Cre Lab
Cre Lab
TECHNOLOGY
(An Autonomous Institution, Approved by AICTE, New Delhi, Affiliated to Anna University, Chennai,)
LABORATORY MANUAL
REGISTER NO :
Course Outcomes (COs):
Upon successful completion of this course, the student will be able to:
PO5 Modern tool usage Create, select, and apply appropriate techniques, resources,
and modern engineering and IT tools including prediction and
modeling to complex engineering activities with an understanding
of the limitations.
PO6 The engineer and Apply reasoning informed by the contextual knowledge to assess
society societal, health, safety, legal and cultural issues and the consequent
responsibilities relevant to the professional engineering practice
Understand the impact of the professional engineering solutions in
PO7 Environment and societal and environmental contexts, and demonstrate the
sustainability knowledge of, and need for sustainable development.
PEO 1: Participate as leaders in their fields of expertise and in activities that support service
and economic development nationally and throughout the world.
PEO 2: Pursue continued life-long learning through professional practice, research and training
programs in the field of chemical engineering and science.
PEO 3: Solve real-life problems in a broad perspective to fulfill ethical, economic,
environmental and social responsibilities.
CHEMICAL REACTION ENGINEERING LABORATORY
CONTENTS
Sl. Date of
Date Particulars Signature
No. submission
5
EXP NO.
DATE:
Aim
To determine the rate constant and the kinetics for saponification of equimolar quantity of ethyl acetate and
sodium hydroxide in a continuous stirred tank reactor.
Apparatus required
Pipette
Burette
Standard measuring jar-250ml beaker
Conical flask
Stop watch
MFR setup.
Chemicals required
Sodium hydroxide (NaOH) Ethyl acetate
(CH3COOC2H5)Acetic acid (CH3COOH)
Water (H2O)
Hydrochloric acid (Hcl) Phenolphthalein
indicator
Theory
A mixed flow reactor or a CSTR is operated at steady state. There is no accumulation. The total mass
flow rate at which the reactants are fed to the reactor is equal to the mass flow rate at which the products
are withdrawn from the reactor. Therefore, the properties in the CSTR do not change with time. The
concentration of reactants drops to the outlet concentration immediately on entering the CSTR. The
concentration of the material does not vary with time. Since the reactor is well mixed, the concentration
throughout the reactors is uniform i.e. there is no spacial variation in concentration in the reactors at any
time. Thus the rate of reaction in a CSTR is constant throughout the reactor at fixed temperature. Since
there is a concentration gradient along the reactor. In flow reactor, space time and residence time
are important parameter. The residence time can be varied either by varying the flow rate and keeping
the volume of reactor constant (or) vice-versa.
As the residence time decreases, the conversion decreases for liquid phase reaction i.e. for reaction
with constant density. The space time which is the time required to process one reactor volume of fluid
is equal to the mean residence time.
The reaction between sodium hydroxide and ethyl acetate can be represented as,
NaOH + CH3COOC2H5 CH3COONa + C2H5OH
𝐶𝐴0
𝑀= = 1 (𝑓𝑜𝑟 𝐸𝑞𝑢𝑖𝑚𝑜𝑙𝑎𝑟)
𝐶𝐵0
TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)
Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:
Volume of
Volume of
Volumetric Volumetric Volume of Volume of Hcl not
Hcl used to
flow rate of flow rate of reaction Hcl added in used to
S.NO arrest the
NaOH ethyl acetate mixture the conical arrest the
reaction
(LPM) (LPM) collected (ml) flask (V0, ml) reaction
(V6, ml)
(V4, ml)
TABULATION IV:
Titre value of
Space time,
NaOH, CA, (mole/lit) XA (no unit) XA/ (1- XA) XA/ (1- XA)2
(Ʈ, sec)
(V5, ml)
CALCULATION:
Initial concentration of NaOH, CA0 = (N2 X Vol. flow rate of NaOH) / Total vol. flow rate
CA0 =
Initial concentration of EA, CB0 = (N4 X Vol. flow rate of EA) / Total vol. flow rate
CB0 =
V4 = ___ _ _
XA =
Ʈ =
Ʈ = ___ _ _ _.
