CHE348 SP25 Wk6 Lab
CHE348 SP25 Wk6 Lab
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Lab Objectives
● CSTR components
● CSTR background
● Factors affecting rate of reaction
● Experiment objectives
● Core theory
● Chemical reaction
● Reaction Rate
● Reactant preparation process
● Reactor Inlet and outlet
● Reaction monitoring
● Experimental procedure
● Results and discussion (table for parameters, equations and plots)
● MSDS
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CSTR Components
Lab View
Industrial View
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CSTR Components Cont.
Reactor vessel and its components with the hot water connections, coil, sensors, glands, stirrer, and valves.
Can you notice the differences between CSTR and batch reactors?
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CSTR Components Cont.
❑ A stainless steel coil inside the reactor provides the heat transfer
surface for either heating or cooling the chemical reactants.
❑ The coil is connected either to the hot water circulator or the optional
chiller. The coil inlet is at the front of the reactor and the coil return is at
the rear of the reactor.
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CSTR Components Cont.
Student exercise: Explain the following PID
Question box
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Reactor Inlet and Outlet
● The two feed pumps on the service unit
pump the chemical reagents from the two
feed bottles into the reactor separately
through connectors in the base of the
reactor.
In order for the fluid to pumped into the reactor, should the pumps
work in a clockwise or anti clockwise motion, explain?
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Background
❑ A continuous stirred tank reactor (CSTR) is a reactor equipped with an impeller or other mixing device to
provide efficient mixing.
❑ In chemical engineering the name CSTR is often used to refer to an idealised agitated tank reactor used to
model operation variables required to attain a specified output.
❑ In flow chemistry, a continuous stirred tank reactor (CSTR) equipped with features to continuously feed and
exhaust reactants is an example of a mechanically mixed flow reactor
❑ The continuous stirred tank reactor in the form of either a single tank or (more often) tanks in series, is used
widely and is particularly suitable for liquid phase reactions. Agitation is used to maintain homogeneity and
to improve heat transfer.
❑ It is particularly used in the organic chemicals, oil and gas & water treatment industry.
❑ Advantages of using CSTR include consistent product quality, straightforward automatic control and low
manpower requirements.
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Comparing a CSTR to a Batch Reactor
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Factors Affecting Reaction Rate
● 1. Reactant concentration
● 2. Physical state of the reactants and surface area
● 3. Presence of catalyst
● 4. Temperature
● 5. Stirring
What are the factors affecting the reaction rate of the batch reactor?
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Experiment objectives
● The CSTR experiment studies the reaction of saponification of Ethyl Acetate in a CSTR reactor,
in which the student has to:
❑ Find the reaction rate constant in a CSTR.
❑ Determine the reaction rate in steady and unsteady states.
❑ Determine the steady state region in the operation of a CSTR.
❑ Calculate the values of sodium hydroxide concentration (𝑎1 ) and sodium acetate concentration (𝑐1 ) and the degree of conversion
(𝑋𝑎 ) and (𝑋𝑐 ) for each of the samples of conductivity taken over the period of the experiment.
❑ Determine the time required for the reaction to reach completion.
● Volume of reactor, feed rate, rate of agitation and baffle implementation are factors studied relative to the experiment
carried out.
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Core Theory
Having recorded the conductivity of the contents of the reactor over the period of the reaction, the
conductivity measurements must now be translated into degree of conversion of the constituents.
Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution whilst ethyl
acetate and ethyl alcohol do not.
The conductivity of a sodium hydroxide solution at a given concentration and temperature, however, is
not the same as that of a sodium acetate solution at the same molarity and temperature and a
relationship has been established allowing conversion to be inferred from conductivity.
The calculations are best carried out using a spreadsheet such as EXCEL so that the results can be
displayed in tabular and graphical form.
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Electrical Conductivity and Saponification
● Conductivity: Conductivity of a substance is defined as 'the ability or power to conduct or transmit heat,
electricity, or sound'. Its units are Siemens per meter [S/m] in SI and millimhos per centimetre [mmho/cm] in
U.S. customary units. Its symbol is k or s.
