EXPERIMENT – 5

SEMI BATCH REACTOR

Preethika .T

2019A1PS0193U

FACULTY INCHARGE : Dr. BG Prakash Kumar

AIM:

To determine the rate constant for the saponification of ethyl acetate with NaOH in a semibatch
reactor.

THEORY:

A semi-batch reactor can be considered as a continuously operated tank reactor where incoming
and outgoing mass flows are not equal to each other; consequently, the total mass of reaction
mixture is not constant.

In a semi-batch reactor one reactant (A) is added initially and the other reactant (B) is added
continuously at constant rate. The continuous feeding of one of the reactant causes change in
the composition in addition to the changes due to the reaction itself.

Consider the reaction k

A + B ⎯⎯→ C + D

in which B is fed to the vat containing only A initially. Mass balance for reactant A gives (at time
t):

number of moles of number of moles of number of moles of

A in the vat at time t = A in the vat initially - A reacted upto time t
NA = N AO - N AO X A

where, XA is the moles of A reacted per mole of A initially in the vat.

Similarly material balance for B gives

number of moles of number of moles of number of moles of number of moles of

B in the vat at time t = B in the vat initially + B added to the vat - B reacted upto time t
t
NB = N Bi + 
0
FBO dt - N AO X A

Where, FBO = molar feed rate of B = CBoνo .

For constant molar feed rate: NB = NBi + FBot - NAO XA
Rate equation is given by:
 dX A
(−rA )V = N Ao
dt

Fluid volume at any time t is V = Vo+ νot

where, Vo = initial volume of sodium hydroxide, νo = flow rate of ethyl acetate. For a second order
irreversible reaction, rate of reaction can be written as.

-rA = k CA CB

N A N A0 (1 − X A )
CA = =
V Vo +  o t
N B N Bi + FBo t − N Ao X A )
CB = =
V Vo +  o t
− dC A N dX A k N A N B
(−rA ) = = Ao =
dt V dt V2
dX A k (1 − X A ) ( N Bi + FBo t − N Ao X A )
=
dt (Vo +  o t )
(1 − X A ) ( N Bi + FBo t − N Ao X A )
t
XA= k dt
0
(Vo +  o t )

PROCEDURE:

1. Prepare 5 liter of 0.1 N NaOH solutions by dissolving 4 gm of NaOH pellets in 1 lit of

water. Transfer the solution to reactor.
2. Prepare 10 liter of 0.1 N ethyl acetate solution by adding 10 ml per liter of water.
Transfer the solution to ethyl acetate tank.
3. Prepare 1 liter of 0.1 N standard oxalic acid solution by dissolving 6.3 gm if oxalic acid
crystals in 1 L of water.
4. Standardize NaOH solution by titrating against 0.1 N oxalic acid using phenolphthalein
as indicator.
5. Prepare sodium acetate solution (500ml) of same standardized NaOH normality.
6. Adjust the mixer speed at a desired level and wait for steady
7. Add measured quantity (2 lit) of aqueous solution of NaOH in the reaction vessel, start
stirrer and wait till the temperature equals the set temperature.
8. Adjust the volumetric flow rate of ethyl acetate solution with the help of rotameter
to 10 LPH. Simultaneously start the stop watch. Note the reading till conductivity
reading is constant.
 9. Above procedure is repeated for different temperature and flow rate of ethyl acetate
also.

OBSERVATIONS:

Attached in the end of this document.

CALCULATIONS:

y = 0.0044x - 0.0027
Calibration chart R² = 0.9995
0.1

0.08

0.06
Normality

0.04

0.02

0
0 5 10 15 20 25

-0.02
Conductivity
 y = 224.87x + 0.6219
Calibration chart R² = 0.9995
25

20
Conductivity

15

10

0
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.1
Normality

y = -0.0717x + 1.4856
Conductivity vs Conversion
1.2

0.8
Conversion

0.6

0.4

0.2

0
0 5 10 15 20 25
-0.2
Conductivity
RESULTS:

k (rate constant) y = 0.5888x - 0.0971

R² = 0.8792
3.00E-01

2.50E-01

2.00E-01
Xa

1.50E-01

1.00E-01

5.00E-02

0.00E+00
0.00E+00 1.00E-01 2.00E-01 3.00E-01 4.00E-01 5.00E-01 6.00E-01 7.00E-01

(1-Xa)*(Nbi + Fbo*t - Nao*Xa) dt/ Vo+(vo*t)

CONCLUSION:

1. The rate constants for the respective time intervals have been determined and are listed
on the table.
2. The k value initially increases and then decreases showing a stagnant trend.