Chemical Reaction Engineering- I (Seventh Sem. IVth yr.

PREPARATION OF REACTANT SOLUTIONS

1. Ethyl acetate: molecular weight of ethyl acetate is 88 grams & density is 0.897
g/cm3.
In order to make 0.1 N ethyl acetate solution, we have to take 8.8 gram of ethyl
acetate (for 1 N solution 88 grams of ethyl acetate so for 1/10N solution 88/10=8.8
grams of ethyl acetate is required). But ethyl acetate available in laboratory is in
liquid state so it can’t be measured in grams so we will convert it into equivalent
volume by dividing it by its density.

𝟖. 𝟖 ÷ 𝟎. 𝟖𝟗𝟕 𝟗. 𝟖𝟏
∴ 𝟎. 𝟏 𝑵 = =
𝟏 𝒍𝒊𝒕 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏 𝟏 𝒍𝒊𝒕 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏

So measure 9.81 ml of ethyl acetate in small measuring cylinder (for more accuracy)
then transfer it to large measuring cylinder & add requisite amount of makeup water
till total volume becomes 1 lit. (i.e. Ethyl acetate + water = 1000 ml= 1lit).

2. NaOH: As NaOH is monovalent compound its molecular weight = equivalent weight

= 40grams.
In order to make 0.1 N NaOH solution, we have to take 4 gram of NaOH (for 1 N
solution 40 grams of NaOH so for 1/10N solution 40/10=4 grams of NaOH is
required).
So dissolve 4 grams of NaOH in 50 ml water (for more accuracy), transfer this to
large measuring cylinder & makeup water till total volume becomes 1000 ml= 1lit.

3. HCL: For HCL also molecular weight = equivalent weight = 36.5, density= 1.18 g/cc
Basis: 100 gram of 35% lab HCL bottle

𝟏𝟎𝟎
= = 𝟖𝟒. 𝟕𝟒 𝐜𝐜
𝟏.𝟏𝟖

𝟑𝟓
Actual HCL in it = 35 grams = 𝒆𝒒 = 𝟎. 𝟗𝟓𝟖 𝒆𝒒
𝟑𝟔.𝟓

𝟏𝟎𝟎𝟎
Normality of bottle HCL = × 𝟎. 𝟗𝟖𝟓 = 𝟏𝟏. 𝟑 𝑵
𝟖𝟒.𝟕𝟒
Bottle HCL: Experimental HCL
N1 V1 = N2 V2
11.3× V1 = 0.1 × 1000
∴ 𝑽𝟏 = 8.84 ml

So measure 8.84 ml of HCL in small measuring cylinder (for more accuracy),

transfer it to large measuring cylinder & makeup water till total volume becomes
1000ml.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

(Note: preparation method of HCL mentioned above is for 35% conc. HCL. If
conc. of HCL changes then 35% term in above calculation must be replaced by
that corresponding value of conc.)

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO.1

Aim: To determine activation energy of saponification of ethyl acetate and NaOH.

Apparatus: Isothermal batch reactor, Pipette, Burette, Conical flask, Beakers, Measuring
cylinder.

Chemicals: 0.1N Ethyl Acetate, 0.1N NaOH, 0.1N HCl, phenolphthalein indicator.

Reaction: CH3COOC2H5 + NaOH CH3COONa +C2H5OH

Theory:

Activation energy:

The minimum amount of energy which the colliding molecules must have in order to
bring about the reaction is known as activation energy. OR the energy barrier that the
molecule must overcome when the reaction system passes from one state to another.

Lower the value of activation energy higher will be the rate at which the reaction will
proceed (as the considerable part of collision between the molecules result in the reaction)
and higher the value of activation energy, lower will be the rate at which the reaction
proceeds.

For many reactions the temperature dependence of the reaction rate constant, k, can be
correlated by the equation of the type

k= ko e-E/RT

Where ko = frequency factor

E = activation energy
R= gas constant = 8.314 J/ (mol K)=1.987 cal/(mol K)
T= absolute temperature, K
Above equation is known as Arrhenius equation/ Arrhenius law

The activation energy is determined experimentally by carrying out the reaction at different
temperatures.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Frequency Factor:

In chemical kinetics, the pre-exponential factor or k0 factor is the pre-exponential constant in

the Arrhenius equation, an empirical relationship between temperature and rate coefficient. It
is usually designated by k0 when determined from experiment.

