Beruflich Dokumente
Kultur Dokumente
FALL 2017-18
S. No LIST OF EXPERIMENTS
I BATCH REACTOR I
II BATCH REACTOR II
VI CSTR REACTOR
1
Expt No: Date:
AIM:
To verify the order and determine the rate constant for the reaction between
equimolar concentration of Sodium Hydroxide and Ethyl acetate in a constant volume batch
reactor.
APPARATUS:
CHEMICALS:
THEORY:
In the batch reactor the reactants are charged in to a container, well mixed and left to
react for a certain period. The resultant mixture is then discharged. This is an unsteady state
operation where in the concentration inside the reactor varies with time but uniform at any
instant of time.
Rate of loss of reactant A within the reactor due to chemical reaction = - rate of accumulation
of reactant A within the reactor
(-rA)V = -dNA/dt = NA0 dxA/dt
xa
therefore, t = NA0 dxA/(-rAV)
0
For a constant volume batch reactor,
Xa
t = CA0 dxA/(-rA)
0
2
Determination of order of reaction by the differential method of analysis
Let the rate equation be represented as -rA = k CAn where k is the reaction rate constant
and n is the order of reaction
ln(-rA) = ln k + n ln CA
The slope of the approximate linear plot of ln (-rA) vs ln CA gives the order of the
reaction n, the y-intercept gives ln k from which rate constant k can be calculated.
This is only an exercise for verification of order, though it is well known that the
order is 2 since this is an elementary reaction
dCA/CAn = -k dt
on integration, we get
CA1-n CA01-n = (n-1)kt
Substituting the value of n as two, k values are calculated for different values of CA.
The steady constant value of k proves that the order of reaction is verified and found to be
two
REACTION :.
PROCEDURE:
Take 250ml of NaOH and 250ml of CH3 COO C2 H5 of known concentrations CA0
and CBO (CA0 = CBO = 0.05N) in a conical flask and start mixing. The conical flask serves as
the batch reactor. Then 10ml of the reaction mixture is taken separately in each of eight
different conical flasks labeled 1 to 8. A reaction time of 5, 10, 15, 20, 25, 30, 40 and 50
minutes is given for each sample respectively. After the reaction time, the reaction is arrested
by adding excess Acetic acid solution of known concentration and volume (0.05N, 20 ml).
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The excess Acetic acid is estimated by titration against Sodium Hydroxide solution of known
concentration (0.05N) to determine the moles of unconverted Sodium Hydroxide in the
reaction mixture at the time of arresting the reaction. From this we can find out the
conversion XA at that instant.
OBSERVATION TABLE:
CALCULATIONS:
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Volume of acetic acid not used (V1 ml) = Volume of NaOH used in the back
Titration
Concentration of NaOH in the reaction mixture at the time of arresting the reaction
Initial concentration of NaOH in the reaction mixture = CAO = 0.05/2 = 0.025 mol/lit
The rate constant can also be determined from the linear plot of XA/(1-XA) Vs time t the
slope of which equal to KCAO from which we can determine the rate constant K by the
integral method of analysis with n equal to 2
RESULT:
For the saponification of ethyl acetate by Sodium hydroxide, the order of the reaction
is determined by the differential method of analysis and verified by the integral method of
analysis and found to be 2 and also the rate constant has been determined .
ANALYSIS REPORT:
Faculty Signature :
Date :
5
Expt No: Date:
AIM:
To determine the rate constant for the reaction between non-equimolar concentrations
of Sodium Hydroxide and Ethyl acetate in a constant volume batch reactor.
APPARATUS:
CHEMICALS:
THEORY:
In the batch reactor the reactants are charged in to a container, are well mixed and are
left to react for a certain period. The resultant mixture is then discharged. This is an unsteady
state operation where in the concentration inside the reactor varies with time but uniform at
any instant of time.
xA
t = CA0 dxA/(-rA)
0
Let the order of the reaction be 2
6
We use the integral method of analysis of data of reactants. For the second order
reaction of non-equimolar concentrations of A and B, A+B.> products,
REACTION :.
In the present experiment the following saponification reaction between Sodium
Hydroxide(NaOH) and ethyl Acetate (CH3 COO C2 H5 ) is studied.
PROCEDURE:
250ml of NaOH and 500ml of CH3 COO C2 H5 of known concentrations CA0 and CBO
(CA0 = CBO = 0.05N) are taken in to a conical flask and start mixing thoroughly. The conical
flask serves as the batch reactor. Then 10ml of he reaction mixture are taken separately in
each of the eight different conical flasks labeled 1 to 8. A reaction time of 5,10,15,20,25,30,
40 and 50 minutes is given for each sample respectively. After the reaction time, the reaction
is arrested by adding excess Acetic acid solution of known concentration and volume (0.05N,
20 ml). The excess Acetic acid is estimated by titration against Sodium Hydroxide solution
of known concentration (0.05N) to determine the moles of unconverted Sodium Hydroxide in
the reaction mixture at the time of arresting the reaction. From this we can find out the
conversion XA at that instant.
