ISOTHERMAL BATCH REACTOR

OBJECTIVE:
Todeterminethe order and the reaction rate constant (k) for the given saponification reactionof ethyl
acetate with aqueous sodium hydroxide solution.

REACTION:
NaOH +CH3COOC2H5 CH3COONa + C2 H5 OH (I)
(A) (B) (C) (D)

CHEMICALS:
0.1N Ethyl acetate -----1 litre
0.1NNaOH ------1 litre
0.1NHCl -----500 ml
0.1N Oxalic acid ----- 100 ml
Phenolphthalein indicator

APPARATUS / GLASSWARE:
Conical flask (1 litre), a dozen conical flasks (250ml), measuring pipette, burette, stop-clock.

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 throughout)
Constant volume (volume of the reaction mixture within the reactor remains constant; there is
no appreciable change in the density of reaction mass)

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
Also
KN A
rA KC A
dt
Combining these two equations yield:

1
ln N A0 ln N A kt or N A N A0 e kt (1)
in terms of Conc.
1 N A0
C A C A0 e kt & t ln
k NA (2)
N A0 =No. of moles of A at t=0

N A = No. of moles of A at t=t

For second order unidirectional reaction
k
2A
product

1 dN A
kC A2
V dt
1 1
kt
CA C A0

V 1 1
t
k N A N A0

fig.no. 1

1
If we plot vs t as shown in fig. no. 1we must get a straight line with slope = k and intercept =
CA
1
C A0
For second order reaction:
k
AB
product

1 dN A k
kC A C B 2 N A N B
V dt V
If N A0 N B 0 then N A N B for all t.

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.

2
DESCRIPTION:
The set up shown in fig. no. 2consists of a reactor fitted in a constant temperature water bath.
One stirrer isfitted for mixing the reactants in reactor and other is fitted in water bath to keep
theuniform temperature throughout in the bath. The temperature of bath can be maintainedfrom
ambient to 90C with the help of digital temperature indicator cum controller.Products from the
reactor are analyzed by chemical titration.

EXPERIMENTALPROCEDURE:
1. Prepare 1L of 0.1N sodium hydroxide solution by dissolving 4 gm of sodium hydroxide in
1L of distilled water.
2. Prepare 1L of 0.1N ethyl acetate solution by mixing 8.8 gm (or 9.8 ml) of ethyl acetate in 1L
of distilled water.
3. With the help of standard oxalic acid, determine the normality of the NaOH solution taken in
the tank.
4. Using this standardized sodium hydroxide solution, determine the normality of hydrochloric
acid solution.
5. Take 10 Nos. of 250ml beakers and put 10ml of 0.1N HCl in each beaker.
6. Take 0.1N NaOH in the burette.
7. Adjust the temperature of water bath at 50C.
8. Take 400ml each of 0.1N CH3COOC2H5 and 0.1N 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 in measuring cylinder that
already contain 10 ml 0.1N hydrochloric acid, by valve V1.
11. Record the reaction temperature.

Explanation: Note that when a sample of reaction mixture is transferred into the conical flask
containing HCl, the alkali in the reaction mixture gets neutralized and so the saponification
reaction stops. Back-titration of the contents of this flask therefore helps in determining the
amount of unreacted NaOH present in the reaction mixture at the time of its removal from the
reactor. In other words, the experiment helps to find the alkali concentration (C A) in the reactor
as a function of time (t).

OBSERVATIONS &CALCULATIONS
Preliminary titrations:

Standardization of NaOH : -
Volume of Oxalic acid taken = 10 ml
Normality of Oxalic acid = -------- (given)
Volume of NaOH run down = --------ml.(titre value)
Normality of NaOH =

3
 Standardization of HCl:-
Volume of HCl taken ,V1 = 10 ml.
Volume of NaOH run down ,V3 = -------- ml.
Normality of HCl =

Tabulation:

S.No. Reaction Volume of Volume of CA -ln( ) 1/CA

Time Sample NaOH (mol/lit) (lit/mol)
(min) (ml) (ml)

Model Graph:

1/CA
k

1/CA0

0
Time(min)

Model Calculation:

= = ---------------- (mol/lit)
(( ) ( ) )
= ( / )

= --------(lit/mol)

NOMENCLATURE:
CA = Conc. of unreacted NaOH in the reactor, mol/lt
CA0 = Initial Conc. of NaOH in the feed mixture, mol/lt
k = Rate constant, lt/ mol. min
NHCL = Number of moles of HCL used, g mol

4
NNaOH = Number of moles of NaOH used, g mol
VHCl = Volume of 0.1N HCl taken for quench, ml
VNaOH = Volume of NaOH used for neutralizing, ml

PRECAUTION & MAINTENANCE INSTRUCTIONS:

Measure the exact volume of water and weigh the chemicals.
Always use distilled water, good quality chemicals and standard solution for titration.
Keep close all the drain valves while filling the reactant in reactor.
Handle the chemicals carefully.
Dont ON heater switch before filling water in the water bath.

RESULT:
Thus the experiment on batch reactor was performed. The value of k is ________(lit/mol.min)
value from graph, 1/CAvs Time = ---------------- at ----------0C

Fig. no. 2