● Electrical Conductivity: Electrical conductivity is a measure of how well electrical current (charge in
motion) can pass through a material under the influence of an applied voltage/electric field. Thermal
conductivity measures how well heat (thermal energy in motion) can pass through a material under a
temperature differential.
● Saponification: Saponification can be defined as a “hydration reaction where free hydroxide breaks the
ester bonds between the fatty acids and glycerol of a triglyceride, resulting in free fatty acids and glycerol,”
which are each soluble in aqueous solutions.
OR
Saponification is a process that involves the conversion of fat, oil, or lipid, into soap and alcohol by the action of
heat in the presence of aqueous alkali (e.g. NaOH). Soaps are salts of fatty acids and fatty acids are monomers
of lipids that have long carbon chains (at least 10) e.g. sodium palmitate. Saponification reactions are generally
exothermic and almost totally irreversible.
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Chemical Reaction
● The reaction chosen for the isothermal demonstration is the saponification of ethyl acetate by sodium
hydroxide. The use of indicators allows following the reaction by changing the color as the reaction takes
place.
● The saponification reaction of ethyl acetate by sodium hydroxide, is a 2nd order reaction overall, and 1st
order reaction with respect to each reactant.
NaOH + CH3COOC2H5 → CH3COONa + C2H5OH
Sodium Hydroxide + Ethyl Acetate Sodium + Ethanol
(a) (b) Acetate (d)
+ Crystal Violet (c)
(The end products of saponification reaction (i. e., sodium acetate and ethanol) are used in various fields–for
instance, the petroleum, textile, cosmetics, and paint industries.)
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Rate of Reaction
● In homogenous reaction systems, reaction rates depend on the concentration of the
reactants.
● r = k. [a]n. [b]m
● Where:
○ r = reaction rate
○ k = rate constant
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Reaction Kinetics
To calculate the specific rate constant, k:
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Reactant Preparation Process
● The experiment uses a 0.1M solution of Ethyl Acetate in the CSTR. This should be made by
diluting concentrated Ethyl Acetate.
● Note: The practice of making a strong solution (e.g. 1M) then further diluting this to the required
concentration (e.g. 0.1M) cannot be applied when using Ethyl Acetate. The required dilution
should be made directly as stated above.
● To get the colorful solution, Crystal Violet should be added to the Ethyl Acetate to make up a final
solution of 10−5 M of crystal violet when both reagents are mixed.
● The other reactant is a 0.1M solution of Sodium Hydroxide. This may be made by dilution of a
strong solution, or dissolution of sodium hydroxide pellets in water.
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Experimental Procedure
Check the Manual
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Reaction Monitoring
1. By conductivity probe as the conductivity of the solution changes with conversion of the reactants to product
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Results and Discussion
Parameter Value Note
𝑭𝒂
𝑭𝐛
𝒂𝛍
Known experimental values /
𝒃𝛍
constants
𝒄𝛍
T
V
𝒂𝟎 concentrations in the mixed feed of
𝒃𝟎 NaOH and Ethyl acetate respectively
Λ𝑜 − Λ𝑡
𝑐1 = 𝑐∞
Λ𝑜 − Λ∞
𝑎0 − 𝑎1
𝑋𝑎 =
𝑎0
𝑐1
𝑋𝑐 =
𝑐∞
Please check experiment manual for additional equations.
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Results And Discussion cont.
● Plot the concentration of NaOH (𝑎1 ) against time t.
● Plot the conversion of NaOH (𝑋𝑎 ) against time t. Show the steady-state period on the graph.
● Plot the concentration of CH3COONa (c1) against time.
● Plot the conversion of CH3COONA (𝑋𝑐 ) against time t. Show the steady-state period on the
graph.
● The value of the reaction rate constant calculated from a batch experiment was different than the
one found using a CSTR. Explain this difference and tell which one is the most reliable.
● Plot a chart of reaction rate ‘r’ vs. time t.
● Can you tell when the beginning of the steady state regime was?
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Nomenclature
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Material Safety Data Sheet (MSDS)
Crystal Violet
Precautions:
▪ Keep away from heat.
▪ Keep away from sources of ignition.
▪ Do not ingest.
▪ Do not breathe dust.
▪ Wear suitable protective clothing
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Additional Information
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