ISOTHERMAL CONTINUOUS STIRRED TANK REACTOR

1. OBJECTIVE:

To study of a non-catalytic homogeneous reaction in a CSTR under isothermal

conditions.

2. AIM:

2.1 To determine the reaction rate constant, (K) for saponification of ethylacetate with
sodium hydroxide at a fixed temperature.

2.2 To study the effect of temperature on the reaction rate constant, (K) and
determine the activation energy, (E) for this reaction.

3. INTRODUCTION:

In an ideal CSTR (that is an ideal steady state flow reactor) 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. These types of reactors are also known
as MIXED FLOW REACTOR.

4. THEORY:

REACTION:

NaOH + CH3COOC2H5 CH3COONa + C2H5OH
(A) (B) (C) (D)

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

For second order reaction


 dC A
rA  dt

rA  KCA2 …………………………………………(1)

Where  rA is rate of disappearance of A, CA is concentration of A at any time t, K

is rate constant.
5. DESCRIPTION:
The set up consists of two feed tanks through which two reactants are fed to the reactor.
Rotameters are provided to measure the individual flow rate of chemicals. The flow rate
can be adjusted by the needle valves provided on respective rotameter. The
compressed air is used for circulation of feed. The CSTR is fitted with stirrer for proper
mixing. Constant temperature water bath arrangement is provided to conduct the
experiment at various temperatures. Pressure regulator, pressure gauge and safety
valve is 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.

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 Laboratory glass ware:-

Conical flask (250 ml) : 01 No.

Measuring cylinder (50 ml) : 01 No.

Burette (50 ml) : 01 No.

6.6 Chemicals:-

Distilled water : 40 Lit.

NaOH Pellets : 100 gm

N/10 NaOH : 100 ml

N/10 HCl : 100 ml

Ethyl acetate : 200 ml

Indicator (phenolphthalein) : Few drops

7. EXPERIMENTAL PROCEDURE:

7.1 STARTING PROCEDURE:

7.1.1 Prepare 20L of N/10 NaOH solution by dissolving 80 gm of sodium

hydroxide in 20L of distilled water.

7.1.2 Prepare 20L of N/10 ethyl acetate solution by mixing 176 gm (or 196 ml) of
ethyl acetate in 20L of distilled water.

7.1.3 Take 20 ml of N/10 hydrochloric acid in measuring cylinder.

7.1.4 Fill the burette by N/10 sodium hydroxide (Standard Solution).

7.1.5 Close all the valves V1-V11.

7.1.6 Open valve V4 and V6, fill sodium hydroxide solution in feed tank A.

7.1.7 Close valve V4 and V6.

7.1.8 Open valve V5 and V7, fill ethyl acetate solution in feed tank B.

7.1.9 Close valve V5 and V7.

7.1.10 Fill the water in water bath.

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

7.1.12 Connect electric supply to the set-up.

o
7.1.13 Set the reaction temperature (ambient to 70 C) by increment, decrement
and set button of DTC.

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

7.1.15 Connect compressed air supply to the set-up at valve V 1.

2
7.1.16 Open valve V1 and set air pressure 0.5 to 1 kg/cm by pressure regulator
and pressure gauge.

7.1.17 Pass sodium hydroxide and ethyl acetate into the reactor by allowing
equal flow rate controlled by valve V2-V3.

7.1.18 Start the stirrer of the reactor.

 7.1.19 After about 10 min or time equal to the residence time of the reactor
(which ever is greater) collect exact 10 ml of the sample from the outlet in
measuring cylinder that already contain 20 ml of hydrochloric acid.

7.1.20 Note down the reaction temperature.

7.1.21 Transfer the sample solution in a conical flask.

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

sodium hydroxide (add NaOH from burette).

7.1.23 Repeat the experiment for different flow rates of feed.

7.1.24 Repeat the experiment for different reaction temperature.

7.2 CLOSING PROCEDURE:

7.2.1 When experiment is over stop flow of feed by close the valve V 2-V3.

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

7.2.3 Switch OFF the stirrer of the reactor.

2
7.2.4 Reduce air pressure to 0 kg/cm by pressure regulator and pressure
gauge.

7.2.5 Close the valve V1.

7.2.6 Drain the reactor, feed tanks and water bath by valve V 8-V11.

8. OBSERVATION & CALCULATIONS:

GIVEN DATA:

Real gas constant R = 1.987 cal/mol K

Working volume of reactor VR = ____ 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
9. NOMENCLATURE:

Nom Column Headings 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
E Activation energy of the reaction Cal/mol Calculated

HClO Amount of HCl taken for quench mole Calculated

HClR Amount of HCl reacted with NaOH mole Calculated

K Rate constant for individual run L/ mole min Calculated

Kt 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 Measured

R Real gas constant Cal/mol K Given

2
S1 Slope of graph ( vs. XA/ [1-XA] ) min Calculated

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

o
T Reaction temperature C Measured
T’ Reaction temperature K Calculated

V1 Volume of NaOH used for titration ml Measured

VSAMP Volume as sample ml Given

VA Volumetric flow rate of NaOH LPH Measured

VB Volumetric flow rate of CH3COOC2H5 LPH Measured
VHCl Volume of N/10 HCl taken for quench Ml Given
VR Working volume of reactor Lit Given
XA Degree of conversion * Calculated
τ Residence time min Calculated

* Symbols are unitless

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 V 8-V11 and vent valves V6-V7 should be open
while filling the reactant in feed tanks.

10.4 Flow should not be disturbed during the experiment.

10.5 Handle the chemicals carefully.

10.6 Do not ON the switch of the heater switch before filling water in the water bath.

11. TROUBLESHOOTING:
11.1 If any type of suspended particles are come in the rotameter, remove the
rotameter clean the tube and fit it at its place.

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

11.3 If rotameter fluctuating more than average tight the control knob properly.

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

11.5 If switch of the heater is ON, but temperature can’t rise but panel LED is ON it
means heater had burned replace it.

12. REFERENCES:
rd
12.1 Levenspiel, Octave (2001). "Chemical Reaction Engineering" 3 Ed. NY: John
Wiley & Sons. pp 27-29, 92, 111.
th
12.1 Fogler H. Scoot (2008). "Elements of Chemical Reaction Engineering" 4 Ed.
ND: Prentice-Hall of India Pvt. Ltd. pp 162-165
13. PHOTOGRAPH:
14. BLOCK DIAGRAM: