KRD_exp4_Iso_BR

February 16, 2022

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EXPERIMENT 4 - ISOTHERMAL BATCH REACTOR

0.0.1 AIM:
To determine the rate constant for the saponification of ethyl acetate with NaOH in a isothermal
batch reactor.

0.0.2 THEORY:
A batch reactor is a closed system such that no stream enters or leaves the reactor. In homogeneous
reactions, all reacting species remain in a single phase. This reactor is very much suitable for liquid
phase reactions. The rate of reaction of any reaction component A is defined as
( )
−rA = V1 dN dt
A
= ( moles (ofunit
A which disappear by reaction )
volume )( unit time )

Rate of reaction is influenced by variables like temperature, pressure, and concentration. The rate
of reaction is a function of concentration at constant temperature, i.e. -r A = k C An where n is the
order of reaction. The interpretation of the kinetic data is a trial and error procedure. A kinetic
model is first selected with a corresponding rate equation, and the concentration-time relationship
predicted by the model is matched with experimental data.
For a second order unidirectional reaction,
2 A −→ Product
Rate of reaction can also be expressed as moles of A disappearing per unit volume per unit time.
( ) ( )
−rA = V1 dN dt
A
= dCA
dt = kCA2

Integration yields:
1 1
= kt +
CA CAo
Where, CAO = Conc. of A at t = 0; CA = Conc. of A at t = t
1
By plotting CA vs t we get the slope as k

[4]: import numpy as np

import pandas as pd
from matplotlib import pyplot as plt

1
[5]: N1 = 0.1*10/9.5
naoh = np.array([20,16,12,8,4,0])
h2o = np.array([0,4,8,12,16,20])
V2 = 20
N2 = N1*naoh/V2
cond_1 = np.array([26,20.7,15.16,10.65,5.72,8.93e-3])
xa = np.array([100,80,60,40,20,0])
cond_2 = np.array([6.84,10.46,14.37,18.11,22.2,26])
tab1 = pd.DataFrame({'H2O (ml)':h2o,'NaOH (ml)':naoh,'Normality':␣
,→N2,'Conductivity mS/cm': cond_1})

tab2 = pd.DataFrame({'NaOH (ml)':h2o,'SA (ml)':naoh,'Conversion (X_A)':␣

,→xa,'Conductivity mS/cm': cond_2})

0.0.3 NaOH Calibration chart

[6]: tab1

[6]: H2O (ml) NaOH (ml) Normality Conductivity mS/cm

0 0 20 0.105263 26.00000
1 4 16 0.084211 20.70000
2 8 12 0.063158 15.16000
3 12 8 0.042105 10.65000
4 16 4 0.021053 5.72000
5 20 0 0.000000 0.00893

[7]: plt.plot(N2,cond_1)
plt.title('NaOH Calibration chart')
plt.xlabel('Normality')
plt.ylabel('Conductivity (mS/cm)')
plt.grid()

2
 y = 243.62x + 0.2252
slope = 243.62
intercept = 0.2252

0.0.4 NaOH + Sodium Acetate Calibration (product)

[8]: tab2

[8]: NaOH (ml) SA (ml) Conversion (X_A) Conductivity mS/cm

0 0 20 100 6.84
1 4 16 80 10.46
2 8 12 60 14.37
3 12 8 40 18.11
4 16 4 20 22.20
5 20 0 0 26.00

[9]: plt.plot(cond_2,xa)
plt.title('NaOH + SA Calibration chart')
plt.xlabel('Conductivity (mS/cm)')
plt.ylabel('Conversion (X_A) %')
plt.grid()

3
 y = -5.1932x + 134.81
slope = -5.1932
intercept = 134.81

0.0.5 DATA:
[17]: t1 = np.linspace(0,60,7)
t2 = np.linspace(120,1080,17)
samp_time = np.concatenate((t1,t2))
cond_3 = np.array([13.5,12.75,12.63,12.5,12.21,12.15,12,11.6,11.2,11,10.95,10.
,→85,10.79,10.73,10.7,10.68,10.67,

10.66,10.65,10.64,10.63,10.62,10.61,10.6])
xa = ((-5.1932*cond_3) + 134.81)/100
ca = 0.1*(1-xa)
yaxis = 1/ca
obs = pd.DataFrame({'Sampling time, s':samp_time,'Conductivity mS/cm':␣
,→cond_3,'Conversion (X_A)':xa,'1/C_A':yaxis})

obs

[17]: Sampling time, s Conductivity mS/cm Conversion (X_A) 1/C_A

0 0.0 13.50 0.647018 28.330056
1 10.0 12.75 0.685967 31.843787
2 20.0 12.63 0.692199 32.488507

4
 3 30.0 12.50 0.698950 33.217074
4 40.0 12.21 0.714010 34.966292
5 50.0 12.15 0.717126 35.351454
6 60.0 12.00 0.724916 36.352532
7 120.0 11.60 0.745689 39.321902
8 180.0 11.20 0.766462 42.819511
9 240.0 11.00 0.776848 44.812504
10 300.0 10.95 0.779445 45.340082
11 360.0 10.85 0.784638 46.433404
12 420.0 10.79 0.787754 47.115078
13 480.0 10.73 0.790870 47.817065
14 540.0 10.70 0.792428 48.175962
15 600.0 10.68 0.793466 48.418234
16 660.0 10.67 0.793986 48.540287
17 720.0 10.66 0.794505 48.662956
18 780.0 10.65 0.795024 48.786247
19 840.0 10.64 0.795544 48.910164
20 900.0 10.63 0.796063 49.034712
21 960.0 10.62 0.796582 49.159897
22 1020.0 10.61 0.797101 49.285722
23 1080.0 10.60 0.797621 49.412193

[14]: plt.plot(samp_time[:12],yaxis[:12])
plt.title('NaOH + SA Calibration chart')
plt.ylabel('1/C_A')
plt.xlabel('sampling time, s')
plt.grid()

5
y = 0.0465x + 32.142
slope = 0.0465
intercept = 32.142

0.0.6 CONCLUSIONS:
The slope of the above graph gives k (rate constant) which is 0.0465 (mol/l)−1 min−1

0.0.7 PRECAUTIONS
1. All solutions should be prepared accurately and must be standardized.
2. Titrations should be carried out precisely.
3. The individual reactants must be first pre-heated to the reaction temperature.
4. While fixing the conductivity meter, care should be taken.
5. Before starting the flow rate of ethyl acetate, temperature should be set at desired tempera-
ture.
6. All the glass wares to be used should be properly rinsed prior to use.