The frequency factor depends on how often molecules collide when all concentrations are
mol/L and on whether the molecules are properly oriented when they collide.

Taking the natural logarithm of above equation

ln k = ln k0 – (E/R) (1/T)

It follows from above equation that the plot of ln k vs 1/T should give a straight line with
slope equal to E/R

Slope = E/R

lnk

(1/T) 103

Figure: Temperature dependency of reaction rate.

So one must have the data of reaction rate constant as a function of temperature for getting E
known

Alternatively, the activation energy can also be obtained by measuring the rate constant k1
and k2 at temperature T1 and T2 respectively.

ln k1 = ln k0 – E/(RT1)

ln k2 = ln k0 – E/(RT2)

ln k2 – ln k1 = – E/(RT2) + E/(RT1)

ln (k2/k1) = - E/R (1/T1 – 1/T2)

ln (k2/k1) = E/R (1/T2 – 1/T1)

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Activation energy and temperature dependency

The temperature dependency of the reactions is determined by activation energy and

temperature level of reaction as illustrated in above graph. These finding are summarised are
as follow:

1. From Arrhenius law a plot of ln k vs 1/T gives a straight line with large slope for
large E and small slope for small E.
2. Reaction with high activation energy is very temperature sensitive; reaction with the
low activation energies is relatively temperature insensitive.
3. Any given reaction is much more temperature sensitive at low temperatures than at a
high temperature.
4. From the Arrhenius law the value of the frequency factor k0 does not affect the
temperature sensitivity.

Procedure:

Initially the experiment is carried out at room temperature

1. Take water in water bath and start stirrer of water bath.

2. Prepare half litre each of 0.1N ethyl acetate and 0.1N NaOH.
3. Pour both of them to batch reactor simultaneously and switch on the stirrer. Note
down the time.
4. Measure HCl (20ml) in a measuring cylinder for neutralisation and transfer to conical
flask.
5. Fill the burette with 0.1 N NaOH. Draw the sample from bottom valve of reactor after
10min and immediately transfer into HCl flask. Stirred for 2-3 min.
6. Pipette out 5ml of stirred mix from it and titrate against 0.1N NaOH using
phenolphthalein as indicator. Note down the burette reading.
7. Draw another sample after 20min,30 min and 40 min, repeat the same procedure.
8. The experiment is carried out at different temperature.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Observation Table:

At room temperature

Sr. Volume of sample Volume of Volume of Burette k

No. from reactor HCl in sample Reading Time (lit/mol.min)
(ml) (ml) For titration (ml) (min)
(ml)
1
2
3
4
5
At 40o C

Sr. Volume of Volume of Volume of sample Burette k

No. sample from HCl in for titration (ml) Reading Time (lit/mol.min)
reactor (ml) (ml) (min)
(ml)

1
2
3
4
5

At 50o C

Sr. No. Volume of Volume of Volume of Burette Time k

sample HCl sample for Reading (lit/mol.min)
from (ml) titration
reactor (ml) (ml) (min)
(ml)

1
2
3
4
5

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

At Room temperature

Sr. Burette HCL0 HCLC HCLR CR Time K k avg

No. Reading (mol/lit) (min) (lit/mol.min) Lit/(mol.min)

(ml)

At 400 C

Sr. Burette HCL0 HCLC HCLR CR Time K K avg

No. Reading (mol/lit) (min) (lit/mol.min) Lit/(mol.min)

At 50 0 C

Sr. Burette HCL0 HCLC HCLR CR Time K K avg

No. Reading (mol/lit) (min) (lit/mol.min) Lit/(mol.min)

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Calculation Table:

Sr. No. T 1/T k ln k

(K) (lit/mil.min)
1

Result:

The activation energy for the reaction between ethyl acetate & NaOH is found to be

Theoretically=

Graphically =

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO.2

Aim: To study the kinetics of reaction between ethyl acetate and NaOH in isothermal batch
reactor.

