ISOTHERMAL SEMI-BATCH REACTOR

MIR AHMED

2110110331

1. OBJECTIVE:

To study a second-order saponification reaction between ethyl acetate and sodium

hydroxide in a semi-batch reactor under isothermal conditions (i.e. at a fixed
temperature).
2. AIM:

To determine experimentally the reaction rate constant (K) and variation of

concentration in sodium hydroxide with time in the reactor.
3. INTRODUCTION:

One of the best reasons to use semi-batch reactors is to enhance selectivity in

liquid-phase reactions. In a batch reactor, a reactant is added to another the
contents in the reactor are well mixed and have uniform composition throughout.
Thus, the exit stream has the same composition as the fluid within the reactor.
4. THEORY:

A semi-batch reactor can operate under isothermal conditions. In this type of reactor, reactant
A, in a solution of concentration CAo (mole/L)is charged to the reactor to a volume Vo (L), then
reactant B is pumped in at the rate of o v(LPH) and the reaction is allowed to take place. There
is no overflow and assuming no change in density.

5. REACTION:

NaOH + CH3COOC2H5 → CH3COONa + C2H5OH

The above reaction is second order reaction (n = 2)

 For second order reactio

5. DESCRIPTION:

The set up consists of a reactor fitted in a constant temperature water bath. Before
starting the reaction the reactor is charged with measured quantity of one reactant.
From a feed tank another reactant is fed to the reactor. Using a sampling pipette
samples can be taken out for analysis after fixed interval. Rotameter is provided
to measure the flow of chemicals. The compressed air is used for circulation of
feed. 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. Temperature
is controlled with the help of digital temperature indicator cum controller. Pressure
regulator, pressure gauge and safety valve are fitted in the compressed air line.
6. UTILITIES REQUIRED:

6.1 Electricity supply: Single phase, 220 V AC, 50 Hz, 5-15 Amp combined socket with
earth connection. Earth voltage should be less than 5 volts.
6.2 Compressed air supply continuous @ 0.5 CFM at 1 Bar.

6.3 Water supply (Initial fill)

6.4 Floor drain required.

6.5 Floor Area Required: 1 m x 0.75 m.

6.6 Laboratory glass ware:-

Beaker (1000 ml) : 01 No.

Conical flask (250 ml) : 02 Nos.

Measuring cylinder (50 ml) : 02 Nos.

Burette (50 ml) : 01 Nos.

 6.6 Chemicals:

Distilled water: 25 Lit

NaOH Pellets: 20 gm

N/10 NaOH: 100 ml

N/10 HCl: 100 ml

Ethyl acetate : 15 ml

Indicator (phenolphthalein) : Few drops

7. EXPERIMENTAL PROCEDURE:

7.1 STARTING PROCEDURE:

7.1.1 Prepare 5L of N/10 sodium hydroxide solution by dissolving 20 gm of

sodium hydroxide in 5L of distilled water.
7.1.2 Prepare 10L of N/10 ethyl acetate solution by mixing 98 ml of ethyl acetate
in 10L of distilled water.
7.1.3 Put N/10 sodium hydroxide solution in the 1000 ml beaker for titration.
7.1.4 Close all the valves V1-V7.

7.1.5 Open the valve V3-V4. Fill 20L of the ethyl acetate solution in the feed tank.

7.1.6 Close the valve V3-V4.

7.1.7 Fill the reactor with 2.2 - 2.4 L of N/10 sodium hydroxide feesolution.

7.1.8 Take 20 ml of N/10 hydrochloric acid in measuring cylinders & transfer it

in the conical flask.
7.1.9 Fill the burette with N/10 sodium hydroxide (Standard Solution) with the
help of funnel.
7.1.10 Ensure that switches given on the panel are at thposition.

7.1.11 Fill water in the water bath.

7.1.12 Connect electric supply to the set-up.

7.1.13 Set the reaction temperature (ambient to 70oC) by increment, decrement

buttons of PID controller.
7.1.14 Start the heater and stirrer of the bath and wait till constant temperature is
attained.
 7.1.15 Start stirrer of the reactor.

7.1.16 Open valve V1 and set air pressure 0.7 to 1 kg/cm2 by pressure regulator and
pressure gauge
7.1.17 Pass ethyl acetate into the reactor by allowing constant flow rate controlled
by valve V2.
7.1.18 At regular intervals of 2-3 min, withdraw 10ml of reaction mixture from
outlet, in measuring cylinder & transfer the sample in conical flask, which
already contain 20 ml N/10 hydrochloric acid.
7.1.19 Note down the reaction temperature.

