chemical Reaction Engineering

CONTENTS Page No

1. RTD STUDIES IN AN ANNULUS 2

2. RTD STUDIES IN SINE TUBE 4

3. RTD STUDIES FOR LAMINAR FLOW 6

4. AGITATED BUBBLE COLUMN 8

5. TANKS IN SERIES MODEL 11

6. DISPERSION MODEL 13

7. CASCADE OF STIRRED VESSEL 15

8. HETEROGENEOUS REACTIONS 17

9. RTD STUDIES IN A SINGLE STIRRED TANK 19

10. RTD STUDIES IN HELICAL COIL TYPE REACTOR 20

11. RTD STUDIES IN STRAIGHT TUBE TYPE REACTOR 22

12. ADIABATIC EFFECT STUDY 24

BEYOND SYLLABUS

 HYSYS simulation for Catalytic Reaction

 HYSYS simulation for absorption with chemical reaction

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 Chemical Reaction Engineering

EXPERIMENT : 1 RTD STUDIES IN AN ANNULUS

AIM: To construct various curves such as E, E, F, F, I and I for the case of flow of water and predict
the conversion for a first order irreversible reaction of known rate constant.

THEORY: The residence time distribution (RTD) studies throw information on the flow pattern of a
fluid in a system. This is accomplished by the stimulus – response techniques i.e. a tracer is injected at
one point of the system and its concentration is analyzed at some another point. Usually, the tracer is so
chosen as to have similar properties of the main fluid and also lend itself for easy analysis. There are
several kinds of input among which the impulse input and step input are widely used. The response of the
former in the normalized form is known as the C curve. The response for the letter is called as the F
curve. I curve represents the internal age distribution.

APPARATUS: annulus, tracer injection device, measuring cylinder (250ml), tracer(NaOH solution),
burette, conical flask, test tubes (12 No.), stop watch, standard HCl etc.

PROCEDURE: In given annulus, a steady flow of water is maintained throughout the course of
investigation. A solution of around 2 N NaOH is used as the tracer. About 2ml of the tracer is injected
through a syringe at the inlet of the annulus as quickly as possible and simultaneously, a stopwatch is
started. At regular interval of time, depending upon the flow rate, a small quantity of water (about 10ml)
from the outlet is collected in a test tube and in this way 12 samples are prepared. These are subsequently
analyzed for the concentration of NaOH using 0.1N HCl. The steady flow rate of water is also measured.
The volume of the annulus is 55ml.
OBSERVATION TABLE:
Sr no. Time B.R. Conc. C E = = F = F I I E*e-kt
(sec) (ml) gmol/l = c/Q Et t/ t
1
2
3
4
5
6
7

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CALCULATIONS: The concentration of the tracer is expressed as mol/lit (same as normality). A graph
is drawn between Concentration and Time in seconds and from such a graph the area Q under the curve is
found out as cdt [(mol/lit)sec]. In order to find E, the concentration at different time is divided by Q  E
= c/Q and a graph is drawn between E and t. this is known as E – curve. The unit of E is sec-1. the average
residence time t is calculated as (volume of annulus / volumetric flow rate of water ). In terms of
dimensionless quantities, a plot of E (= t E) Vs.  (t / t ) is also made. F is calculated as Edt . for various
times, this is known as F – curve. In dimensionless quantity, a plot of F Vs.  is also made. I is
calculated as I = 1 - F. A plot of I Vs.  and also I (=I/ t ) Vs. t are made. To find out the conversion
(X) for an irreversible I order reaction, the following equation is used.
1 – X =  exp(-kt) E dt
Where k = rate constant. It is assumed to be 0.05sec-1.

GRAPHS: Ct
1. E Vs. t 2. E Vs.  3. F Vs. t
4. F Vs.  5. I Vs. t 6. I Vs. 
7. exp(-kt) E Vs. t

RESULTS:
The above curves are drawn for the given annulus for the flow rate of water (___________ml/sec) and the
conversion predicted for k = 0.05sec-1 = ___________%.

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 Chemical Reaction Engineering

EXPERIMENT : 2 RTD STUDIES IN A SINE TUBE

AIM: To construct various curves such as E, E, F, F, I and I for the case of annular flow of water and
predict the conversion for a first order irreversible reaction of known rate constant.

THEORY: The residence time distribution (RTD) studies throw information on the flow pattern of a
fluid in a system. This is accomplished by the stimulus – response techniques i.e. a tracer is injected at
one point of the system and its concentration is analyzed at some another point. Usually, the tracer is so
chosen as to have similar properties of the main fluid and also lend itself for easy analysis. There are
several kinds of input among which the impulse input and step input are widely used. The response of the
former in the normalized form is known as the C curve. The response for the letter is called as the F
curve. I curve represents the internal age distribution.

APPARATUS: Sine tube, tracer injection device, measuring cylinder (250ml), tracer(NaOH solution),
burette, conical flask, test tubes (12 No.), stop watch, standard HCl etc.

