Foreword

Welcome to value-conscious company. We are proud of the advanced engineering and

quality construction of each equipment we manufacture.

This manual explains the working of equipment. Please read it thoroughly and have all
the occupants follow the instructions carefully. Doing so will help you enjoy many years
of safe and trouble free operation.

When it comes to service remember that K.C. Engineers knows your equipment best
and is interested in your complete satisfaction. We will provide the quality maintenance
and any other assistance you may require.

All the information and specifications in this manual are current at the time of printing.
However, Because of K.C. Engineers policy of continual product improvement we
reserve the right to make changes at any time without notice.

Please note that this manual explains all about the equipment including options.
Therefore you may find some explanations for options not installed on your equipment.

You must follow the instructions and maintenance instructions given in the manual
carefully to avoid possible injury or damage. Proper maintenance will help ensure
maximum performance, greater reliability and longer life for the product.

K.C. Engineers
 Contents

1. Objective …………………………………… 1

2. Aim …………………………………… 1

3. Introduction …………………………………… 1

4. Theory …………………………………… 1

5. Description …………………………………… 4

6. Utilities Required …………………………………… 4

7. Experimental Procedure …………………………………… 5

8. Observation & Calculation …………………………………… 5

9. Nomenclature …………………………………… 7

10. Precautions & Maintenance Instructions …………………………………… 7

11. Troubleshooting …………………………………… 8

12. References ……………………………………. 8

Isothermal Batch Reactor

 ISOTHERMAL BATCH REACTOR

1. OBJECTIVE:
To Study of a Non-Catalytic Homogeneous reaction in an isothermal batch
reactor.

2. AIM:
To determine the reaction rate constant (k) for the given saponification
reaction of ethyl acetate in aqueous sodium hydroxide solution.
To study the effect of temperature on k and determine the activation energy.

3. INTRODUCTION:
A Batch Reactor is a closed system with no input and output streams. A batch
reactor can operate under the following conditions:
− Isothermal (temp. of reaction mass remains constant)
− Perfectly mixed (composition of the reaction mixture is uniform through
out)
− Constant volume (volume of the reaction mixture within the reactor
remains constant; there is no appreciable change in the density of reaction
mass)

4. THEORY:
In a homogeneous reaction, all the reactants remain in single phase. The rate
of reaction for such a reaction is expressed as moles of Product formed per
unit volume of reaction mixture per unit time. For a first order unidirectional
reaction:
k
A → Product
Rate of reaction can also be expressed as moles of A disappearing per unit
volume per unit time.
1 dN A
− rA =
V dt
k NA
Also − rA = k C A =
V

Isothermal Batch Reactor 1

 Combining these two equations yield.
ln N A = ln N Ao − − k t or N A = N Ao e − kt
or in terms of Conc.
1 N
C A = C Ao e − kt & t = ln Ao
k NA
NAo = No. of moles of A at t=0
NA = No. of moles of A at t=t
For second order unidirectional reaction
2A 
→ Product
1 dN A
− = k C A2
V dt Slope = k
1
1 1 CA
= kt +
CA C Ao 1
Intercept =
C Ao
V  1 1 
t=  − 
k  N A N Ao  t

If we plot 1/CA vs t we must get a straight line with slope = k and intercept = 1/CAo
For second order reaction:
A+B
→ Product
1 dN A k
− = k CA CB = 2 N A N B
V dt V
If NAo = NBo then NA =NB for all t
It reduces to: 2A 
→ Product
Degree of conversion X is defined as:
N Ao − N A
X=
N Ao

And N B = N Bo − N Ao X for NAo ≠ NBo

V N N 
t= ln  A Bo 
k ( N Ao − N Bo )  N Ao N B 

The effect of Conc. on the rate of reaction is generally determined

experimentally in a batch reactor by studying the rate of reaction at constant
temperature. The interpretation of the kinetic data involves a trial and error
procedure. A kinetic model is first assumed and the experimental observed
conversion – time rate is matched with the selected model. The reaction rate

Isothermal Batch Reactor 2

 constant is a strong function of reaction temperature. The temperature
dependence of k is expressed in terms of Arrhenius equation:
k = A e − E A / RT
A = frequency factor or Arrhenius constant
EA = activation energy
R = gas law constant
This equation can be written in the form:
− EA  1 1 
ln k =  −  + ln k o
R  T To 

Where To = mid temp. For temperature range considered

k o = A e − E A / RTo
Thus EA/R may be evaluated from the slope of a plot of ln k vs (1/T – 1/To).
The intercept ln ko is evaluated at (1/T – 1/To) = 0 and A is calculated from the
definition of ko. Alternatively a plot of ln k vs 1/T shall also yield EA & A.

0.7

lnko

lnk Slope= -EA/R

0.001
-11 15
1 1 
 −  x10 3 K −1
 T To 
R = 8.314 J/g mole K
R = 1.98 cal/g mole K
E = J/g mole, cal/g mole
A = min-1 or s-1
If k is known at four temps: T1, T2, T3, T4.
(T1 + T2 + T3 + T4 )
Then To =
4
In case of second order reversible reaction with CAo = CBo

Isothermal Batch Reactor 3

 K1
A + B C + D
K2

 X − (2 X Ae − 1) X A   1 
ln Ae  = 2 k1  − 1C Ao t
 X Ae − X A   X Ae 
C Ao − C A
XA =
C Ao
XAe = fractional conversion at equilibrium
Saponification of Ethyl acetate & NaOH:
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
40 gm 88 gm 82 gm 46 gm
A + B C + D

5. DESCRIPTION:
The set up consists of a Reactor fitted in a constant temperature water bath.
One stirrer is fitted for mixing the reactants in reactor and other is fitted in
water bath to keep the uniform temperature throughout in the bath. The
temperature of bath can be maintained from ambient to 90°C with the help of
Digital Temperature indicator Cum Controller. Samples can be taken out with
the help of a sampling pipette.

