JADAVPUR UNIVERSITY

Faculty of Engineering & Technology

Department of Chemical Engineering
Reaction Engineering & Thermodynamics Laboratory

SECTION : A2
EXPERIMENT : ISOTHERMAL SEMI BATCH REACTOR
GROUP : 03

Name Roll No.

Shantanu Hazra 001810301112
Anik Mondal 001810301113
MD Faisal 001810301114
Marshal Murmu 001810301115
Protim Das 001810301116
Aims of The Experiment 2

• To study a second order saponification reaction (between Ethyl Acetate &

Sodium Hydroxide) in a isothermal semi batch reactor (i.e. at a fixed
temperature).
• To determine experimentally the reaction rate constant k or variation of
concentration of Sodium Hydroxide with time in the semi batch reactor.
Summary of Experimental Procedure 3
 

Diagram:
 Summary of Experimental Procedure cont. 4
 

• First, we prepare standardized chemical solutions, we fill the stirred tank semi batch reactor initially with NaOH
solution (A) and fill the feed tank with Ethyl Acetate (B) of known concentration and volume.
• After that, using temperature controller we set a steady state temperature of water bath to maintain the isothermal
condition. We set the flowrate of ethyl acetate with the help of compressed air and rotameter calibration.
• After that, at different time intervals we pipette out 10 mL of sample and mix it with the 20 mL quench HCl
solution to neutralize the unreacted NaOH present in the product sample.
• Now, the excess amount of HCl left after neutralization is find by the acid-base titration method with the help of
standardized NaOH present in burette and Phenolphthalein as indicator.
• This way, we prepare a table to calculate the concentration of unreacted NaOH with time along with the increasing
volume of reactant and product mix inside the reactor.
 Results & Findings : Table 5
Volume of NaOH Concentration of
Amount of HCl reacted
required to Unreacted NaOH Conversion of Moles of NaOH in Average K
Time Reaction with unreacted NaOH = k (L/gmol-
neutralize = Ca = (HCl)r * NaOH = Xa = 1 - the mix = Na = Ca * (-) dNa/dt (L/gmol-
(min) Volume (L) (HCl)r = (HCl)o - min)
(burrete reading) (1000/Sample (Ca*V/Ca0*Vo) V(L) min)
(V(NaOH)*N(NaOH)/1000)
(ml) taken)
RUN-1 2 12.4 1.166666667 0.000858 0.0858 0.046666667 0.1001 0.00664 6.57699241
( 5 LPH) 4 14 1.333333333 0.00069 0.069 0.123809524 0.092 0.00628 4.47612259
6 15.9 1.5 0.0004905 0.04905 0.299285714 0.073575 0.00592 6.49761347
8 16.7 1.666666667 0.0004065 0.04065 0.354761905 0.06775 0.00556 4.64965556 5.60976622
10 17.9 1.833333333 0.0002805 0.02805 0.510238095 0.051425 0.0052 6.22962456
12 18.4 2 0.000228 0.0228 0.565714286 0.0456 0.00484 5.22858871

Volume of NaOH Concentration of

Amount of HCl reacted
required to Unreacted NaOH Conversion of Moles of NaOH in Average K
Time Reaction with unreacted NaOH = k (L/gmol-
neutralize = Ca = (HCl)r * NaOH = Xa = 1 - the mix = Na = Ca * (-) dNa/dt (L/gmol-
(min) Volume (L) (HCl)r = (HCl)o - min)
(burrete reading) (1000/Sample (Ca*V/Ca0*Vo) V(L) min)
(V(NaOH)*N(NaOH)/1000)
RUN-2 (ml) taken)
( 7.5 2 13 1.1875 0.000795 0.0795 0.100892857 0.09440625 0.0044 6.78570568
LPH) 4 14.2 1.375 0.000669 0.0669 0.123928571 0.0919875 0.0053 3.23523106
6 15.8 1.5625 0.000501 0.0501 0.254464286 0.07828125 0.0062 4.19056068
5.51734903
8 16.9 1.75 0.0003855 0.03855 0.3575 0.0674625 0.0071 4.9162868
10 17.7 1.9375 0.0003015 0.03015 0.443660714 0.058415625 0.008 5.62570658
12 18.6 2.125 0.000207 0.0207 0.581071429 0.0439875 0.0089 8.35060337
 Results & Findings : Graph 6

RUN-1 RUN-2
No. of moles of unreacted NaOH in reactor vs Time No. of moles of unreacted NaOH in reactor vs Time
0.12 0.1
Na (mole)

0.09 f(x) = − 0 x² − 0 x + 0.1

0.1 R² = 0.99
f(x) = 0 x² − 0.01 x + 0.12 0.08
0.08 0.07
0.06

Na (Mole)
0.06 0.05
0.04
0.04
0.03
0.02 0.02
0.01
0
0 2 4 6 8 10 12 14 0
1 2 3 4 5 6 7 8 9 10
Time (min) Time (min)
Results & Findings : Sample Calculation 7
Volumetric feed rate of ethyl acetate, F = 5 LPH
Time of collection of sample, t = 6 min
Initial volume of reaction mass at reactor = 1 Liter
 5× 6 
Volume of the reaction mass at time t, V = V0 + Ft =  1 +  = 1.5 Liter
 60 
Volume of 0.105 N NaOH used for neutralizing unreacted HCl in the quench, VNaOH = 15.9 mL
Volume of 0.108 N HCl taken as quench, VHCl = 20 mL
VHCl × N HCl
Amount of HCl taken as quench, HCl 0 = gmol = 0.00216 gmol
1000
VNaOH × N NaOH
Amount of HCl reacted with the unreacted NaOH of the reaction sample, HCl R = HCl 0 -
1000
15.9× 0.105
= 0.00216 - gmol
1000
= 0.0004905 gmol
 Results & Findings : Sample Calculation Cont. 8
Volume of sample added to quench, VS = 10 mL
HCl R ×1000 0.0004905×1000
Concentration of unreacted NaOH in the reaction mixture, CA = = = 0.04905 gmol / L
VS 10
Number of moles of the unreacted NaOH in the reaction mixture, N A = CA × V = 0.04905×1.5 = 0.073575 gmol
Now, we fit the N A vs T data to a polynomial : N A = a 0 + a1t + a 2t 2
We use a spreadsheet to find the values of constants,
a0 = 0.115 , a1 = - 0.007 , a 2 = 9×10-5
dN A
Now, -
dt
 
= -  a1 + 2a 2 t  = 0.007 - 6× 2× 9×10 -5 = 0.00592

dN A
- ×  V0 + Ft 
dt 0.00592×1.5 L
Hence, The reaction rate constant, k = =
N A ×  FtCB0 -  V0CA0 - N A    5× 6× 0.1   gmol × min
0.073575×   -  0.105 - 0.073575  
 60  
L
= 6.49761347
gmol × min
Discussions 9

• The rate constant value can be depicted to be approximately in the range of 5-6 L/gmol-min.
• Semi Batch reactors are advantageous when we want to maximize the desired product for
one reactant by maximizing the instantaneous selectivity.
• The flowrate of ethyl acetate is maintained in such a way that the reactor must not overflow
and also this flowrate is important when there are series-parallel reactions.
• The temperature of the reactor during operation must be kept constant so that rate we get
rate constant is only function of concentration.