PROCEDURE: In given annulus, a steady flow of water is maintained throughout the course of
investigation. A solution of around 2N NaOH is used as the tracer. About 2ml of the tracer is injected
through a syringe at the inlet of the annulus as quickly as possible and simultaneously, a stopwatch is
started. At regular interval of time, depending upon the flow rate, a small quantity of water (about 10ml)
from the outlet is collected in a test tube and in this way 12 samples are prepared. These are subsequently
analyzed for the concentration of NaOH using 0.1N HCl. The steady flow rate of water is also measured.
The volume of the annulus is 70ml.

OBSERVATION TABLE:
Sr no. Time B.R. Conc. C E = = F = F I I E*e-kt
(sec) (ml) gmol/l = c/Q Et t/ t
1
2
3
4
5
6

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CALCULATIONS: The concentration of the tracer is expressed as mol/lit (same as normality). A graph
is drawn between Concentration and Time in seconds and from such a graph the area Q under the curve is
found out as cdt [(mol/lit)sec]. In order to find E, the concentration at different time is divided by Q  E
= c/Q and a graph is drawn between E and t. this is known as E – curve. The unit of E is sec-1. the average
residence time t is calculated as (volume of annulus / volumetric flow rate of water ). In terms of
dimensionless quantities, a plot of E (= t E) Vs.  (t / t ) is also made. F is calculated as Edt . for various
times, this is known as F – curve. In dimensionless quantity, a plot of F Vs.  is also made. I is
calculated as I = 1 - F. A plot of I Vs.  and also I (=I/ t ) Vs. t are made. To find out the conversion
(X) for an irreversible I order reaction, the following equation is used.
1 – X =  exp(-kt) E dt
Where k = rate constant. It is assumed to be 0.05sec-1.

GRAPHS: C  t
1. E Vs. t 2. E Vs.  3. F Vs. t
4. F Vs.  5. I Vs. t 6. I Vs. 
7. exp(-kt) E Vs. t

RESULTS:
The above curves are drawn for the given annulus for the flow rate of water (___________ml/sec) and the
conversion predicted for k = 0.05sec-1 = ___________%.

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 Chemical Reaction Engineering

EXPERIMENT : 3 RTD STIDIES IN LAMINAR FLOW

AIM: To obtain the F – curve from the experimental E- curve and compare with theory for the given
laminar flow system.

THEORY: A tubular system with laminar flow can be taken as good approximate to segregate flow with
the assumption that the molecular diffusion is negligible. Since the flow is segregated and the velocity
profile is known, the residence time distribution can be calculated. It is of interest to compare the results
with those for mixed and plug flow systems.

APPARATUS: An empty tube of about 1cm diameter and 100cm length, tracer injected device (syringe)
, measuring jar (100ml), tracer (NaOH solution), burette, conical flask, test tubes, stopwatch, standard
solution of HCl etc…

PROCEDURE: Water is allowed to flow through the empty tube at steady flow .Care is taken as to
maintain laminar flow. A solution of NaOH of 2 N is taken as tracer. About 2ml of the tracer is injected
through a syringe at the inlet of the tube as quickly as possible and at the same time the stopwatch is
started. At regular interval of time depending upon the flow rate, a small quantity of water is collected at
the outlet and in this way 12 samples are collected to analyze. These samples are then analyzed against
the standard solution of 0.1N HCl. The steady flow of water is also measured.

PHYSICAL DATA:
THE VOLUME OF THE TUBE =150ml
DIAMETER OF THE TUBE = 1.2cm.
OBSERVATION TABLE:
Sr Time B.R. Conc. C E = = F = F F F F
no. (sec) (ml) gmol/l = c/Q Et t/ t (expt) (thro.) (mix) P.F.
1 1–0.25/2 1 – e-
2 1
3
4
5
6
7

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CALCUALATIONS: The concentration of the tracer is expressed as mol/lit. A graph is drawn between
the concentration Vs. time in seconds and from such a graph, the area (Q) under is curve is calculated as
Q = cdt [(mol/lit)sec]. In order to find E, the concentration at different time is divided by Q  E = c/Q;
E = = t E) Vs.  (t / t ) is also made. From such a graph F is calculated as
F =  Ed. A plot of F Vs.  is made. This is the F - curve. According to the theory F = 0 for 0   
0.5 and F = 1 – (0.25/2) for  > 0.5. Based on these equations, the theoretical curve is generated for
various values of  and compared with the experimental one. For mixed flow F = 1 – e- and for the plug
flow F = 0 for  <1and F = 1 for  1. The F -curve is generated for these ideal cases also and
compared with that for the laminar flow as in the present condition.
GRAPH: On a single graph paper, the following curves are drawn. C  t
1. F Vs.  (laminar flow – experimental data)
2. F Vs.  (laminar flow – theoretical data)
3. F Vs.  (mixed flow)
4. F Vs.  (plug flow)

RESULTS: The Reynolds number in the present experiment is _______________________thereby

ensuring laminar flow of fluid and above mentioned curves are drawn on a single graph sheet.