7.1.20 Titrate the solution, using phenolphthalein as an indicator against N/10

sodium hydroxide (add NaOH from burette).
7.1.21 Repeat the experiment for different volume of sodium hydroxide feed
solution.
7.1.22 Repeat the experiment for different flow rate of ethyl acetate. 7.1.23 Repeat

the experiment for different reaction temperature.

7.2 CLOSING PROCEDURE:

7.2.1 When experiment is over switch OFF the motor ofreactor.

7.2.2 Switch OFF the heater and stirrer of the water bath.

7.2.3 Drain the feed tank, reactor and water bath by valve V5-V7.

8. OBSERVATION & CALCULATION:

8.1 DATA:

Real gas constant R = 1.9872 cal/mole K

Initial volume of NaOH in reactor Vo = 2.2 - 2.4 Lit

Volume of HCl VHCl = 20 ml

 Volume of sample VSAMP = 10 ml

Normality of NaOH in feed solution NNaOH = 0.1 g eq/L

Normality of NaOH used for titration N1 = 0.1 g eq/L

Normality of HCl NHCl = 0.1 g eq/L

Normality of ethyl acetate NEA = 0.1 g eq/L

8.2 OBSERVATION TABLE:

S. No. T(oC) t (min) V1 (ml) VB (LPH)

1. 30 3 14.5 10

2. 30 6 17.5 10

3. 30 9 17.8 10

4. 30 12 19.6 10
 CALCULATION TABLE: 2

S.No. T(oC) t XA K (L/mole

(min) min)

1 30 3 0.3125 3.3939

2 30 6 0.6250 5.7503

3 30 9 0.615 5.2729

4 30 12 0.92 25.8013
 Plot: Isothermal Semi-batch Reactor
0.06

0.05 y = -0.0052x + 0.0655

0.04

0.03

0.02

0.01

0
0 2 4 6 8 10 12 14
t (min)

RESULT AND DISCUSSION:

Therefore, from the graph, we can infer that the rate of change in concentration with
respect to time is -0.0052 mole/ L min. This also suggests that at rate constant k which is
3.3939 L/mole min, conversion occurs, and reactant A and reactant B will start to
dissipate after 3-minute intervals. The sample is then titrated and conversion is
calculated.

9. NOMENCLATURE:
Nom Column Heading Units Type

CA Concentration of unreacted NaOH in the reactor mole/L Calculated

CAo Initial concentration of NaOH in the feed mixture mole/L Calculated

dCA Derivatives of concentration of NaOH mole/L Calculated

dt with respect to time min

HClO Amount of HCl taken for quench mole Calculated

HClR Amount of HCl reacted with NaOH mole Calculated

K Rate constant L/ mole Calculated

min
 N1 Normality of NaOH used for titration g eq /L Given

o
T temperature C Measured

Normality of ethyl acetate g eq /L Given

NEA

NHCl Normality of HCl g eq /L Given

NNaOH Normality of NaOH in feed solution g eq /L Given

R Real gas constant cal/mole Given

K

t Time min Measured

VSAMP Volume of sample ml Given

V Volume of feed solution at any time t Lit Calculated

V1 Volume of NaOH used for titration ml Measured

VB Volumetric flow rate of ethyl acetate LPH Measured

VHCl Volume of N/10 HCl taken for quench ml Given

Vo Initial volume of NaOH in reactor Lit Given

XA Degree of conversion * Calculated

* Symbols represent unitless quantity.

10. PRECAUTION & MAINTENANCE INSTRUCTIONS:

10.1 Measure the exact volume of water and weight of chemicals.

10.2 Always use distilled water, good quality chemicals and standard solution for
titration.
 10.3 Keep close all the drain valves V5-V7, and vent valve V4 should be open while filling
the reactants in feed tank and reactor.

10.4 Handle the chemicals carefully.

10.5 Don’t ON the switch of heater before filling water in the water bath.

11. TROUBLESHOOTING:

11.1 If there is any leakage tight that part or fix it again after wrapping teflon tape.

11.2 If D.T.C do not display on display board it means sensor connection is not proper
(tight computer jacket).

11.3 If switch of the heater is ON but temperature can’t rise but panel LED is ON it means
bath heater had burned replace it.
12. REFERENCES:

12.1 Fogler H. Scoot (2008). Elements of Chemical Reaction Engineering. 4th Ed. ND:
Prentice-Hall of India Pvt. Ltd. pp 218-221.