CL451: Process Dynamics and Control Lab 14 Sept

CL 451

Process Dynamics and Control

Lab

Exp 6: Saponification in Batch

Reactor

Group A:

1. Aditya Shekhar Sinha 19110002

2. Akhilesh Chauhan 19110003
3. Akshay Chourasiya 19110004

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CL451: Process Dynamics and Control Lab 14 Sept

Aim:
To determine the rate constant of a reversible second order saponification reaction at room
temperature using Batch Reactor.

Assumptions:
- Ideal Batch Reactor, hence infinite mixing.
- Temperature is assumed to be constant at room temperature (298 K)
- No volume change throughout the course of the experiment.
- It is assumed that the conductivity value does not depend on the placement of the
conductivity probe inside the reactor.

Observations:
Table1: Observed Values of Conductivity vs Concentration of NaOH
Concentration of NaOH, Conductivity meter
gmol/lt reading, mS/cm
0.01 1.818
0.02 3.821
0.03 5.945
0.04 7.839
0.05 9.899

Fig1: Calibration curve

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 CL451: Process Dynamics and Control Lab 14 Sept

Table2: Time taken to reach steady state and calculated conversion (theoretical and experimental)
from the conductivity and concentration data

Conductivity
meter Concentration of kCA0[(1-XA)2-(X
Time (s) Xa EXP ΔXA/dt XA Theoritical
reading, NaOH, gmol/lt A2/KC)
mS/cm

0 9.789 0.049447968 0.011040634 0 0 0.048902031

30 9.22 0.046628345 0.067433102 0.001879749 0.094954125 0.043484051

60 8.626 0.043684836 0.126303271 0.001962339 0.173439458 0.038167299

120 7.814 0.039661051 0.206778989 0.001341262 0.295608703 0.031459979

180 7.278 0.037004955 0.259900892 0.000885365 0.386314143 0.027387334

300 6.589 0.033590684 0.328186323 0.000569045 0.511996033 0.022566681

420 6.167 0.031499504 0.370009911 0.00034853 0.594949693 0.019844376

600 5.79 0.029631318 0.407373637 0.000207576 0.677245207 0.0175603

900 5.455 0.027971259 0.440574827 0.000110671 0.758890375 0.015647826

1080 5.338 0.027391477 0.452170466 6.44E-05 0.790663124 0.01500586

1260 5.253 0.026970268 0.460594648 4.68E-05 0.815037024 0.014547907

1440 5.191 0.026663033 0.466739346 3.41E-05 0.834326974 0.014218346

1620 5.141 0.026415263 0.471694747 2.75E-05 0.849973381 0.013955322

1800 5.102 0.026222002 0.47555996 2.15E-05 0.86291947 0.013751868

1980 5.07 0.026063429 0.478731417 1.76E-05 0.873808758 0.013586047

2100 5.052 0.025974232 0.480515362 1.49E-05 0.880155496 0.013493214

2400 5.018 0.025805748 0.483885035 1.12E-05 0.893541247 0.013318733

slope (k) 0.069944245

Using the Linest Function in Excel, we calculated the slope of the below curve substituting
intercept to be 0 and the slope is our rate constant, k = 0.069944245 [L/g-mol-s]

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CL451: Process Dynamics and Control Lab 14 Sept

Fig2: we have put the intercept = 0, knowing the fact that initially the conversion is 0 and hence,
dX/dt = 0

Calculations:
𝑚𝑜𝑙 𝑤𝑒𝑖𝑔ℎ𝑡* 𝑉 (𝑙) *𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦
Weight to NaOH required = 𝑛−𝑓𝑎𝑐𝑡𝑜𝑟

Amount of NaOH required to make 0.5L of 0.05 Normality after putting in the above formula
- Weight of NaOH required: 1 g

𝑚𝑜𝑙 𝑤𝑒𝑖𝑔ℎ𝑡* 𝑉 (𝑙) *𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦

Weight to Ethyl Acetate required = 𝑛−𝑓𝑎𝑐𝑡𝑜𝑟

Amount of EA required to make 0.4L of 0.05 Normality after putting in the above formula
- Weight of EA required: 1.76 g
- Density of Ethyl Acetate = 0.902 g/ml
- Volume of Ethyl Acetate required: 1.96 ml

Calibration Curve Calculation

We found the relationship between conductivity and concentration of NaOH, which came to
be a straight line with the following equation:
y = 201.8x - 0.1896
- Here, y is conductivity (mS/cm) and x = Concentration (mol/L)

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CL451: Process Dynamics and Control Lab 14 Sept

Fig3: Concentration(mol/L) vs Time (s)

Design equation in terms of conversion:

𝑑𝑋𝐴 ∆𝑋𝐴 2 2
𝑑𝑡
≈ ∆𝑡
= 𝑘𝐶𝐴 [(1 − 𝑋𝐴) − (𝑋𝐴 /𝐾𝐶)]
0

Where 𝐾𝐶 = 10^(3885.44/T)

We have neglected the 2nd term (X2A/KC) while calculating the theoretical conversion because of the
very large value of Kc and neglecting it makes our calculations simple as well as not adding much
error.

Hence, we calculated XA theoretical by integrating the remaining equation and we get:

𝑘*𝐶𝐴𝑂*𝑡
= 𝑋𝐴 = 1+𝑘*𝐶𝐴𝑂*𝑡

Results:
- Forward reaction rate for saponification reaction = 0.07 (L/g-mol/s)

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CL451: Process Dynamics and Control Lab 14 Sept

Sources of Error:
- We observe from the plots that theoretical and experimental data are similar initially, but they
diverge out eventually. This happened because we neglected the term responsible for
backwards reaction to avoid complex calculations. As the reaction progresses forward,
backward reaction becomes significant which is not depicted by the theoretical curve.

Fig4: Theoretical and experimental Conversion

- Human Error
- Conductivity probe error in measurement.
- The temperature might not remain constant at 298 K and may fluctuate.
- Parallax Error