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 Chemical Reaction Engineering

EXPERIMENT : 4 AGITATED BUBBLE CONTACTOR

Aim: To study the kinetics of oxidation of Sodium Sulphite in an agitated bubble contactor by passing air
through it.

Theory: Bubble contactors are generally used in heterogeneous reactors where the surface area/volume of
liquid is quite low. It is more suited for reactions which take place in the bulk of the liquid phase. In the
semi-batch operation, the gas is continuously bubbled through the column of reacting liquid. The gas
concentration is more or less constant. It enters the bulk of liquid and reacts with it. If the rate of reaction
is proportional to the concentration of the substance in the liquid phase, Pseudo first reaction results.

Apparatus: Agitated bubble contactor, air supply, sodium sulphite solution of 0.1(N), Iodine solution of
0.02(N), Saturated sodium Thiosulphate solution, starch solution of 0.5% wt.

CHEMICAL REACTION:-
2Na2SO3 + O2  2Na2SO4
Na2SO3 + I2 + H2O  Na2SO4 + 2HI

PREPARATION OF THE SOLUTION REQUIRED:-

1) PREPARATION OF Na₂S₂O₃*5H₂O SOLUTION 0.02 (N):-
I. Take 100 ml of distilled water.
II. Add to the above 4.96 gm of sodium thiosulphate crystals and dissolve it to get a clear
solution.
III. Make it up to the 1000 ml.
IV. Store it in a amber colored bottle.
(NOTE:- EQUIVALENT WEIGHT =248)
2) PREPARATION OF 0.02 (N) I₂ SOLUTION:-
I. First prepare 0.03 (N) of I₂ solution.
(127*0.03*0.2=0.76 gm of I₂
0.76 * 6 = 4.57 gm of KI )
-Take 200 ml of distilled water.
-Add to the above 4.57 gm of potassium iodide(KI) and make a clear solution.
-To the above, add 0.76 gm of iodine (I₂) crystals. Dissolve it completely.

So , now 0.03 (N) solution of I2 is ready.

(NOTE:- ALWAYS TAKE 6 TIMES OF KI THEN I2 . )

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 Chemical Reaction Engineering

II. STANDARDIZATION OF I₂ SOLUTION:-

-Take 20 ml of I₂ sol. In a conical flask.
-Titrate it against a standard sol. of sodium thiosulphate till a pale yellow color
develops.
-Add a few drops of starch sol. (about 4 drops)
-Titrate further to the end point which is indicated by the blue color turning colorless.
Normality of iodine * V = normality of sodium thiosulphate *V
Nı₂ * 20 = 0.02 * V
Nı₂=________ (N) of I₂
( This will be nearer to 0.03(N) )
Now, dilute this solution such a way that,
the solution become 0.02 (N) of I₂.
And store it in amber colored bottle.
3) PREPARATION OF STARCH SOLUTION:-
I. Take 100 ml of water. Heat it till it start boiling.
II. Remove the flame and add immediately 0.5 gm of soluble starch and thoroughly stir.
III. Cool the above to room temperature.
4) PREPARATION OF SODIUM SULPHITE SOLUTION 0.05 (N):-
I. Take 100 ml of water and add to it 1.575 gm of Na₂SO₃ and stir well to get a clear
solution.
II. Make it up to 1000 ml.
III. Store the above in an air tight container.

Procedure:
 Take 500ml the sodium sulphite solution in the bubble contactor.
 Now, start the flow of air and a stopwatch is started simultaneously.
 After 10 minute take a first sample of 10 ml from bubble contactor and add it into beaker which
already contains 40 ml of water.
 From this take 10 ml, add 15 ml of 0.02 (N) iodine solution and titrate it against 0.02 (N) of
sodium thoisulphate till a pale yellow color develops.
 Add a few drops of starch sol.(about 4 drops) to get dark blue color and titrate further which gives
colorless solution from blue color.
 Note the titer value.

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 Chemical Reaction Engineering

 Take 10 ml of the sample at the interval of 10 minutes up to 60 minutes and repeat the above
procedure.
 This method is called the back titration and is used for the analysis of sodium sulphite
concentration.
Calculation:
Let V ml be the titer value of the std. solution of sodium thiosulphate.
If Vs ml is the actual volume of I2 sol. consumed by sodium sulphite solution, Then ,
(15 - Vs)* normality of I2 = V * normality of sodium thiosulphate
From this, Vs can be calculated. Therefore,
Vs * normality of I2 = 10 * normality of sodium sulphite
This normality is calculated multiplied by 5.
This value corresponds to the normality of sodium sulphite in the bubble column.
Dividing this value by 2, gives the concentration in mol/lit.
A plot of ln(Cₐₒ/Cₐ) Vs time(t) gives clue about the kinetics. If it is a straight line, the slope gives the
psedo -first order rate constant.
Observation Table:
Sr.no. Time Burette reading Normality Cᴀ ln(Cᴀo/Cᴀ)
(min) ( diff.)(ml) (N) (mol/lit)

0 00

1 10

2 20

3 30

4 40

5 50

6 60

Graphs:
(a) CA  t (2) ln(Cₐₒ/Cₐ) Vs time(t)

Results:
The Pseudo First order rate constant at ______C = ______min-1.

