Batch CSTR Experiment

Experimental Determination of Kinetic Rate Constants Using Batch and CSTR Reactors
CHE-431 UNIT OPERATIONS LAB I
Department of Chemical Engineering University of Tripoli Libya
Instructor
Dr. A. A. Ballut
Spring Semester / 2012
CHE-431 UNIT OPERATIONS LAB I / SPRING 2012

Experimental Determination of Kinetic Rate Constants Using Batch and CSTR Reactors
Dr. A. A. BALLUT
In this experiment, the use of both a batch reactor and a CSTR will be demonstrated to generate data for the determination of kinetic parameters. The reaction The reaction selected in this experiment is the saponification of ethyl acetate. This reaction is elementary and second-order. The reaction equation is
NaOH + CH 3 COOC 2 H 5 CH 3 COONa + C 2 H 5 OH
A + B The apparatus
+ D
The apparatus is the Armfield continuous stirred tank reactor which is designed to study the kinetics of a chemical reaction in this type of reactor (as well as the special case when it is run as a batch reactor). It can conveniently be used to study the effects of varying the process conditions such as reaction temperature, reactor volume, stirring rate, feed rate etc. on reaction kinetics.
General Procedure
The reactor volume can be varied by adjusting the height of the internal standpipe. The actual volume can be checked by filling the reactor with water to the overflow then draining the reactor contents into a measuring cylinder. For the CSTR experiment, the feed pumps should be calibrated. This can be achieved by pumping water from the reagent tanks to a measuring cylinder over a time period for a range of pump speeds. A calibration graph for each pump of % speed vs. flow rate (ml/min) can then be drawn. The conductivity of the reacting solution in the reactor changes with the degree of conversion and this provides a convenient method for monitoring the progress of the reaction either manually or by computer. In this experiment, the manual procedure is used. Thus, the conductivity can be recorded manually at suitable time intervals (half a minute or so) by reading the value directly from the conductivity meter in the console. The reaction temperature can be varied and maintained using the special heater available in accordance with the instructions given in the Armfield manual which is available on this companys website or can be accessed by clicking Armfield manual as given in the website www.the-seventh-dimension.com.
Theory For a bimolecular second order reaction, the rate equation is:
r = k C AC B
The stoichiometric equations in terms of fractional conversion X are:C A = C Ao C A o X A = C A o (1 X A ) C B = C Bo C Bo X B
But when ,
C Ao = C Bo and C Ao X A = C Bo X B
Then, C B is also equal to C A o (1 X A ) and the rate equation becomes:r = kC A o 2 (1 X A )2
A) Batch Reactor
For a constant volume isothermal batch reactor, the component mass balance equation is:
1 dN A dC A = = (rA )app = r V dt dt
(1)
Combining the above equations, equation (1) becomes:dC A = kC Ao 2 (1 X A ) 2 dt
But
dC A dX A = C Ao dt dt
Then the result is:dX A kC A o (1 X A ) 2 dt
Integration will yield:

XA = k t C Ao 1XA
(2)
Equation (2) can be easily used to determine the value of k. B) CSTR For an isothermal steady state CSTR, the component mass balance equation is:
FAo FA + V (rA )app = 0
Since for a flow reactor C A = FA / Q and since Q is constant ( constant volume system), then this equation becomes:QC Ao QC A + V (r ) = 0
Substituting for r , and using the previously mentioned stoichiometric equations, the following equation can be obtained:XA V = Q kC Ao (1 X A ) 2
(3)
Equation (3) can then be used to determine the value of k.
Conductivity as a measure of conversion The measurements of conductivity are related to the conductivity of a sodium hydroxide (A) and sodium acetate (C) solution as follows: = A + C where : A = 0.195 [1 + 0.01184(T 294)]C A C = 0.07 [1 + 0.0284(T 294)]C C For T > 294K For T > 294K
Using the stoichiometric equations given previously to eliminate CA and CC in terms of XA , then an equation for XA in terms of , C Ao , and T can be easily obtained (eq. 4). You need to derive such an equation in the simplest possible form and use it. Use of the equations in the Armfield Manual to calculate conversion is not acceptable. Report
The report should conform to the outline provided to you by the Lab instructors. Your grade will depend to a great extent on following that outline closely. In addition to that, the following should be included in the report:1) Detailed derivation of equations (2) and (3) as well as eq.( 4) mentioned previously for calculating XA. 2) Determination of the rate constant of the reaction from the data obtained using the batch reactor and the CSTR. Sample calculations are required. 3) Comparison of results obtained from both reactors, as well as comparison with the experimental data reported in the literature for similar conditions. 4) Comments on the differences in the results obtained and discussion of the results and the quality of the data and experimental procedures (difficulties and uncertainties).
References 1. Levenspiel, O., Chemical Reaction Engineering, John Wiley & Sons, Toronto, Ed. 2, 1972, p. 283-90. 2. Armfield manual.

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Experimental Determination of Kinetic Rate Constants Using Batch and CSTR Reactors

CHE-431 UNIT OPERATIONS LAB I

Department of Chemical Engineering University of Tripoli Libya

Spring Semester / 2012

CHE-431 UNIT OPERATIONS LAB I / SPRING 2012

The stoichiometric equations in terms of fractional conversion X are:C A = C Ao C A o X A = C A o (1 X A ) C B = C Bo C Bo X B

Then, C B is also equal to C A o (1 X A ) and the rate equation becomes:r = kC A o 2 (1 X A )2

Combining the above equations, equation (1) becomes:dC A = kC Ao 2 (1 X A ) 2 dt

Then the result is:dX A kC A o (1 X A ) 2 dt

Integration will yield:

Equation (3) can then be used to determine the value of k.

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