To determine the rate constant and kinetis for saponification of equimolar quantity of ethyl acetate
andsodium hydroxide in a CSTR
Apparatus Required:
Cascade CSTR setup (series)
Conical flask
Beaker
Standard measuring flask
Measuring jar
Stop watch
Chemicals Required:
Sodium hydroxide (NaOH)
Ethyl acetate (CH3COOC2H5)
Acetic acid (CH3COOH)
Water (H2O)
Hydrochloric acid (Hcl)
Phenolphthalein indicator
Theory:
Consider a system of mixed flow reactor (or) CSTR connected in series. Though the concentration is
uniform ineach reactor, there is, nevertheless a change in concentration as the fluid moves from reactor to
reactor. This stepwise drop in the concentration suggests that the large, the number of units in series, the
closer should be the behaviour of the system, approaches plug flow. The reaction between sodium hydroxide
and ethyl acetate is represented by the stoichiometry as follows:
TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)
Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:
TABULATION IV:
Titre value of
Space time,
NaOH, CA, (mole/lit) XA (no unit) XA/ (1- XA) XA/ (1- XA)2
(Ʈ, sec)
(V5, ml)
TABULATION V:
Volume of
Volume of Volume of Hcl
Volumetric Volumetric Volume of Hcl Hcl used
reaction not used to
flow rate of flow rate of added in the to arrest
Reactor mixture arrest the
NaOH ethyl acetate conical flask the
collected reaction
(LPM) (LPM) (V0, ml) reaction
(ml) (V4, ml)
(V6, ml)
TABULATION VI:
Titre value of
Space time,
NaOH, CA, (mole/lit) XA (no unit) XA/ (1- XA) XA/ (1- XA)2
(Ʈ, sec)
(V5, ml)
CALCULATION:
Initial concentration of NaOH, CA0 = (N2 X Vol. flow rate of NaOH) / Total vol. flow rate
CA0 =
Initial concentration of EA, CB0 = (N4 X Vol. flow rate of EA) / Total vol. flow rate
CB0 =
V4 = ___ _ _
V = πr2L
V = ___ _ __
Ʈ = ___________ _.
The PFR is operated at steady state i.e. the conditions in the plug flow reactor do not vary with time.
The steady state flow condition means that the total mass
flow rate at which the reactants are fed to the reactor is equal to the total mass flow rate of the products
withdrawn from the reactors. There is no accumulation in the plug flow reactor. The concentration varies
in the axial direction. Therefore there is a concentration gradient along the axial direction (there is no
mixing along axial direction) but there may be mixing in the radial direction. Therefore a plug flow
reactor is otherwise called as an ideal tubular reactor.
The reaction between sodium hydroxide and ethyl acetate can be represented as,
Procedure:
1. The solution of sodium hydroxide, hydrochloric acid, acetic acid and ethylacetate of
required strength are prepared.
2. Sodium hydroxide and hydrochloric acid solutions are standardized.
3. The storage reservoirs were filled with --------- lit of sodium hydroxide and
------------- lit of ethyl acetate solution.
4. The required flow rates of sodium hydroxide and ethyl acetate were adjusted using rotameter
such that the flow rate of both sodium hydroxide and ethyl acetate were different (for feeding
on non equimolar quantity of sodium hydroxide and ethyl acetate).
5. Steady state conditions were allowed to be obtained. i.e. outlet flow rate is equal to inlet flow
rate.
6. 20ml of product was collected from CSTR and transferred into the flask containing 20 ml
of standardized hydrochloric acid for arresting the reaction.
7. This solution was mixed thoroughly and titrated against standardized NaOH.
8. 20ml of product was collected from PFR and transferred into the flask containing 20 ml of