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 Chemical Reaction Engineering

EXPERIMENT : 5 TANKS IN SERIES MODEL

AIM: To apply tanks in series model to annular flow of water.

THEORY: In tanks in series model, the actual system is simulated by a certain numbers (N) of ideal
stirred tanks in series. The total volume of the tanks is same as that of the system under study. Thus for
given flow rate of fluid, the total mean residence time ( t ) is also the same. The mean residence time per
tank is ( t /N). When N tends to infinity, plug flow is achieved; for N =1, perfect back-mix condition is
achieved.
APPARATUS: Annulus, tracer injecting device (syringe), measuring cylinder (100ml), tracer (NaOH),
burette, conical flask, test tubes, stopwatch, standard HCl etc…
PROCEDURE: Water is allowed to flow through the annulus steadily. About 2ml of tracer is injected
which is approximately 2N NaOH solution through a syringe at the inlet of the annulus as quickly as
possible and at the same time a stopwatch is started. At regular interval of time depending upon flow rate
the samples of the out coming water is taken for the analysis. In the same way 12 different samples are
collected form the system to analyze it against the standard solution of 0.1N HCl. The steady flow rate of
the water is also noted. The volume of the system is taken as = 55ml.
OBSERVATION TABLE:
Sr Time B.R. Conc. C E = = 2 E E = e-
no. (sec) (ml) gmol/l = c/Q Ct t/ t (theo.)
1
2
3
4
5
6
7
8
9
10
11
12

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 Chemical Reaction Engineering

CALCULATIONS: The concentration of the tracer is expressed as mol/lit. A graph is drawn between the
concentration Vs. time in seconds and from such a graph, the area (Q) under is curve is calculated as Q =
cdt [(mol/lit)sec]. In order to find E, the concentration at different time is divided by Q  E = c/Q; E =
t E) Vs.  (t / t ) is also made. According to tanks in series model
E = N(N)(N -1)exp(-N)/(N - 1)!
Where N = number of tanks in series.
 = dimensionless time.
The variance is given by 2 = 1/N. 2 is first calculated for the experiment E - curve using the
equation,
2 = [2Ed] –1
In order to apply the tanks in series model it is necessary to fix the value of N before generating the
theoretical curve. This is easily accomplished by putting N = 1/ 2. If this is a fraction, it is rounded off
to the nearest integer. The theoretical E - curve is now generated and compared with the experimental
one.
GRAPH: E Vs.  (both experimental and theoretical on a single graph) C  t

RESULT: The tanks in series model is applied to annular flow of water and the number of equivalent
tanks in series: ____________________

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 Chemical Reaction Engineering

EXPERIMENT : 6 DISPERSION MODEL

AIM: To obtain the dispersion number in the case of relatively low flow rate (30 – 40ml/min) and for
high flow rate (60 – 80ml/min) of water through a packed bed using the dispersion model and
subsequently the dispersion coefficient.

THEORY: Consider the plug flow of a fluid on the top of which is superimposed degree of back mixing,
the magnitude of which is independent of position within the vessel. This condition implies that there
exist no stagnant pockets and no gross bypassing or short circulating of fluid in the vessel. This is called
as DISPERSION MODEL or simply the plug flow model. This model is generally valid for packed beds
for which deviation from the ideal plug flow is not much owing to the presence of packing.

APPARATUS: Packed bed, tracer injecting device (syringe), measuring cylinder (100ml), tracer
(NaOH), burette, conical flask, test tubes, stopwatch, standard HCl etc…

PROCEDURE: Water is allowed to flow through the packed bed steadily. (Maintain the flow rates
between 30 – 40ml/min). About 2ml of tracer is injected which is approximately 2N NaOH solution
through a syringe at the inlet of the packed bed as quickly as possible and at the same time a stopwatch is
started. At regular interval of time depending upon flow rate the samples of the out coming water is taken
for the analysis. In the same way 12 different samples are collected form the system to analyze it against
the standard solution of 0.1N HCl. The steady flow rate of the water is also noted.
OBSERVATION TABLE:
Sr Time B.R. Conc. C E = = 2 E E = e-
no. (sec) (ml) gmol/l = c/Q Et t/ t (theo.)
1
2
3
4
5
6
7
8
9