6. UTILITIES REQUIRED:
Electricity Supply: Single Phase, 220 V AC, 50 Hz, 1.5 kW with earth
connection
Water Supply.
Drain.
5 conical flasks
Measuring cylinder
Burette
Stop watch
CHEMICALS: QUANTITY:
N/10 NaOH 1 Ltr.
N/10 HCl 1 Ltr.
Ethyl acetate 1 Ltr.
Indicator (phenolphthalein) Few drops

Isothermal Batch Reactor 4

7. EXPERIMENTAL PROCEDURE:
1. Prepare a solution of N/10 ethyl acetate by mixing 8.8 gm (or 9.8 ml at
20°C) of ethyl acetate in 1L of solution.
2. Prepare a solution of N/10 NaOH by dissolving 4 gm/1L of solution.
3. Prepare a solution of N/10 HCl for the titration.
4. Use phenolphthalein as indicator.
5. Take 6 Nos. of 250ml beakers and put 20ml of N/10 HCl in each beaker.
6. Take N/10 NaOH in the burette.
7. Adjust the temperature of water bath at 50°C.
8. If the volume of reactor is 1L then take 400ml each of N/10
CH3COOC2H5 and N/10 NaOH in two separate flasks and keep these in
the water bath for about 15 min.
9. Transfer these solutions quickly in the batch reactor. Start immediately the
mixer and the stop watch.
10. At regular intervals of 3-5 min withdraw 10ml of reaction mixture and put
it in the marked beakers containing N/10 HCl. Take at least 6 samples at
regular interval of time.
11. Transfer the solution from beakers to the conical flasks, and titrate the
excess N/10 HCl in each flask using N/10 NaOH from burette and
phenolphthalein as indicator.
12. Record the reaction temperature.
13. Equilibrium conversion can be determined at reaction time of 1/2 hr.
14. In order to study the effect of temp. On K, the above steps may be
repeated at temp.=35°C and 50°C. All the reactants must be pre-heated in
the water bath before mixing in the reactor.

8. OBSERVATION & CALCULATIONS:

DATA:

R = ------------ cal/g mol K

CAo = ------------ g mol/L
VHCL = ------------ ml
VSAMP = ------------ ml
NNaOH = ---------- g mole/L

Isothermal Batch Reactor 5

 NHCL = ---------- g mole/L

OBSERVATION:

VNaOH = ---------- ml

CALCULATIONS:
V HCL N HCL
HCLO = , g mole = ---------------- g mole
1000
(V NaOH N NaOH )
HCLR = HCLO − , g mole = ----------------- g mole
1000
HCLR
CA = × 1000 , g mole/L = ----------------------- g mole/L
VSAMP

(C Ao − C A )
XA= = ---------------
C Ao

S. No. t XA/ [1-XA]2

2
3
4

Plot t vs. XA/ [1-XA]2 on a simple graph, the slope is = 1/ (K CAo); from the
slope find K and report K at the reaction temp.

CALCULATION FOR ACTIVATION ENERGY (EA):

Isothermal Batch Reactor 6

 S. No. T, K K, L/g mole (T-1-To-1),
min K-1
1

2
3
4

Plot K vs (1/T-1/To), K-1 on a simple graph

− EA
slope = = ------------
R
E A = slope × R , cal/g mole = --------------- cal/g mole

9. NOMENCLATURE:
CA = Conc. of unreacted NaOH in the reactor, g mole/L
CAo = Initial Conc. of NaOH in the feed mixture, g mole/L
D = Reactor diameter, m
EA = Activation energy, cal/g mol
HCLO = Amount of HCL taken for quench, g mole
HCLR = Amount of HCL reacted with NaOH, g mole
K = Rate constant, L/g mol min
L = Effective height of liquid in the reactor, m
NHCL = Number of moles of HCL used, g mole
NNaOH = Number of moles of NaOH used, g mole
R = Real gas constant, cal/g mol K
T = Reaction temperature, K
To = Initial temperature of solution before heating, K
VR = Reactor volume, L
Vo = Volumetric feed rate, LPH
VHCl = Volume of N/10 HCl taken for quench, ml
VSAMP = Volume of sample taken, ml
VNaOH = Volume of NaOH used for neutralizing, ml
XA = Degree of conversion,
τ = Residence time, min

Isothermal Batch Reactor 7

10. PRECAUTIONS & MAINTENANCE INSTRUCTIONS:
1. Measure the exact volume of water and weigh the chemicals.
2. Always use clean water and good quality chemicals and standard solution
for titration.
3. Use electronic balance for weighing of chemicals. Don’t mix the droppers
of different chemicals.
4. Keep close all the drain valves and vent valve should open while filling
the reactant in feed tanks.
5. Flow should not be disturbed during the experiments.
6. Handle the chemicals carefully.
7. Don’t ON heater switch before filling the water in the bath.
8. There should be no air in the flow during experiment.

11. TROUBLESHOOTING:
1. If there is any leakage tight that part or remove that and fix that again after
wrapping Teflon tape.
2. If D.T.C display ‘1’ on display board it means sensor connection is not
OK tight that.
3. If switch ON the heater but temperature can’t rise but panel LED is ON it
means bath heater had burned replace that.

12. REFERENCES:
1. Octave Levenspiel, “Chemical reaction engineering,”3rd ed., John Wiley &
Sons, NY, 2001, Page 91-93.
2. Coulson & Richardson, “Chemical Engineering Vol-3” 4th ed, Asian Books
Pvt.Lt, ND, 1991, Page 3-4, 17-18, 27-28, 63-64.

Isothermal Batch Reactor 8