OBSERVATION TABLE:
7
CALCULATIONS:
Volume of acetic acid not used (V1 ml) = Volume of NaOH used in the back titration
Volume of acetic acid taken (Vo ml) = 20 ml
Volume of acetic acid used for arresting = (Vo V1) ml
Moles of acetic acid used = (Vo V1) * 0.05 * 10-3
= Moles of NaOH unused in the reaction
mixture at the time of arresting
Concentration of NaOH in the reaction mixture at the time of arresting the reaction (CA) =
Moles of NaOH unused / Volume of reaction mixture.
= [((Vo V1) * 0.05 * 10-3 / 10*10-3] mol/lit
Initial concentration of NaOH in the reaction mixture = CAO = 0.05/3 = Mol/lit
Conversion = XA = (CAO CA)/CAO
M= CB0/CA0 =2
GRAPH:
The plot of [(M-XA)/M(1-XA)] Vs time t gives a straight line of slope equal to KC AO (M-
1) from which we can determine the rate constant K.
Related Exercise: (i) Derive rate equation for non Equimolar system for elementary second
order reaction, (ii) analysis the result by doing the experiments with one reactant as excess.
RESULT:
For the saponification of ethyl acetate by Sodium hydroxide, the rate constant has
been determined and found to be
8
Faculty Signature:
Date :
Expt No: Date:
AIM:
To study the performance of semi batch reactor for the second order reaction of
saponification of ethyl acetate by sodium hydroxide
APPARATUS:
Conical flasks
Burette
Pipette
Stop watch
CHEMICALS:
Ethyl acetate
Sodium hydroxide
Acetic acid
Phenolphthalein indicator
THEORY:
There are two basic types of Semi batch reactors. In the first type, one of the
reactants is slowly fed to a rector containing the other reactant, which has already been
charged to the reactor. This type of reactor is used when unwanted side reactions occur at
high concentrations of A or the reaction is highly exothermic. In the second type, both the
reactants are fed to a reactor at constant flow rates. In the present case, we are studying the
performance of semi batch reactor of first type.
The performance equation of the semi batch reactor is same as that of constant
volume batch reactor with time t being replaced by t.
Over the total reaction time of t minutes, the semi batch reactor is treated as a series
of N (=t/t) constant volume batch reactors.
PROCEDURE:
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of known concentration (0.05N) at a constant known flow rate for a known reaction or
operation time of t minutes (say 30 minutes, the total volume of the reaction mixture must
increase to about 100ml). Take a sample of 20ml of reaction mixture into another conical
flask and arrest the reaction by adding excess acetic acid of known concentration and volume
(0.05N, 20ml). The quantity of acetic acid in excess is determined by titration against
standard NaOH solution. This gives the quantity of unreacted NaOH left in the reactor at the
time of arresting the reaction (at the reaction time t ) from which we can determine the
conversion of NaOH in the semi batch reactor. We can also determine the conversion
theoretically from the batch reactor performance equation by approximating the semi batch
reactor as a series of N batch reactors. Refer any chemical reaction engineering book for
derivation.
Xa =
OBSERVATIONS:
MODEL CALCULATIONS:
Moles of acetic acid left in the analysis sample after arresting the reaction
= Moles of NaOH consumed in the back titration
= X * 10-3*0.05
Moles of acetic acid used to neutralize NaOH to completely arrest the reaction
= 20*10-3*0.05 X* 10-3*0.05
Moles of Na OH left at the end of reaction time in 20ml analysis sample
= 0.05* (20-X) * 10-3
Volume of reaction mixture in the reactor = (50 + QB * t) ml
Therefore, moles of Na OH left in the reactor at the end of reaction time
= [(50 + QB *t) / 20] * 0.05 * (20-X) * 10-3
Moles of Na OH initially taken in the reactor = 50 * 0.05 * 10-3 = NAO
Experimental value of conversion = XA exp = (NAO-NA)/NAO
THEORETICAL CALCULATIONS:
10
For equimolar concentrations, for a second order reaction by the integral method of
analysis
XA/(1-xA) = kCA0 t k can be calculated by substituting the values of x A, CA0,
t(=30min)
N= 2
NB02 =NB1+ Ethyl acetate added in the second interval
=(NB1 + t * QB * 10-3 * 0.05) moles
NA02 = NA1 moles
Volume of the reaction mixture = V2 =(50+2 * t * QB ) ml
CB02 =Nbo2/V2
CA02 =NA02/V2
M2 = CB02/ CA02
K CA 02 (M2-1) * t = In [ ( M2 XA2 )/M2 (1-XA2)]
the same k value can be substituted from which xA2 can be calculated
Faculty Signature:
11 Date :
Expt No: Date:
AIM:
To study the reaction rate under adiabatic condition for hydrogen peroxide and sodium
thiosulfate reaction.