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CALCULATIONS: The concentration of the tracer is expressed as mol/lit. A graph is drawn between the
concentration Vs. time in seconds and from such a graph, the area (Q) under is curve is calculated as Q =
cdt [(mol/lit)sec]. In order to find E, the concentration at different time is divided by Q  E = c/Q; E =
t E) Vs.  (t / t ) is also made.
The variance is given by,
2 = [2Ed] –1
Using the graphical integration, the first term of the expression on the R.H.S. is evaluated and 2 is
computed. According to the dispersion model, for small extent of dispersion 2 = 2[D/UL] where D =
dispersion coefficient,cm2/sec; L = length of the packed bed, cm; U = superficial velocity/voidage of the
bed. This is same as flow rate of water/[(cross sectional area)(voidage of bed)], cm/sec. from the above
equation for 2, the value of D/UL and subsequently D are found out. Also from the dispersion number,
the theoretical E - curve is generated using the following equations and compared with the experimental
one.
E = 1/[2( D/UL)] exp [1(1 - 2)/(4 D/UL)]
PHYSICAL DATA: volume of the tube = 58ml
Volume of the packing = 22ml
Cross section area of the tube = 1cm2
Length of the packed bed = 64cm.
Bed voidage = 0.3

GRAPH: E Vs.  (both theoretical and experimental) C  t

RESULTS: For the flow rate of ____________ml/sec of water, the dispersion number D/UL
is____________. The dispersion coefficient (D) = ______________cm2/sec. also the E - curves, both
theoretical and experimental are compared as shown in the graph.

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 Chemical Reaction Engineering

EXPERIMENT : 7 CASCADE OF STIRRED VESSELS

AIM: To obtain the response of a cascade of stirred vessels for a step change in the concentration of
entering stream and compare the theoretical results.

THEORY: The cascade consist of a number of well stirred vessels all connected in series. The output of
one vessel will become the input for the second one. The response become more and more sluggish as
number of stirred vessels, it is possible to find out the response analytically when they are all
interconnected. When an increase in the number is made, the plug flow pattern tends to develop.

APPARATUS: two stirred vessels, , measuring cylinder (100ml), NaOH, burette, conical flask, test
tubes, stopwatch, HCl etc…
PROCEDURE: The cascade is chosen to consist of two stirred vessels in series. They contains 0.2N HCl
which is kept well stirred. At time t = 0, water is allowed to flow through the cascade in a steady manner
and at regular interval of time, depending on the flow rates, water is withdrawn from the outlet of the
second vessel in a test tube and in this manner 12 samples are collected. These samples are then analyzed
against 0.1N NaOH solution. The steady flow rate is also noted.
OBSERVATION TABLE:
Sr Time B.R. Conc. C E = = 2 E E = e-
no. (sec) (ml) gmol/l = c/Q Et t /t (theo.)
1
2
3
4
5
6
7
8
9
10
11
12

CALCULATIONS: Ci = initial concentration of HCl = 0.2N

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 Chemical Reaction Engineering

Cf = final concentration of HCl = 0N

C = concentration of HCl at any intermediate time
F = (c - ci)/(cf -ci) = 1 – (c/0.2)
F is obtained for various  = (t/ t ) where is the average residence time. This is equal to (volume of all
vessels in series/volumetric flow rate of water). A plot of F Vs.  is made. The theoretical curve is
generated as F = 1 – [exp.(-2)](1 + 2) for two vessels in series.

GRAPHS: F Vs.  (BOTH THEORETICALLY AND GRAPHICALLY) C  t

RESULTS: The response of the cascade of stirred vessels for a step change is experimentally found out
and compared with the theory as shown in the graph.

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 Chemical Reaction Engineering

EXPERIMENT : 8 HETEROGENEOUS REACTION

AIM: To evaluate the mass transfer effect relative to the intrinsic kinetics for ethyl acetate and sodium
hydroxide system conducted in a heterogeneous manner.
THEORY: Heterogeneous reactions requires at least two phases for the reaction to be proceed. It is
observed that one reactant crosses the interface and then meets the other to effect the reaction. Mass
transfer effect is thus brought into the picture followed by intrinsic kinetics.
APPARATUS: Coincal flask – 150ml (4 Nos.), 100ml conical flask (reactor), magnetic stirrer, measuring
cylinder, burette, chemicals such as NaOH, CH3COOC2H5, C6H6.
PROCEDURE:
(1) HOMOGENEOUS REACTION: Prepare 100ml of 0.2N NaOH solution and 0.2N ethyl acetate
solution in water. Take 10ml of NaOH solution in the reactor. Add a few drops of phenolphthalein as
indicator. To this ass 10ml of ethyl acetate solution and kept the contents of the reactor well stirred. After
15sec., add about 50ml of water to the reactants in order to reduce the rate of reaction. Afterwards, titer
the contents against the standard solution of 0.1N HCl. Form the titer value calculate the concentration of
NaOH. Repeat the above experiment for the reaction time of 30, 45, 60 and 75 seconds.
(2) HETEROGENEOUS REACTION: Prepare 100ml of 0.1N NaOH solution and 0.1N ethyl acetate
solution in water. Take 10ml of NaOH solution in the reactor. Add a few drops of phenolphthalein as
indicator. To this ass 10ml of ethyl acetate solution and kept the contents of the reactor well stirred. After
15sec., add about 50ml of water to the reactants in order to reduce the rate of reaction. Afterwards, titer
the contents against the standard solution of 0.1N HCl. Form the titer value calculate the concentration of
NaOH. Repeat the above experiment for the reaction time of 6, 9, 12 and 15 minutes.
OBSERVATION TABLE: (Heterogeneous as well as homogeneous reaction)
Sr no. Time B.R. Conc.
(sec) (ml) gmol/l
1
2
3
4
5
6

