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BATCH REACTOR Page 1

DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR


OBJECTIVE

Study of a non-catalytic homogeneous reaction in a batch reactor between NaOH and
Ethyl Acetate and to determine,

1. Order of the reaction
2. Rate Constant (k)
3. The effect of temperature on k and determine Activation Energy























BATCH REACTOR Page 2
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
APPARATUS REQUIRED
Apparatus Quantity
i. Measuring cylinder (1000ml) 1
ii. Measuring cylinder (500ml) 1
iii. Pipette (5ml/10ml) 1
iv. Burette (25ml) 1
v. Conical flask (2500ml) 4
vi. Beaker (100ml) 3
vii. Volumetric flask 1
viii. Bucket 2
ix. Mug 1
x. Thermometer 1
xi. Conical funnel 1

REAGENTS REQUIRED
Reagents
i. NaOH pellets
ii. HCl
iii. Ethyl acetate
iv. Sodium carbonate
v. Phenolphthalein indicator











BATCH REACTOR Page 3
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
INTRODUCTION

In the batch reactor the reactants are initially charged into a container, are well
mixed and are left to react for a certain period. The resultant mixture is then
discharged. This is an unsteady-state operation where composition changes with
time; however, at any instant the composition throughout the reactor is uniform.
















BATCH REACTOR Page 4
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
THEORY

IDEAL BATCH REACTOR
Make a material for any component A. For such an accounting we usually select
the limiting component. In a batch reactor, since the composition is uniform
throughout at any instant of time, we may make the accounting about the whole
reactor. Noting that no fluid enters or leaves the reaction mixture during reaction,
which was written for component A, becomes
Input = Output + disappearance + accumulation
(Eq.1)
Evaluating the terms of Eq.1, we find

By replacing these two terms in Eq.1, we obtain

Rearranging and integrating then gives

This is the general equation showing the time required to achieve a conversion
XA for either isothermal or non-isothermal operation. The volume of reacting fluid
and the reaction rate remain under the integral sign, for in general they both change
as reaction proceeds.
This equation may be simplified for a number of situations. If the density of the
fluid remains constant, we obtain

BATCH REACTOR Page 5
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR



For all reactions in which the volume of reacting mixture changes
proportionately with conversion, such as in single gas-phase reactions with
significant density changes, then it becomes



They are applicable to both isothermal and non isothermal operations. For the
latter the variation of rate with temperature, and the variation of temperature with
conversion, must be known before solution is possible.
Graphical representation of two of these equations
Graphical representation of the performance equations for batch reactors, isothermal
or nonisothermal
Space-Time and Space-Velocity

Just as the reaction time t is the natural performance measure for a batch reactor,
so are the space-time and space-velocity the proper performance measures of flow
reactors. These terms are defined as follows

Space-time:

BATCH REACTOR Page 6
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR


Space- Velocity:





Thus, a space-velocity of 5 hr
-l
means that five reactor volumes of feed at
specified conditions are being fed into the reactor per hour. A space-time of 2min
means that every 2 min one reactor volume of feed at specified conditions is being
treated by the reactor.
Now we may arbitrarily select the temperature, pressure, and state (gas, liquid,
or solid) at which we choose to measure the volume of material being fed to the
reactor. Certainly, then, the value for space-velocity or space-time depends on the
conditions selected. If they are of the stream entering the reactor, the relation
between s and r and the other pertinent variables is


It may be more convenient to measure the volumetric feed rate at some standard
state, especially when the reactor is to operate at a number of temperatures. If, for
example, the material is gaseous when fed to the reactor at high temperature but is
liquid at the standard state, care must be taken to specify precisely what state has
been chosen. The relation between the space-velocity and space-time for actual feed
conditions (unprimed symbols) and at standard conditions (designated by primes) is
given by


BATCH REACTOR Page 7
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR

In most of what follows, we deal with the space-velocity and space-time based on
feed at actual entering conditions; however, the change to any other basis is easily
made.





































BATCH REACTOR Page 8
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
DIAGRAM






Schematic Diagram of batch reactor























BATCH REACTOR Page 9
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
PROCEDURE

1. Measure the volume of the reactor using water .Let it be V.
2. Prepare 10L of N/40 HCl. Put 20 ml of this into each of the 6 different conical
flasks.
3. Put 0.3V of ethyl acetate and NaOH solution one by one into the reactor and
switch on the magnetic stirrer. Note down the temperature of the reaction at T
o
C.
4. After an interval of 5 minutes, withdraw 10 ml of sample through pipette from the
reactor and transfer this into the 20 ml of HCL in a conical flask.
5. Titrate 10ml aliquot from the solution against N/100 NaOH using phenolphthalein
indicator and note end point.
6. Repeat step 5. To get 5 different sets of sample at an interval of 5 minutes for a
total of 30 minutes and analyse them as described in step 6.
7. Repeat the above procedure for two more sets at temperature T+10
o
C and T+15
o
C.
8. Titrate 10 ml of a mixture (5ml N/100 NaOH + 20ml N/40 HCl+ 5ml M/100 ethyl
acetate) against N/100 NaOH using Phenolphthalein as the indicator. The reading of
this titration is to be used in the calculation of the C
Ao
.
9. Ensure that the stock solutions of the individual reactant must have been stirred
before using them.
























BATCH REACTOR Page 10
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR












































BATCH REACTOR Page 11
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
CALCULATIONS & GRAPHS

1. CALCULATION FOR C
A0
(INITIAL CONCENTRATION)
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 11.5 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*11.5)*(N/100) = 4.6ml
Volume of HCl reacted with feed solution
V
4
= 20-4.6 = 15.4ml
So, concentration of solution initially
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(15.4/10) = 0.0385N
Normality = Molarity = 0.0385mol/lit

2. CALCULATION FOR COCENTRATION AT TEMPERATURE =39.2
o
C

I. Time = 5 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 12 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*12)*(N/100) = 4.8ml
Volume of HCl reacted with feed solution
V
4
= 20-4.8 = 15.2ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(15.2/10) = 0.0380N
Normality = Molarity = 0.0380mol/lit

II. Time = 10 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 12.8 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*12.8)*(N/100) = 5.12ml
Volume of HCl reacted with feed solution
V
4
= 20-5.12 = 14.88ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(14.88/10) = 0.0372N
Normality = Molarity = 0.0372mol/lit


BATCH REACTOR Page 12
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
III. Time = 15 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 13.4 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*13.4)*(N/100) = 5.36ml
Volume of HCl reacted with feed solution
V
4
= 20-5.36 = 14.64ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(14.36/10) = 0.0366N
Normality = Molarity = 0.0366mol/lit

IV. Time = 20 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 14 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*14)*(N/100) = 5.6ml
Volume of HCl reacted with feed solution
V
4
= 20-5.6 = 14.4ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(14.4/10) = 0.036N
Normality = Molarity = 0.0360mol/lit

V. Time = 25min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 14.7 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*14.7)*(N/100) = 5.88ml
Volume of HCl reacted with feed solution
V
4
= 20-5.88 = 14.12ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(14.12/10) = 0.0353N
Normality = Molarity = 0.0353mol/lit

VI. Time = 30 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 15.2 ml
Volume of HCl consumed in titration = V
1
ml

BATCH REACTOR Page 13
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*15.2)*(N/100) = 6.08ml
Volume of HCl reacted with feed solution
V
4
= 20-6.08 = 13.92ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(13.92/10) = 0.0348N
Normality = Molarity = 0.0348mol/lit


Thus for temperature =39.2
o
C
C
A0
=0.0385 mol/lit
C
A1
=0.0380 mol/lit
C
A2
=0.0372 mol/lit
C
A3
=0.0366 mol/lit
C
A4
=0.0360 mol/lit
C
A5
=0.0353 mol/lit
C
A6
=0.0348 mol/lit



