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The objective of the experiment is to the study a non catalytic homogeneous phase
(saponification) reaction in a straight tube plug flow reactor.
Aim
To determine the reaction rate constant, k for the given saponification reaction of ethyl
acetate in aqueous sodium hydroxide solution.
To study the progress of reaction under ambient conditions at different flowrates of
reactant.
Introduction
Plug flow reactor is also called as the tube flow reactor. In a plug flow reactor, the
concentration of reactant decreases progressively through the system. A plug flow reactor is
more efficient than the mixed flow reactors for a reaction to get higher conversion at given
reaction conditions. In an ideal plug flow reactor (PFR) there is no mixing in the direction of
flow and complete mixing perpendicular to the direction of flow. Concentration of the
reactant varies along the length of the reactor but remains constant in the radial direction.
Theory
Reaction
We consider the equimolar reaction of A and B. The reaction can hence be written as 2A B
Assuming the reaction under study is a second order reaction (n = 2)
A plot of 1/CA vs. τ gives a straight line graph for an assumed second order reaction with slope
equal to the rate constant k
The set up consists of two feed tanks through which the reactants are fed to the reactor. The
setup is provided with rotameters to measure the individual flow rate of chemicals. The flow
rate can be adjusted by operating the needle valve on the respective rotameter. The overhead
tank system is used for circulation of feed with the help magnetic pumps. Reactor inlet is also
provided with a facility to inject tracer. Products coming out from the reactor are analyzed by
chemical titration. The reactions are studied under ambient conditions so no temperature
controllers are provided.
Glassware
Beaker (500 mL) 02
Conical flasks (250 mL) 02
Burette (50 mL) 01
Chemicals
Distilled Water 40L
NaOH Pellets 100 gm
0.1N HCl (for titration) 100 mL
Ethyl Acetate 200 mL
Phenolphthalein Indicator
Experimental Procedure
Pre-Preparation
Prepare 20L of 0.1N sodium hydroxide solution
Prepare 20L of 0.1N ethyl acetate solution
Prepare 100mL of 0.1N HCl and fill the burette
Precautions
Ensure all the valves of the setup are closed initially.
Ensure that the power supply from the panel is OFF before starting the reaction.
Precisely measure the volume/weight of the chemical used in the experiment.
Standardize the solution normality before using in the reaction.
Handle all the chemicals carefully ensuring personal and equipment safety.
Data Collection
Fill the reservoir feed tanks with the reactants, sodium hydroxide (tank A) and ethyl
acetate (tank B)
Connect the power supply to the set-up and switch ON
Start the pumps for each of the feed tank and wait for the flow from both of the over head
tanks.
Start the feed of the reactants to the reactor maintaining the equal flow rate of both the
reactants using the rotameters.
After about 10 min or time equal to the 4-5 space time (τ) of the reactor (whichever is
greater) withdraw 5mL of reaction mixture and titrate the sample against 0.1N HCl using
phenolphthalein as an indicator, endpoint from pink to colourless.
Experiment has to be performed at different flowrates of the feed.
Shut Down
Stop the flow of the reactants to the reactor and switch OFF the pumps regulating the flow.
Switch OFF the stirring of the reactor.
Drain the reactor and water bath and close the valves
Given Data
Observation Table
Calculations
Conversion, XA calculations
Plot XA / (1-XA) vs τ, get the value of slope to get the value of rate constant k
Get the values of rate constant k obtained for the reaction at different flowrate.