GRAPHS AND CALCULATIONS: Plot the concentration of NaOH (CA) Vs. time both in the
homogeneous and heterogeneous reactions are at t 1 and t2 respectively. (t2 – t1) gives the mass transfer

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 Chemical Reaction Engineering

effect. T1 gives the intrinsic kinetics. Therefore the ratio (t2 – t1)/ t1 gives the relative resistance to mass
transfer to the intrinsic kinetics. Such ratio is obtained for about 4 values of C A within the range of C A
obtained. The results are tabulated.
RESULTS: The relative resistance of mass transfer to the intrinsic kinetics is evaluate at various
concentration levels of the reactants (NaOH) for the heterogeneous system comprising of NaOH in
aqueous solution and ethyl acetate in Benzene phase.

APPENDIX:
1. 100ml of 0.2N & 0.1N NaOH solution is prepared by diluting suitably a concentrated NaOH solution.
2. 0.2N diluting with water 2ml of ethyl acetate such that the total volume is 100ml makes ethyl acetate
solution in water.
3. 0.1N diluting with benzene 1ml of ethyl acetate such that the total volume is 100ml makes ethyl
acetate solution in benzene.

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 Chemical Reaction Engineering

EXPERIMENT : 9 RTD STUDIES IN A SINGLE STIRRED TANK

AIM: To compare the experimental and theoretical E - curve and also generate the E-curve for the given
stirred tank.
THEORY: The E - curve is experimentally obtained from the response of an impulse input to the
system. F- curve is corresponds to the response for a step input. From E , F- curves can be generated
even without experiments.
APPARATUS AND PROCEDURE: The vessel is of 40cm diameter and 60cm height. The wall
thickness is 4mm. The material of construction is SS316. There are 4 baffles each of width 3.5cm and
thickness 4mm. They provide good turbulence during agitation, which is effected by a propeller type high
speed stirrer. The length of the agitator shaft can be adjusted. The vessel has an outlet pipe near the
bottom and the flow of liquid is controlled by SS gate valve. The top of the vessel is open to atmosphere.
The impulse of reactor is introduced at the top of the liquid and the samples are collected at the bottom
periodically for analysis.
EXPERIMATL DATA:
TIME CONC OF
TRACER
0.0 0.0
2.5 10.1
5.0 10.7
10.0 8.2
15.0 6.5
20.0 5.1
30.0 3.0
40.0 1.7
50.0 0.9
65.0 0.2
80.0 0.0

GRAPHS: E Vs.  (both theory and expt.) C  t

F Vs.  (both theory and expt.)
RESULTS: The theoretical and experimental E and F curves are compared as shown in the graph.

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EXPERIMENT : 10 RTD STUDIES IN HELICAL COIL TYPE REACTOR

AIM: To construct various curves such as E, E, F, F, I and I for the case of flow of water through a
helical coil type reactor using step change in concentration and predict the conversion for a first order
irreversible reaction of known rate constant.

THEORY: Step change is one of stimulus response technique by which the reactor’s behavior can be
predicted. There are several kinds of input among which the impulse input and step input are widely used.
The response of the later in the normalized form is known as the F curve.
APPARATUS:
Reactor: 0.7lit volume and made up of SS, feed tanks 2nos SS 20lit, feed circulation by compressed air,
flow: Rota meter 2Nos, piping SS & PVC, pressure regulator 0-2kg pressure gauge bourdon gauge, Air
compressor 0.5hP, CFM with motor and automatic pressure switch

Compressor 2 CFM, 0.5hP, single stage, 40lit storage capacity with pressure gauge, flow control valve,
safety valve, drain valve, guard etc, MS frame with powder coating.
Measuring cylinder (250ml), NaOH solution, burette, conical flask, test tubes (12 No.), stop watch,
standard HCl etc.

PROCEDURE: First fill the storage tanks with water and 0.1 N NaOH solutions. Then close the vent
valves of the storage tanks. Start compressor and build up the air pressure as required. In given helical coil
reactor, a steady flow of water is flowed and maintained throughout the course of investigation with the
help of a compressed air. At time t = 0, a step change in concentration is given by stopping water flow and
allowing the NaOH flow through the reactor. At regular interval of time, depending upon the flow rate, a
small quantity of sample (about 10ml) from the outlet is collected in a test tube and in this way 12
samples are prepared. These are subsequently analyzed for the concentration of NaOH using 0.1N HCl.
The steady flow rate of is also measured.
OBSERVATION TABLE:
Sr no. Time B.R. Conc. F E= = F = F I I E*e-kt
(sec) (ml) gmol/l = C/Co dF/dt t/ t
1
2
3

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 Chemical Reaction Engineering

4
5
6
7
8
9
10
11
12

CALCULATIONS: The concentration of NaOH in outlet is expressed as mol/lit (same as normality).