3. CALCULATION FOR COCENTRATION AT TEMPERATURE =46.2
o
C

I. Time = 5 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 13 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*13)*(N/100) = 5.20 ml
Volume of HCl reacted with feed solution
V
4
= 20-5.20 = 14.80 ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(14.80/10) = 0.0370N
Normality = Molarity = 0.0370mol/lit

II. Time = 10 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 14 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*14)*(N/100) = 5.60ml
Volume of HCl reacted with feed solution

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DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
V
4
= 20-5.60 = 14.4ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(14.4/10) = 0.036N
Normality = Molarity = 0.0360mol/lit

III. Time = 15 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 14.9 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*14.9)*(N/100) = 5.96ml
Volume of HCl reacted with feed solution
V
4
= 20-5.96 = 14.04ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(14.04/10) = 0.0351N
Normality = Molarity = 0.0351mol/lit

IV. Time = 20 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 15.4 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*15.4)*(N/100) = 6.16ml
Volume of HCl reacted with feed solution
V
4
= 20-6.16 = 13.84ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(13.84/10) = 0.0346N
Normality = Molarity = 0.0346mol/lit

V. Time = 25min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 15.95 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*15.95)*(N/100) = 6.38ml
Volume of HCl reacted with feed solution
V
4
= 20-6.38 = 13.62ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(13.62/10) = 0.03405N

BATCH REACTOR Page 15
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
Normality = Molarity = 0.03405mol/lit

VI. Time = 30 min
Volume of aliquot sample = 30ml
Volume of NaOH consumed = 16.3 ml
Volume of HCl consumed in titration = V
1
ml
N
1
V
I
= N
2
V
2

V
1
= ((40/N)*16.3)*(N/100) = 6.52ml
Volume of HCl reacted with feed solution
V
4
= 20-6.52 = 13.48ml
So, concentration of solution
N
1
V
4
= N
3
V
3

N
3
= (N/40)*(13.48/10) = 0.0337N
Normality = Molarity = 0.0337mol/lit


Thus for temperature =39.2
o
C
C
A0
=0.0385 mol/lit
C
A1
=0.0370 mol/lit
C
A2
=0.0360 mol/lit
C
A3
=0.0351 mol/lit
C
A4
=0.0346 mol/lit
C
A5
=0.03405 mol/lit
C
A6
=0.0337 mol/lit




















BATCH REACTOR Page 16
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
4. GRAPH BETWEEN ln(C
Ao
/C
A
) &TIME


For Temperature =39.2
o
C





For Temperature =39.2
o
C




0
0.02
0.04
0.06
0.08
0.1
0.12
0 5 10 15 20 25 30 35
l
n
(
C
A
o
/
C
A
)


Time
0
0.02
0.04
0.06
0.08
0.1
0.12
0.14
0 5 10 15 20 25 30 35
l
n
(
C
A
o
/
C
A
)

Time

BATCH REACTOR Page 17
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
RESULT

From graphs it is clear that reactions follows first order (because of straight line
graph between ln(C
Ao
/C
A
) &time).
So,
Value of k at Temperature, T=39.6
o
C
K
1
= Slope of the straight line of graph-1 = 0.0035 min
-1

And at Temperature, T= 46.2
o
C
K
2
= Slope of the straight line of graph-2 = 0.0043 min
-1

We know
ln (K
1
/K
2
) = E/R*(1/T
2
-1/T
1
)
where E=Activation Energy and
R=constant
So, E= 25.8745 KJ/ mol





CONLUSIONS

The performance equation of batch reactors is similar as the PFR reactors.
For endothermic reaction as the temperature is increases the rate of the reaction is
also increases.



















BATCH REACTOR Page 18
DEPARTMENT OF CHEMICAL ENGINEERING, MNIT JAIPUR
PRECAUTIONS

All apparatus should be clean and dry.
Note down the readings only after steady state has been attained.
Burette reading should be noted carefully.
Titrate carefully as end point can come on any one drop.







REFERENCES

i. Octave Levenspiel, Chemical Reaction Engineering., 3
rd
edition.
ii. Jones, R.W., Chemical Engineering Programme.