BATCH REACTOR

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

Reaction: (A) CH3COOC2H5+(B) NaOH (C)CH3COONa + (D) C2H5OH

Apparatus required: Heater with magnetic stirrer, Thermometer, conductivity meter with
temperature sensor, glass beakers, measuring cylinders, pipettes and stop watch.

Chemicals required: Sodium Hydroxide, Ethyl Acetate and Distilled Water

Procedure:

1. Prepare stock solution of Sodium Hydroxide of 0.05N and then use some of the stock
solution to find the calibration curveof conductivity vs. concentration of NaOH

2. Now find out the volumes of Ethyl Acetate and Sodium Hydroxide required by choosing
theconstant reactor volume and make the molar ratio (i.e., ratio of moles of Ethyl Acetate to
moles of Sodium Hydroxide) equal to one

3. Add the calculated volume of NaOH into the reactor. Start the stirrer. Switch on the
conductivity meter

4. Switch on the heater and set the temperature at the desired value. So the temperature in the
reactor is maintained at the required temperature

5. Add the required (calculated) volume of Ethyl Acetate solution (preheated to the required
temperature) to the reactor and at the same time start the stopwatch

6. At different time intervals of 30s, 1, 2, 3, 5, 7, 10, 15 …….min, note down the conductivity
meter reading (conductivity in mS/cm) of the reaction mixture

7. This procedure is continued until no change in the value of conductivity meter reading is
observed

8. Determine the concentration of unreacted NaOH in the reaction mixture by using the
conductivity vs. concentration of NaOH calibration curve

Theory:

The Batch reactor is the generic term for a type of vessel widely used in the process
industries. In a batch reactor the reactants and the catalyst are placed in the reactor and the
reaction is allowed to proceed for a given time whereupon the mixture of unreacted material
together with the products is withdrawn. Provision for mixing may be required. In an ideal
batch reactor, the concentration and temperature are assumed to be spatially uniform. In
practice, the condition can be approximately realized by vigorous agitation or stirring.All the
elements of the fluid spend the same amount of time in the reactor, and hence have the same
residence time. From the viewpoint of thermodynamics, a batch reactor represents a closed
system. The steady states of the batch reactor correspond to states of reaction equilibria.
Batch reactors are simple and needs little supporting equipment, and are therefore ideal for
small scale experimental studies on reaction kinetics.Industrially it is used when relatively
small amounts of material are to be treated and when the product demand varies. Batch
reactors are often used in the pharmaceutical industry, where small volumes of high-value
products are made.
Researchers typically use a batch reactor to study reaction kinetics under ideal conditions. A
batch reactor can be used to find the reaction rate constant,activation energy and order of the
reaction.
The data reflect the intrinsic kinetics for the reaction being investigated. A typical batch
reactor consists of a tank with an agitator and integral heating/cooling system. Liquids and
solids are usually charged via connections in the top cover of the reactor. Vapours and gases
also discharge through connections in the top. Liquids are usually discharged out of the
bottom.

The advantages of a batch reactor lie in its versatility. A single vessel can carry out a
sequence of different operations without the need to break containment. This is particularly
useful when processing, toxic or highly potent compounds.

Sample Observation Table:

For Calibration curve: (At a particular temperature)

Concentration of NaOH, gmol/lt Conductivity meter reading, mS/cm

Calculation Table:

Time, min Conductivity Concentration of Conversion of Δ𝑿𝑿𝑨𝑨 /Δ𝒕𝒕

meter reading, NaOH, gmol/lt NaOH
mS/cm

Rate equation for a second order reversible reaction:

−𝒅𝒅𝑪𝑪𝑨𝑨
-rA= = 𝒌𝒌[𝑪𝑪𝑨𝑨 𝑪𝑪𝑩𝑩 − (𝑪𝑪𝑪𝑪 𝑪𝑪𝑫𝑫 /𝑲𝑲𝑪𝑪 )]
𝒅𝒅𝒅𝒅

Assume𝑪𝑪𝑨𝑨𝟎𝟎 = 𝑪𝑪𝑩𝑩𝟎𝟎

Design equation in terms of conversion:

𝒅𝒅𝑿𝑿𝑨𝑨 𝚫𝚫𝑿𝑿𝑨𝑨
≈ = 𝒌𝒌𝑪𝑪𝑨𝑨𝟎𝟎 [(𝟏𝟏 − 𝑿𝑿𝑨𝑨 )𝟐𝟐 − (𝑿𝑿𝑨𝑨 𝟐𝟐 /𝑲𝑲𝑪𝑪 )]
𝒅𝒅𝒅𝒅 𝚫𝚫𝒕𝒕
Where 𝑲𝑲𝑪𝑪 = 10^(3885.44/T)

Graph: plot Δ𝑿𝑿𝑨𝑨 /Δ𝒕𝒕vs 𝑪𝑪𝑨𝑨𝟎𝟎 [(𝟏𝟏 − 𝑿𝑿𝑨𝑨 )𝟐𝟐 − (𝑿𝑿𝑨𝑨 𝟐𝟐 /𝑲𝑲𝑪𝑪 )] and find out rate constant (𝒌𝒌)

Result:
The rate constant for the saponification of ethyl acetate with NaOH at a temperature of _____
ºC is, k =……………. (L/g.mol-sec).

Expectations:

• Find forward reaction rate constant

• Plot XA Vs time: both experimental and predicted

Questions to ponder about

1. What is Saponification? What are it’s by products and their uses?

2. Why do we measure the conductivity of NaOH, but not of CH3COOC2H5?
3. What is the effect of temperature on the conversion of this saponification reaction?
4. What is a limiting reagent?
5. What are uses of Batch reactor?
6. What parameters are to be modified in this reaction to yield good conversions?
7. How can we increase the compatibility of X vs t between experimental and
theoretical?
8. Draw X vs T for reversible exothermic reaction.
9. Difference between conductivity and conductance?
10. What is a standard solution? Difference between primary and secondary solutions and
give examples?
11. Can we do simulations for this type of experiments? If yes, what type of soft wares
available?
12. Mention the other ways of finding the concentration of unreacted NaOH. So which is
the best method and why?
13. What is the effect of rate constant (k), on the conversion (X)?
14. Conductivity cell and its working principle?