standardized hydrochloric acid for arresting the reaction
9. This solution was mixed thoroughly and titrated against standardized NaOH.
10. The titrate value was repeated for different flow rate and result were tabulated.
OBSERVATION:
Normality of ethyl acetate, N4 = 0.1N
Normality of acetic acid, N1 = 0.1N
Diameter of reactor, d = cm
Length of reactor, L = cm
TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)
Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:
S.No Inter
MFR+ MFR+ MFR+ Over
NaOH EA MFR MFR MFR media
PFR PFR PFR all
te
CALCULATION:
MFR: PFR:
Diameter of MFR = Diameter of PFR =
Length of MFR = Length of PFR =
Volume of reactor = πr2L Volume of reactor = πr2L
= =
Concentration of NaOH in the feed stream, CA0 = (StrengthxFlow rate of NaOH)/ Total flow
rateCA0 =
Concentration of EA in the feed stream, CB0 = (StrengthxFlow rate of EA)/ Total flow rate
CB0 =
CA, Intermediate = [(NHcl x VHcl) – (NNaOH x VNaOH)]MFR / Total vol of sample in the conical
flaskCA, Intermediate =
CA, Overall = [(NHcl x VHcl) – (NNaOH x VNaOH)]MFR + PFR / Total vol of sample in the conical flask
CA, Overall =
CA, Overall =
Overall conversion, XA =
XA =
RESULT:
The conversion for the combined system of MFR-PFR is studied for different flow rates
and the results are given as follows:
To determine the effect of temperature on the reaction rate constant, k and determine the
activation energy E for the saponification reaction.
Apparatus Required:
MFR setup
Conical flask
Beaker
Standard measuring flask
Measuring jar
Stop watch
Heater
Chemicals Required:
Sodium hydroxide (NaOH)
Ethyl acetate (CH3COOC2H5)
Acetic acid (CH3COOH)
Water (H2O)
Hydrochloric acid (Hcl)
Phenolphthalein indicator
Theory:
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 not in the radial direction. V is the volume of the reactor, Vo is the volumetric feed rate,
CAo is the feed conc. of A, x is the degree of conversion. In case of a Coil, turbulence is introduced due
to frequent change in direction of flow and presence of secondary flow. So a higher value of k is expected
in case of a coil type PFR. For steady state rate operation of a PFR: In case of a Coil, turbulence is
introduced due to frequent change in direction of flow and presence of secondary flow. So a higher value
of k is expected in case of a coil type PFR.
Procedure:
1. Fill the tanks with sodium hydroxide and ethyl acetate solution.
2. Fill the water bath with water.
3. Start the heater and stirrer of the bath.
4. Using rotameter set the different flow rate for both the solution i.e. CA0 not equal to CB0
5. After steady state is achieved, collect 20 ml of the sample of the liquid at the outlet in
theconical flask which already contains 20 ml of Hcl
6. Using phenolphthalein as indicator, titre this solution against NaOH
7. Collect the sample for every 5 degree rise in temperature and repeat the steps.
OBSERVATION:
Normality of ethyl acetate, N4 = 0.1N
Normality of acetic acid, N1 = 0.1N
Diameter of reactor, d = cm
Length of reactor, L = cm
TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)
Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:
Vol. of
NaoH
Temp CA CB k -r
S. (Titre
%Conversion
No value)
0c
gmole Integ Differ Differe
ml gmole Integral
/lit /lit ral ential ntial
AVERAGE VALUE
CALCULATION:
Concentration of NaOH in the feed stream, CA0 = (Strength x Flow rate of NaOH)/ Total flow
rateCA0 =
Concentration of EA in the feed stream, CB0 = (Strength x Flow rate of EA)/ Total flow rate
CB0 =
CA = [(NHcl x VHcl) – (NNaOH x VNaOH)] / Total vol of sample in the conical flask
CA =
CB = CA0 – CB0 +
CA CB =
-r (integral) = k C2 A
-r (integral) =
Activation energy:
ln (r2 / r1) = -E/R (1/ T1 – 1/T2)
Integral: E =
=
Differential: E =
E=
RESULT:
The value of rate constant for reaction between NaOH and EA is,
Kdifferential =
Kintegral =
The activation energy is determined as,
Normality of NaOH =
Tabulation:
Volume of
Volume of NaOH required Concentration
Time
S.No sample collected, for neutralizing of H2SO4 in C/C0
(min)
V1 (ml) the sample, V2 sample, N1
(ml)
Model calculations:
N1 =
C / C0 = N1 / N2 =
GRAPH1: Plot the graph between C/C0 (y axis) time (x axis) and identify five different slope
values.
Time (min)
Slope (min-1)
GRAPH 2: Plot the graph between slope which was identified from graph 1 (y axis) time (x
axis).
RESULT:
Thus the experiment of RTD in CSTR was performed and the reading was tabulated and
curve was plotted successfully.