Experiment No: 4 Date: 13/9/2011 CONTINUOUS STIRRED TANK REACTOR

4.1 AIM To determine the rate constant (K) for saponification of ethyl acetate (CH3COOC2H5) with sodium hydroxide and thereby study the performance of Continuous Stirred tank reactor. 4.2 APPARATUS REQUIRED 4.3 THEORY Continuous stirred tank reactor is an ideal reactor. The exit concentration is the same as that of the bulk of fluid in the CSTR. A stirred tank can be used either as batch reactor or as a flow reactor. Assumptions: Constant density Isothermal Steady state Single irreversible reaction. Perfect mixing of reactants No phase change Stirred tank reactor with an agitator Conical flask with beaker/beaker (100/50 ml) Pipette (10 ml)/ syringe (10 ml) Standard flask (1000ml, 250ml, and 100ml) Burette (50ml) 16 Nos 1 No: 1 No: 1 No:

Continuous stirred take reactors are having wide application in chemical and biological process industries and also used in activated sludge reservoirs for waste water treatment.

The saponification reaction we consider in this experiment is, CH3COOC2H5 + NaOH CH3COONa + C2H5OH Rate equation is: -rA = kCACB (1)

The performance equation of CSTR is /CA0 = V/0CA0 = V/FA0 = XA/-rA -rA = kCACB = kCA0(1-XA)CA0(CB0/CA0-XA) = kCA02(1-XA)(m-XA) /CA0 = XA/kCA02(1-XA)(m-XA) k = XA/CA0(1-XA)(m-XA) (3) (2)

(4)

(5)

A plot of XA/CA0(1-XA)(m-XA) vs gives a straight line of slope k passing through origin

4.4 SOLUTIONS REQUIRED 100 ml of 0.1 N oxalic acid 1000ml of 0.1 N NaOH 250ml of 0.1 N hydrogen chloride 100ml of ethyl acetate

4.5 PROCEDURE a) Make 0.1N solution of NaOH by dissolving 40g of NaOH in 10 L of water and fill one tank with this solution. b) Make 0.1N ethyl acetate by mixing 98 mL of concentrated ethyle acetate with 9902 ml of water and fill the other. c) Set the pressure of 15 Psi . open outlet of the reservoir connected to flow meters rotameter 1& rotameter 2. d) Adjust the flow rate in the rotameter to read 5 lit/hr and switch on the stirrer.

e) Wait until overflow of the reactor vessel happens. f) Take 50ml of overflow from the reactor to a beaker. g) 20 ml of this is transferred to a conical flask h) Add 20ml of 0.1N HCl and 2-3 drops of phenolphthalein indicator to it. i) Titrate the resultant solution against 0.1N NaOH from the burette to find unreacted excess HCl. j) Repeat step 6 with different flow rates (6 LPH, 8 LPH, 9 LPH, 10 LPH). Plot graph of XA/(1-XA)2 vs CA0V/V0 and use the slope of this straight line to determine the rate constant K of the reaction.

k) Tabulate observation table l)

OBSERVATION 1 TABLE 4.1: STANDARDISATION OF NaOH Oxalic acid x NaOH Sl No: Volume of Oxalic Acid (ml) 1 2 10 10 0 0 8.8 8.8 8.8 8.8 Burette reading (ml) Initial Final Phenolphthalein Volume of NaOH (ml)

TABLE 4.2: STANDARDIZATION OF HCl HCl x Na2CO3 Sl No: 1 2 Volume of Na2CO3 (ml) 10 10 Burette reading (ml) Initial 0 0 Final 9.3 9.3 Methyl Orange Volume of HCl (ml) 9.3 9.3

TABLE 4.3: OBSERVATION TABLE Phenolphthalein Sl No: Volume of HCl added (ml) 1 2 3 4 5 6 7 8 9 10 20 20 20 20 20 20 20 20 20 20 5 5 6 6 8 8 9 9 10 10 Flow rate (LPH) Initial 0 7.6 0 5.4 0 5.2 0 5 0 4.8 Volume of NaOH (ml) Final 7.6 15.2 5.4 10.8 5.2 10.4 5 10 4.8 9.6 Volume of NaOH (ml) 7.6 7.6 5.4 5.4 5.2 5.2 5 5 4.8 4.8

CALCULATION 1. Normality of NaOH NNaOH = (V x N) oxalic acid / volume of NaOH = (10 x 0.1) / 8.8 = 0.1136 N
2. Normality of HCl

NHCl

= (V x N)sodium carbonate / volume of HCl = (20 x0.099)/19.5 =0.1075 N

3. Volume of the CSTR

= x d2 x h / 4 =3.14x152x15/4 =2649.375cm3 =2.649l

4. Model calculation set 3 CA0 V = 0.1136 moles/litre = (V x N) HCl / NNaOH = 20 x 0.1075 / 0.1136 = 18.926 ml CA = (V titer value) x CA0 of mixture / (volume of mixture + HCl) = (18.926 5.2) x 0.1136 / (20 + 20) = 0.38981 moles/L XA = 1-(CA / CA0) = 1- (0.38981 / 0.1136) = 0.6568 XA / (1-XA)2 CA0 x (v / v0) = 5.5782 = 0.1136 x 2.6491 / 8 = 0.0355 mol hr/L

5. TABLE 4.4: CALCULATION TABLE XA / (1-XA)2

Sl No: 1 2 3 4 5

Flow rate (LPH) 5 6 8 9 10

CA (mol / L) 0.035 0.03841 0.03898 0.03954 0.040117

XA

CA0 (mol s/L)

0.69184 0.66184 0.6568 0.6518 0.6468

7.286 5.788 5.5782 5.37787 5.18658

0.0568 0.04733 0.0355 0.03155 0.0284

6. GRAPH 4.1:

XA/(1-XA)2 vs CA0
8 7 6 XA / (1-XA)2 5 4 3 2 1 0 0 0.01 0.02 0.03 CA0 0.04

(mol s/ L)

0.05 0.06 y = 65.063x + 3.2463 R = 0.8492

4.6 RESULT A graph of XA/(1-XA)2 vs CA0 is plotted and the value of k is determined to be 0.018L/mol.s.