The ratio of outlet to inlet concentration is calculated. This ratio is nothing but the values of F at different
time intervals. Plot F versus time graph. In order to find E, draw tangents at different time intervals on
this plot and find out slopes(i.e. dF/dt). These slopes are the values of E at corresponding time instants.
Plot then E versus t. This is known as E – curve. The unit of E is sec-1. The average residence time is
calculated as (volume of helical coil / volumetric flow rate of water ). In terms of dimensionless
quantities, a plot of E (= t E) Vs.  (t / t ) is also made.. I is calculated as I = 1 - F. A plot of I Vs. 
and also I (=I/ t ) Vs. t are made. To find out the conversion (X) for an irreversible I order reaction, the
following equation is used.
1 – X =  exp(-kt) E dt
Where k = rate constant. It is assumed to be 0.05sec-1.

GRAPHS: C  t
1. E Vs. t 2. E Vs.  3. F Vs. t
4. F Vs.  5. I Vs. t 6. I Vs. 
7. exp(-kt) E Vs. t

RESULTS:
The above curves are drawn for the given helical coil for the flow rate of water (___________ml/sec) and
the conversion predicted for k = 0.05sec-1 = ___________%.

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 Chemical Reaction Engineering

EXPERIMENT : 11 RTD STUDIES IN STRAIGHT TUBE TYPE REACTOR

AIM: To construct various curves such as E, E, F, F, I and I for the case of flow of water through a
straight tube type reactor using step change in concentration and predict the conversion for a first order
irreversible reaction of known rate constant.

THEORY: Step change is one of stimulus response technique by which the reactor’s behavior can be
predicted. There are several kinds of input among which the impulse input and step input are widely used.
The response of the later in the normalized form is known as the F curve.
APPARATUS:
Reactor: Reactor 0.7lit SS, feed tanks 2nos SS 20lit, feed circulation by compressed air, flow: Rotameter,
piping SS & PVC, pressure regulator 0-2kg.
Compressor 2 CFM, 0.5hP, single stage, 40lit storage capacity with pressure gauge, flow control valve,
safety valve, drain valve, guard etc, MS frame with powder coating.
Measuring cylinder (250ml), NaOH solution, burette, conical flask, test tubes (12 No.), stop watch,
standard HCl etc.
PROCEDURE: First fill the storage tanks with water and 0.1 N NaOH solutions. Then close the vent
valves of the storage tanks. Start compressor and build up the air pressure as required. In given straight
tube reactor, a steady flow of water is flowed and maintained throughout the course of investigation with
the help of a compressed air. At time t = 0, a step change in concentration is given by stopping water flow
and allowing the NaOH flow through the reactor. At regular interval of time, depending upon the flow
rate, a small quantity of sample (about 10ml) from the outlet is collected in a test tube and in this way 12
samples are prepared. These are subsequently analyzed for the concentration of NaOH using 0.1N HCl.
The steady flow rate of is also measured.
OBSERVATION TABLE:
Sr no. Time B.R. Conc. F E= = F = F I I E*e-kt
(sec) (ml) gmol/l = C/Co dF/dt t /t
1
2
3
4
5
6

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 Chemical Reaction Engineering

7
8
9
10
11
12

CALCULATIONS: The concentration of NaOH in outlet is expressed as mol/lit (same as normality).

The ratio of outlet to inlet concentration is calculated. This ratio is nothing but the values of F at different
time intervals. Plot F versus time graph. In order to find E, draw tangents at different time intervals on
this plot and find out slopes(i.e. dF/dt). These slopes are the values of E at corresponding time instants.
Plot then E versus t. This is known as E – curve. The unit of E is sec-1. The average residence time is
calculated as (volume of straight tube / volumetric flow rate of water). In terms of dimensionless
quantities, a plot of E (= t E) Vs.  (t / t ) is also made.. I is calculated as I = 1 - F. A plot of I Vs. 
and also I (=I/ t ) Vs. t are made. To find out the conversion (X) for an irreversible I order reaction, the
following equation is used.
1 – X =  exp(-kt) E dt
Where k = rate constant. It is assumed to be 0.05sec-1.

GRAPHS: C  t
1. E Vs. t 2. E Vs.  3. F Vs. t
4. F Vs.  5. I Vs. t 6. I Vs. 
7. exp(-kt) E Vs. t

RESULTS:
The above curves are drawn for the given straight tube reactro for the flow rate of water
(___________ml/sec) and the conversion predicted for k = 0.05sec-1 = ___________%.

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 Chemical Reaction Engineering

EXPERIMENT : 12 Adiabatic Batch Reactor

Aim: Study of a catalytic homogeneous reaction in a batch reactor under adiabatic condition.
To study the hydrolysis of acetic anhydride with water in presence of an acid catalyst (H2SO4). To predict
the degree of conversion from time temperature data.

Introduction:
Industrial scale chemical reactions are frequently complicated by variations occurring in the temperature
of the reactor during operation. Temperature changes always affect the physical properties of the reaction
mixture and the reaction rate constant.

