EXPERIMENT No: RK-1 Homogeneous Batch Reactor-1

Objective:
To determine the order and value of the rate constant for the homogeneous liquid phase reaction of caustic soda with ethyl acetate in a batch reactor:

NaOH + CH 3 COOC2 H 5

C2 H 5OH + CH 3COONa

Introduction
A batch reactor may be described as a vessel in which chemicals are placed to react. Batch reactors are normally used in small-scale laboratory set-ups to study the kinetics of chemical reactions. To determine the order and rate constant of a chemical reaction, the variation of a property of the reaction mixture is observed as the reaction progresses. Data collected usually consist of changes in variables such as concentration of a component, total volume of the system or a physical property like electrical conductivity or refractive index. The data are then analyzed using pertinent equations to find desired kinetic parameters.

Theory For any given reaction in a constant volume system, the rate of the reaction can be represented by:

rA = kf ( C A ) =

dC A dt

(1)

Where rA is the rate of disappearance of reactant A among the reacting species. Equation (1) can be rearranged to give:
dC
A A

f (C )

= kdt

(2)

Integrating equation (2) analytically yields

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Af

CA

t dC A = k dt = kt f (C A ) o

(3)

By postulating various forms for f(CA) in equation (3) and correlating the resulting equation with the experimental data, the rate constant k, and order of the reaction can be determined assuming that the rate of reaction can be expressed by an equation of the form:
n ( rA ) = kC A

(4)

The values of n and k can be determined experimentally, and has also been reported in literature.

Procedure

1)

In the reactor (see Figure 1), mix 1.0 liter of the 0.1M caustic soda solution with 1.0 liter of the 0.1M ethyl acetate solution at an arbitrary time (t = 0) at room temperature. Switch on the stirrer immediately and set it to an intermediate speed to avoid splashing. Start the timer as soon as you start mixing the reactants. After a certain time interval, use a pipette to withdraw 25ml sample from the reactor, and immediately quench it with 25ml of excess 0.05M hydrochloric acid.[You should have the quenching acid sample ready before taking the sample from the reactor.] Add 2 - 3 drops of phenolphethalene to the quenched sample and back titrate with 0.05M NaOH solution until the end point is detected (in this case a stable pink color) . Record the amount of NaOH used in the titration (Vtit.). Repeat steps (3) - (5) every 3 minutes for the first five samples and thereafter every 5 minutes. Take a total of 14 samples making sure that you record the time for each new sample.

2) 3)

4)

5) 6)

Note : It is recommended that you prepare the 25ml quenching acid samples in different flasks before starting the reaction.

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Stirrer

Inlet orifice

Thermometer

Reactor wall

Reaction mixture

Drain valve

Figure 1: Batch Reactor Set-up

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Report Requirement

1.

Using the volume of 0.05M NaOH used in the titration, calculate the concentration (in mol/lit) of unreacted NaOH in each sample withdrawn from the reactor. The following equation may be used:

CA =
Note

[ 25.0 - Vtit. ] xCA 0

25.0

(mol/lit)

(5)

You should know the basis of this equation, and that this is not a general formula for all cases. Here CA0 is the concentration of the standard NaOH solution.

2.

Apply the integral method of analysis to determine the reaction order and rate constant of the reaction. This could be done as follows : a. Assume an expression (f(CA)) for the reaction rate (zero-order, 1st order, 2nd order etc.) b. Substitute the expression into equation (3) and integrate. c. Rearrange the resulting expression and plot. Note : all the above steps should be shown in the report

3.
Note

From the literature, find both the order and rate constant of the reaction.
You must mention in your report the exact reference i.e. title, author and page number of the source from which you obtained the values. Also attach a copy of the page containing the information.

4.

Compare between the theoretical and experimental values and give reasons for the deviations.

Nomenclature

CA CAf

= Concentration of A, mol/lit. = Final concentration of reactant A (mol/lit) = Inlet concentration of A, mol/lit = Rate constant for the reaction. = Order of reaction = rate of reaction moles A/lit. sec.

C A0
k n

rA

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t V Vtit.

= time, min. = Volume of mixture, lit = Volume of NaOH used in titration (ml)

References

1.

Levenspiel, O., "Chemical Reaction Engineering", 2nd ed., Wiley and Sons, N.Y., p. 41 (1977). Smith, J.M., "Chemical Engineering Kinetics", 3rd ed., McGraw-Hill Book Comp., N.Y., p. 37 (1981). Holland, C. D "An Introduction to Chemical Engineering Kinetics & Reactor Design. " Chp. 8, John Wiley Inc., N.Y., (1977).

2.

3.

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LOG SHEET FOR EXPERIMENT RK-1

Names and ID # students:

1: ________________________ ID# __________ 2: ________________________ ID# __________ 3: ________________________ ID# __________

Date: Table 1: Experimental Data Sample # Time (min) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 3 6 9 12 15 20 25 30 35 40 45 50 55 60 Initial Burette reading [R1] (ml) Final Burette reading [R2] (ml) Volume NaOH used in Titration [R2-R1](ml)

Sample Volume = 25ml Volume of 0.05M HCl used in quenching = 25 ml

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