APPARATUS:
THEORY :
The effect on the temperature of the reaction mixture consisting of H2O2 and Na2S2O3
when the reaction is carried out adiabatically can be observed and correlated with the rate of
the reaction. As the reaction is exothermic, temperature increases as the reaction proceeds
and becomes constant when reaction is completed. The rate of the reaction and temperature
for the reaction is correlated to various parameters as
1/(TF T)2 dT/dt = KOCAO e-E / RT / (TF TO)
where,
EXPERIMENTAL SETUP :
The apparatus consists of an insulated Dewar vessel (Thermo flask ) fitted with a two
holed rubber cork carrying a long mercury thermometer (0-10000C) through one hole and a
glass funnel with a valve in the other. A stopwatch is used to record the time at various
intervals and the temperature is noted.
PROCEDURE :
Prepare solutions of Na2S2O3 and H2O2 each of 0.10(or) 0.05N concentration. Transfer
exactly 200ml of Na2S2O3 solution into the reactor and note its temperature. Transfer exactly
200ml of H2O2 solution. Mix the contents well and after attaining the maximum steady
temperature and record the temperature at regular intervals of time until the maximum
temperature is reached.
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OBSERVATIONS and CALCULATIONS
60
90
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150
180
210
240
270
300
330
360
390
420
450
480
510
540
570
600
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630
660
690
720
750
GRAPH :
A plot of T vs t is made . various dT/dt values are calculated. Then plot a graph between
1/T Vs In [1/(TF-T)2 dT/dt]. From the Slope and intercept, we can calculate the activation
energy (E) and frequency factor (K0)
RESULT :
Faculty Signature:
Date :
14
Expt No: Date:
AIM :
To establish the nature of temperature dependency of the reaction rate constant for the
saponification reaction of ethyl acetate with Na OH solution.
APPARATUS ;
CHEMICALS:
Ethyl acetate
Sodium hydroxide
Acetic acid
Phenolphthalein indicator
THEORY:
K = ko exp (-E/RT)
Where ko is called frequency factor and E is called the activation energy of the reaction. This
expression fits experiment well over wide temperature ranges and is strongly suggested from
various stand points as being a very good approximation to the true temperature dependency.
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REACTION:
PROCEDURE:
Place 400ml 0.05N NaOH solution in a 1000ml conical flask which as a reactor.
Transfer 20ml of Acetic acid solution into each of Eight 250ml conical flasks which are
serially labeled. Place the reactor on a hot plate cum magnetic stirrer and start heating by
stirring the contents uniformly till the desired temperature is obtained. Carefully transfer
200ml of 0.05N ethyl acetate into the reactor & start the stopwatch simultaneously. At the
time intervals of 10 minutes, pepett out 20 ml of the reaction mixture, into each of the conical
flask. The Acetic Acid already present in the analysis flask neutralizes the alkali in the
sample reaction mixture and arrests the saponification reaction. Back Titrate these reaction
sample mixtures with aqueous NaOH solution using phenolphthalein as indicator. Note down
the room temperature and conduct the experiment at various temperatures (minimum two
temperatures.)
OBSERVATION
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MODEL CALCULATIONS: ( For temp T1)
M= CB0/ CA0
Repeat the above procedure at the other two temperatures also and the corresponding
k values are noted against the corresponding temperatures.
TABULATION
T1 T2 T3
t (mins) XA In [(M-XA)/M(1- XA In [(M-XA)/M(1- XA In [(M-XA)/M(1-
XA)] XA XA)]
1
2
3
4
5
6
7
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8
9
10
S.No T 1/T K In K
1 T1 K1
2 T2 K2
3 T3 K3
GRAPH:
Plot a graph of ln k vs 1/T, rate constant k and frequency factor k0 can be calculated
from slope and y-intercept respectively
RESULT:
Faculty Signature:
18 Date :
Expt No: Date:
AIM :
To study the performance of a Mixed Flow Reactor for carrying out a second order
reaction of saponification of ethyl acetate by NaOH
CHEMICALS :
THEORY :
In mixed flow reactor, properties of the reaction mixture are uniform
throughout the volume. With equimolar concentration of reactants at inlet for this second
order reaction, the outlet concentration of reactants also remain equimolar.
A straight line plot is approximated from the plot of xA/(1-xA)2 vs t , the slope of which gives
k CA0 from which the rate constant k can be calculated
REACTION
EXPERIMENTAL SETUP
Its consists of a cylindrical container with flow connections for inlet and outlet
sections. The constant inflow of reactants can be maintained by rotameters.
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PROCEDURE
Sodium hydroxide and ethyl acetate solutions of known concentrations (CAO = CBO
= 0.05 N ) are allowed to enter at constant flow rates in the mixed flow reactor. Sufficient
time is given for system to attain steady state conditions.. Now product is collected and the
reaction is arrested by adding excess acetic acid(20ml, 0.05N). After mixing thoroughly,
ttitration with standard NaOH is done taking 10ml of mixture.
OBSERVATIONS:
GRAPH :
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These are compared with those of the experimental values.
RESULT :
For the given reaction, the conversion is calculated experimentally and compared
with theoretical values as well as with graphical technique.
Faculty Signature:
Date :
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