The temperature dependence specific reaction rate constant k, is expressed in terms of Arrhenius equation
as:
 E 
k  k o exp  
 RT 
Theory:
In case of an exothermic reaction, the heat relieved by the chemical reaction increases the reaction
temperature, which in turn increases the reaction rate constant and hence the rate of reaction. Degree of
conversion, x, is correspondingly effected.
For non-isothermal operation of a batch reactor, the analysis is carried out by using the basic
material balance equation in conjunction with an energy balance and an Arrhenius type expression for the
reaction rate.

A+BC

Reaction:
(CH3CO)2O + H2O  2CH3COOH H = -58562 J/mol

The reaction takes place in presence of solvent acetic acid is of 1st order.
Reaction rate constant, k for this reaction is expressed as:
ln(k) = 16.0502 – 5344.5/T, where T is the reaction temperature in K, k is in min-1, average specific heat
of reaction mixture may be taken as Cpavg = 3768.3 J/kg K

The energy balance around the reactor is:

Heat transfer  Heat of  Energy accumuatio n 

   
from Surrounding  Reaction  in reactor 

On substituting corresponding quantities the energy equation is:

UATs  T dt  (rA )V R Hdt  mC p dT
UATs  T dt  n A HdX  mC p dT
Where
U = overall heat transfer coefficient between the reactor surface and the ambient atmosphere
A = Heat transfer area
TS = temperature of heat coil
T = reaction mixture temperature
VR = volume of reactor

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 Chemical Reaction Engineering

X = fractional conversion
m = mass of reaction mixture
nA = initial moles of A

For an Adiabatic Process:

The energy equation reduces to
 n A HdX  mC p dT
 n H  …..(1)
T  To   A X
 mC pavg 
 
Corresponding Batch Time for first order reaction is given by:
x x
dx dx
t  C A, o   …..(2)
0
kC A , 0 (1  x ) 0
k (1  x )
where
 E 
k  k o exp   …..(3)
 RT 
From the observed values of temperature (T) as a function of time (t), degree of conversion, x is obtained
from equation 1 and corresponding reaction rate constant; k is obtained from equation 3. Knowing value
of x, the required batch time for the first order reaction for the desired degree of conversion x is obtained
from equation 2. Equation 2 can be solved graphically or by R-K method.

Experimental Procedure:
1. Preparation of Chemicals
Solution A
Acetic anhydride = 200ml
Acetic acid = 300ml
Solution B
Water = 210ml
H2SO4 = 0.1% wt of water
2. Start the stirrer.
3. Start the temperature indicator
4. Put solution A and solution B simultaneously into the reactor and start the stopwatch.
5. Record the reaction temperature immediately after the reactor has loaded at t = 0, this is T0.
6. Record time – temperature data till around 60C.
7. Stop the stirrer and cut the power supply and gently remove the contents of the reaction mixture.
8. Wash the reactor with water.

Formulae:
5344.5
ln k   16.0502 
T
 n H 
T  To   A X
 , mC p , avg 
 

Observations and Calculation:

Properties of reactants:
Acetic anhydride

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 Chemical Reaction Engineering

MW = 102.09
Density = 1.082 gm/cc
Acetic acid
MW = 60.05
Density = 1.049 gm/cc
Water
MW = 18.01
Density = 1 gm/cc
Volume of acetic anhydride taken = 200ml
Volume of acetic acid taken as solvent fro acetic anhydride = 300ml
Volume of acidified water = 210ml
Moles of acetic anhydride taken = 2.116gmol
Moles of acetic acid taken = 2.116gmol
Moles of water taken = 2.116gmol
Heat of reaction = -58562 J/gmol of acetic anhydride reacted
Average specific heat of reaction mixture Cpavg = 3768.3 J/kg K
Average density of mixture = 1.0448 gm/cc
Total reaction mixture = 741.1gm

Observation Table:
Time, 0 2 4.3 6.2 8.1 10.2 12 13
min
Reaction 299 300 309 314 321 329 344 361
T, K

T = To + 44.378X

Calculate X = ________
Calculate k = _________
Calculate batch design parameter 1/k(1-x) = __________

Plot:
(1) T Vs t (2) k Vs T (3) X Vs. t (4) 1/k(1-X) Vs t
Nomenclature:
T = Temperature of reaction mixture at t, To = initial Temperature at t= 0, H = Heat of reaction, t = time,
k = reaction rate constant, min-1, X = conversion, m = total mass of reaction mixture, nA = moles of
reactant A, Cpavg = average heat capacity of mixture.

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 Chemical Reaction Engineering

SIMULATION OF CATALYTIC REACTION USING HYSYS

Aim: The production of propylene Glycol. The ethylene glycol is produced by reacting propylene oxide
with water in CSTR with 96% minimum conversion. This is a liquid phase reaction. The reactor outlet is
then sent to a plate column where glycol is recovered from the bottom of the tower.
H2O + C3H6O  C3H8O2

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