ISOTHERMAL BATCH REACTOR

OBJECTIVE:

To study a non-catalytic homogeneous reaction in an isothermal batch reactor.

AIM:

1. To determine the reaction rate constant (K) for the given saponification reaction of
ethyl acetate in aqueous sodium hydroxide solution.

2. To study the effect of temperature on reaction rate constant K and determine the
activation energy E of this reaction.

INTRODUCTION:
A batch reactor is a closed system with no input and output streams. A batch reactor can
operate under the following conditions:

• Isothermal (temperature 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).

THEORY:

REACTION:

NaOH + CH3COOC2H5 🡪 CH3COONa + C2H5OH

(A) (B) (C) (D)

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

For second-order reaction

…………………………………………(1)

Where is the rate of disappearance of A, is the concentration of A at any time t, K is the

rate constant.
The performance equation for the batch reactor is:

……………………………………… (2)

Where t is time of reaction, is initial concentration of A, is concentration of A at any

time t.

Substitute the value of in eqn (2) from eqn (1)

…………………………………….. (3)

On solving the above equation we get

Rate constant,

Degree of conversion,

Also, a plot of t vs. XA/ (1-XA) shall yield a straight line for an assumed second order reaction
with slope = 1/ (KCAo). From this slope rate constant, K can be calculated. Effect of
temperature on reaction rate constant is expressed in terms of

Arrhenius‘law

is the frequency factor and E is called the activation energy of reaction, R is real gas
constant, and T is reaction temperature.
A plot of ln vs. 1/T on semi log paper yields a straight line with slope = -E/R

From this slope, activation energy, E can be calculated.

DESCRIPTION:
The set up consists of a reactor fitted in a constant-temperature water bath. One stirrer is
fitted for mixing the reactants in the reactor and the other is fitted in a 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. Product from
the reactor is analyzed by chemical titration.

UTILITIES REQUIRED:

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.

2. Water supply (Initial fill).

3. Floor Drain Required.

4. Floor Area Required: 1.0 m X 0.5 m

5. Laboratory glassware: -

Beaker (500 ml) : 02 Nos.

Conical flasks (250 ml) : 02 Nos.

Measuring cylinder (50 ml) : 02 Nos.

Burette (50 ml) : 01 No.

6. Chemicals: - Distilled water: 02 Lit

NaOH Pellets: 10 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:

1. Prepare 2L of N/10 sodium hydroxide solution by dissolving 8 gm of sodium

hydroxide in 2L of distilled water.

2. Prepare 1L of N/10 ethyl acetate solution by mixing 9.8 ml of ethyl acetate in 1L of

distilled water.
 3. Put 1000 ml sodium hydroxide solution in beaker-1 and ethyl acetate solution in 1000
ml beaker-2.

4. Take 20 ml of N/10 hydrochloric acid in measuring cylinders & pore it in conical

flask.

5. Fill the burette by N/10 sodium hydroxide.

6. Close all the valves V1-V2.

7. Fill water in the water bath.

8. Fill ethyl acetate solution in the reactor.

9. Ensure that ON/OFF switches given on the panel are at OFF position.

10. Set the reaction temperature (ambient to 70 oC) by increment, decrement and set
button of PID.

11. Connect the electric supply to the set-up.

12. Start the heater and stirrer of the bath and wait till constant temperature is attained.

13. Fill sodium hydroxide solution into the reactor.

14. Start the motor and stirrer of the reactor.

15. At regular intervals of 10-20 sec withdraw 10 ml of the reaction mixture in a

measuring cylinder that already contain 20 ml N/10 hydrochloric acid, by valve V1.

16. Note down the reaction temperature.

17. Transfer the sample solution in a conical flask.

18. Titrate the solution, using phenolphthalein as an indicator against N/10 sodium
hydroxide (add NaOH from burette).

19. Repeat the experiment for different reaction temperature.

7.2 CLOSING PROCEDURE:

1. When experiment is over switch OFF the motor and stirrer of reactor.

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

3. Drain the reactor and water bath by open the valve V1-V2.

OBSERVATION & CALCULATION:

8.1 DATA:

Real gas constant R = 1.987 cal/mole K

The volume of HCl VHCl = 20 ml

The 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

8.2 OBSERVATION TABLE:

S. No. T (oC) t (se) V1 (ml)

1. 25 10 13

2. 25 20 13.4

3. 25 30 13.5

4. 25 40 13.5

5. 25 50 13.6

6. 25 70 13.8

7. 25 80 14

8. 25 90 14.2

SAMPLE CALCULATIONS:

CAo = NNaOH (mole/L) = 0.1 mol/l

 (mole)

(mole)

(mole/L)

(L/mole min)

(K)

= (L/mole min)

SAMPLE CALCULATIONS:
 T t V1 HCLR CA XA K XA/(1-XA)
25 0.167 13 0.0007 0.07 0.3 25.71 0.4286
25 0.333 13.4 0.00066 0.066 0.34 15.45 0.5152
25 0.500 13.5 0.00065 0.065 0.35 10.77 0.5385
25 0.667 13.5 0.00065 0.065 0.35 8.08 0.5385
25 0.833 13.6 0.00064 0.064 0.36 6.75 0.5625
25 1.167 13.8 0.00062 0.062 0.38 5.25 0.6129
25 1.333 14 0.0006 0.06 0.4 5.00 0.6667
25 1.500 14.2 0.00058 0.058 0.42 4.83 0.7241

Avg K 10.2308

Plot t vs. XA/ [1-XA] on a simple graph, and find slope S1

RSULTS AND CONCLUSION:

• With increase in time ,conversion also increases reaction rate constant

decreases.
• Conversion increases in a batch reactor as the mixing happens properly.

NOMENCLATURE:
Nom Column Heading Units Type

Concentration of unreacted NaOH in the reactor mole/L Calculated

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

E The activation energy of the reaction cal/mole Calculated

HClO Amount of HCl taken for quench mole Calculated

HClR Amount of HCl reacted with NaOH mole Calculated

The rate constant for individual run L/ mole min Calculated

The rate constant obtained from slope S1 L/ mole min Calculated

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

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 K Given

 S1 Slope of graph (t vs. XA/ [1-XA]) Min Calculated

S2 Slope of graph (ln vs 1/T’) K Calculated

o
T Reaction temperature C Given

T’ Reaction temperature K Calculated

t Time min Measured

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

VSAMP Volume of sample ml Given

VNaOH Volume of NaOH used for titration ml Measured

XA Degree of conversion * Calculated

* Symbols represent unitless quantity.

PRECAUTION & MAINTENANCE INSTRUCTIONS:

1. Measure the exact volume of water and weigh the chemicals.

2. Always use distilled water, good quality chemicals and standard solution for titration.

3. Keep close all the drain valves while filling the reactant in reactor.

4. Handle the chemicals carefully.

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

TROUBLESHOOTING:

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

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

3. If the switch of the heater is ON but the temperature can’t rise but the panel LED is
ON it means the bath heater has burned replace that.

REFERENCES:

1. Levenspiel, Octave (2001). Chemical Reaction Engineering. 3rd Ed. NY: John Wiley
& Sons. pp 27-29, 44, 92, 111.
 2. Fogler H. Scoot (2008). Elements of Chemical Reaction Engineering. 4th Ed. ND:
Prentice-Hall of India Pvt. Ltd. pp 148-150, 152-155.

BLOCK DIAGRAM: