You are on page 1of 19

EXPERIMENT NO-

Date:

REACTION KINETIC STUDIES IN A BATCH REACTOR


AIM:

Conduct a simulation experiment and determine the rate constant for the
saponification of ethyl acetate (A) with NaOH (B) in a batch reactor at a
specified temperature.

APPARATUS:

Conductivity meter, Measuring cylinders, stop watch, etc.

CHEMICALS:

Ethyl acetate, NaOH, Water, etc.

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mixture of unreacted material together with the products is withdrawn.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.
Bacth reactors are simple and needs little supporting equipment, and is therefore
ideal for small scale experimental studies on reaction kinetics. Industrially it is
used when relatively small amounts of material are to 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.

Chemical Reaction Engineering (CRE-I)

Page

PROCEDURE: 1. Standardize the NaOH stock solution and note down its concentration. Note
down the strength of ethyl acetate stock solution.
2. Calculate the volume of NaOH(VB) and ethyl acetate(VA) (required to make
the required initial concentration ratio of M (a value equal to or greater than
1) and total reactor volume (select the required volume batch reaction
vessel). Choose initial molar ratio of B to A (M) to be taken. Choose stock
concentration of A and the stock concentration of B. Chose the reaction
temperature. Now calculate the volume of stock solutions of B and A to be
taken so as to maintain the chosen M and the total volume of the reactor.
VA +VB = VT .. (1)
VT is the total reactor volume
M = (CBS*VB)/(CAS*VA) = moles of B/ moles of A
VB/VA = .. .(2)
From Eq (1) and (2) , VA =......mL , VB=......mL
Where VA and VB are the the volumes of ethyl acetate and NaOH.
Cas and Cbs are the concentrations of stock solutions of A and B.
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. Pump the
water from heating tank for circulation in the jacket. 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.
Note: Some conductivity meters may display conductance (mS) not the
conductivity(mS/cm) [ Refer theory for more information].
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
Chemical Reaction Engineering (CRE-I)

Page

using the conductivity meter calibration equation. Since the conductivity


meter calibration at 28C is only provided, calculate the conductivity meter
reading at the required temperature using the temperature compensation
equation provided.
9. Repeat the experiment at different temperatures.

Chemical Reaction Engineering (CRE-I)

Page

OBSRVATIONS:
A= Ethyl acetate
B= NaOH
1. Strength of Ethyl acetate in stock = 0.02 gmol/L
2. Strength of NaOH in stock solution= 0.02 gmol/L
3. V = volume of the reactor = 1000 cm3
4. Reaction temperature= 30 C
5. Initial concentration of A in the reaction mixture, CA0= 0.01 gmol/L
6. Initial concentration of B in the reaction mixture, CB0= 0.01 gmol/L

Chemical Reaction Engineering (CRE-I)

Page

CALCULATIONS:

Chemical Reaction Engineering (CRE-I)

Page

RESULT:
1. The rate constant for the saponification of ethyl acetate with NaOH at a temperature of
.. C is, k = . min-1(L/gmol)

CONCLUSION:

Chemical Reaction Engineering (CRE-I)

Page

EXPERIMENT NO-

Date:

REACTION KINETIC STUDIES IN A MIXED FLOW REACTOR


AIM:

Conduct simulation based experiments to determine the rate constant for


the saponification of ethyl acetate with NaOH at different temperatures
using a mixed flow reactor (continuous stirred tank reactor).

APPARATUS:

Conductivity meter, Measuring cylinders, stop watch, etc.

CHEMICALS:

Ethyl acetate, NaOH, Water, etc.

THEORY:

Flow Reactors: There are two types of flow reactors in common use in the
chemical industry. They are the continuous stirred tank reactor (CSTR)
and the tubular reactors. CSTR or Mixed flow reactor(MFR) is
configured much like a batch reactor except reactants and products
continuously flow in and out of the reactor. Steady state flow reactors are
ideal for industrial purposes when large quantities of material are to be
processed and when the rate of reaction is fairly high to extremely high.
Flow reactors need more supporting equipment like pumps. But good
product quality can be obtained.

PROCEDURE:

1. Standardize the NaOH stock solution and note down its concentration.
2. Calculate the concentration of ethyl acetate in stock solution
3. Fill the reservoirs with NaOH and ethyl acetate stock solutions
4. Measure the volume of the reactor.
5. Switch on the pump and allow ethyl acetate to flow into the reactor at
certain flowrate and measure the flowrate using rotameter.
6. Set the required temperature to be maintained in the reactor. Switch
on the heater to heat the reactor contents to the required temperature.
7. Calculate the flowrate of NaOH required to keep the desired value of
M may be greater than or equal to one. Calculate the total flowrate
(Q).
8. Adjust the flowrate of NaOH to the calculated value, without
changing the EA flowrate.
9. Calculate the actual value of M obtained after adjusting the flowrates.
10. Calculate the space time using the total flow rate.

Chemical Reaction Engineering (CRE-I)

Page

11. Start the stirrer in the reactor. Close the drain valve completely. Allow
the reaction to proceed till steady state is attained, as indicated by
constant reading in the conductivity meter.
12. Note down the conductivity (in mS/cm) of the reaction mixture in,
after steady state is attained. Note: Some conductivity meters may
display conductance (mS) not the conductivity(mS/cm) [Refer theory
for more information].
13. Determine the concentration of unreacted NaOH in the reaction
mixture by using the conductivity meter calibration equation.
14. Repeat steps (6) to (12) for different EA flowrates.
15. Conduct the experiment at different temperatures

Chemical Reaction Engineering (CRE-I)

Page

OBSRVATIONS:
A= Ethyl acetate
B= NaOH
1. Strength of Ethyl acetate in stock = 0.02 gmol/L
2. Strength of NaOH in stock solution= 0.02 gmol/L
3. V = volume of the reactor = 5 L
4. Reaction temperature= 30 C

Chemical Reaction Engineering (CRE-I)

Page

CALCULATIONS:

Chemical Reaction Engineering (CRE-I)

Page

Chemical Reaction Engineering (CRE-I)

Page

RESULTS:
1. The rate constant for the saponification of ethyl acetate with NaOH at a temperature
of .. C is, k = . min-1(L/gmol)
CONCLUSION:

Chemical Reaction Engineering (CRE-I)

Page

EXPERIMENT NO-

Date:

REACTION KINETIC STUDIES IN A PLUG FLOW REACTOR

AIM:

To determine the rate constant for the saponification of ethyl acetate with
NaOH at ambient temperature of 280C using a Plug flow reactor.

APPARATUS:

Conductivity meter, Measuring cylinders, stop watch, etc.

CHEMICALS:

Ethyl acetate, NaOH, Water, etc.

THEORY:

Tubular reactors are one category of flow reactors. This reactor has
continuous inflow and outflow of material. In the tubular reactor, the feed
enters at one end of a cylindrical tube and the product stream leaves at the
other end. The long tube and the lack of provision for stirring prevents
complete mixing of the fluid in the tube. Hence the properties of the
flowing stream will vary from one point to another, namely in both radial
and axial directions.
Ideal tubular reactor is referred as a plug flow reactor(PFR). The key
assumption is that as a plug flows through a tubular reactor, the fluid is
perfectly mixed in the radial direction but not in the axial direction
(forwards or backwards). Each plug of differential volume is considered as
a separate entity, effectively an infinitesimally small batch reactor, limiting
to zero volume. As it flows down the tubular PFR, the residence time () of
the plug is a function of its position in the reactor. In the ideal PFR, the
residence time distribution is therefore a Dirac delta function (small and
tall) with a value equal to . The PFR model works well for many fluids:
liquids, gases, and slurries. An ideal plug flow reactor has a fixed residence
time: Any fluid (plug) that enters the reactor at time t will exit the reactor at
time t +, where is the residence time of the reactor.
Residence time in the reactor is equal to the space time if the conditions in
the reactor like pressure and temperature are same as those at the entrance.
In the ideal tubular reactor, which is called the plug flow reactor, specific
assumptions are made about the extent of mixing:
1. no mixing in the axial direction, i.e., the direction of flow

Chemical Reaction Engineering (CRE-I)

Page

2. complete mixing in the radial direction


3. a uniform velocity profile across the radius.
The absence of longitudinal mixing is the special characteristics of this type
of reactor. It is an assumption at the opposite extreme from the complete
mixing assumption of the ideal stirred tank reactor. The validity of the
assumptions will depend on the geometry of the reactor and the flow
conditions. Deviations, which are frequent but not always important, are of
two kinds:
1. mixing in longitudinal direction due to vortices and turbulence
2. incomplete mixing in radial direction in laminar flow conditions

PROCEDURE:

1. Note down the concentration of ethyl acetate(EA) and NaOH in stock


solution
2. Fill the reservoirs with NaOH and ethyl acetate stock solution
3. Calculate the volume of the tubular reactor.
4. Switch on the pump and allow ethyl acetate to flow into the reactor at
certain flowrate and measure the flowrate(vA) using rotameter.
5. Set the required temperature to be maintained in the reactor.Switch on
the heater to heat the reactor contents to the required temperature .
6. Calculate the flowrate of NaOH required to keep the desired value of M
may be greater than or equal to one. Calculate the total flowrate (Q).
7. Adjust the flowrate of NaOH to the calculated value, without changing
the EA flowrate.
8. Calculate the actual value of M obtained after adjusting the flowrates.
9. Calculate the space time using the total flow rate.
10. Start the stirrer in the reactor. Close the drain valve completely. Allow
the reaction to proceed till steady state is attained, as indicated by
constant reading in the conductivity meter.
11. Note down the conductivity (in mS/cm) of the reaction mixture in, after
steady state is attained. Note: Some conductivity meters may display
conductance (mS) not the conductivity(mS/cm).

Chemical Reaction Engineering (CRE-I)

Page

12. Determine the concentration of unreacted NaOH in the reaction mixture


by using the conductivity meter calibration equation.
13. Repeat steps (6) to (12) for different EA flowrates.
14. Conduct the experiment at different temperatures.

Chemical Reaction Engineering (CRE-I)

Page

OBSERVATION:
A= Ethyl acetate
B= NaOH
1. Diameter of reactor coil= 0.33 m
2. No. of turns in the coil= 5
3. Diameter of reactor= 0.011 m
4. Strength of Ethyl acetate in stock = 0.02 gmol/L
5. Strength of NaOH in stock solution= 0.02 gmol/L
6. V = volume of the reactor = 0.4926 L
7. Reaction temperature= 30 C

Chemical Reaction Engineering (CRE-I)

Page

CALCULATION:

Chemical Reaction Engineering (CRE-I)

Page

Chemical Reaction Engineering (CRE-I)

Page

RESULTS:
2. The rate constant for the saponification of ethyl acetate with NaOH at a temperature of
.. C is, k = . min-1(L/gmol)
CONCLUSION:

Chemical Reaction Engineering (CRE-I)

Page

You might also like