Apparatus: Reactor vessel with stirrer, conical flasks, Burette, Pipette.

Chemicals: 0.1N ethyl acetate, 0.1N NaOH, 0.1N HCl, phenolphthalein indicator.

Reaction: CH3COOC2H5 + NaOH > CH3COONa +C2H5OH

Theory:
The Batch reactor is the generic term for a type of vessel widely used in the process
industries. Its name is something of a misnomer since vessels of this type are used for a
variety of process operations such as solids dissolution, product mixing, chemical reactions,
batch distillation, crystallization, liquid/liquid extraction and polymerization. In some cases,
they are not referred to as reactors but have a name which reflects the role they perform (such
as crystallizer, or bio reactor).

A typical batch reactor consists of a tank with an agitator and integral heating/cooling system.
These vessels may vary in size from less than 1 litre to more than 15,000 litres. They are
usually fabricated in steel, stainless steel, glass lined steel, glass or exotic alloy. Liquids and
solids are usually charged via connections in the top cover of the reactor. Vapors and gases
also discharge through connections in the top. Liquids are usually discharged out of the
bottom.

The advantages of the batch reactor lie with its versatility. A single vessel can carry out a
sequence of different operations without the need to break containment. This is particularly
useful when processing toxic or highly potent compounds.

Analysing kinetic data for particular reaction means finding a rate of equation to fit the data
which in turn means determining the order of the reaction with respect to reactants and rate
constant for given reaction. The steps to be followed for applying the complete rate equation
by differential method.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

1. Hypothesis a mechanism and obtain from if rate equation, assume rate equation in
terms
-CA = -dCA/dt = k f(C)
For A Product
2. From the experiment obtain time concentration data.
3. Plot the concentration time data.
4. Determine the value of slope.
5. Evaluate function f(C).
6. Plot –dCA/dt i.e. If we obtain a line from origin then equation is constant with data
i.e. order of reaction is correct; the slope of straight line gives values of rate constant.
7. For the reaction,
CH3COOC2H5 + NaOH CH3COONa +C2H5OH
A+B products; M=CB0/CA0 (M=Reactant ratio)
-rA =- rB = kCACB ; when M=1, Then –rA= kCACB=kCA2
kindividual = [(1/CA) –(1/CAo)] (1/t); kavg = (k1+k2+k3+k4)/4

Procedure:

Initially the experiment is carried out at room temperature

1. Take water in water bath and start stirrer of water bath.

2. Prepare half litre each of 0.1N ethyl acetate and 0.1N NaOH.
3. Pour both of them to batch rector simultaneously and switch on the stirrer. Note down
the time.
4. Measure HCl (20ml) in a measuring cylinder for neutralisation and transfer to conical
flask.
5. Fill the burette with 0.1 N NaOH. Draw the sample from bottom valve of reactor after
10min and immediately transfer into HCl flask. Stirred for 2-3 min.
6. Pipette out 5ml of stirred mix from it and titrate against 0.1N NaOH using
phenolphthalein as indicator. Note down the burette reading.
7. Draw another sample after 20min and 30 min and repeat the same procedure.
8. The experiment is carried out at different temperature.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Observation table:

Sr. No. Volume of Volume of Volume of Burette Time K

sample from HCl sample for Reading Lit/(mol)(min)
reactor (ml) (ml) titration
(ml) (ml) (min)

1
2
3
4
5

Calculation Table:

Sr. No. T CA 1/CA

1
2
3

Result:

The kinetics of saponification reaction between ethyl acetate and NaOH is found average
given by

-rA = k graphically =
-rA = k analytically =

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO.3

Aim: To study the kinetics of saponification of ethyl acetate & NaOH in Plug Flow Reactor.

Apparatus: Pipette, burette, conical flask, beakers, measuring cylinder.

Chemicals: 0.1 N Ethyl acetate, 0.1 N NaOH, 0.1 N HCl, Phenolphthalein indicator.

Reaction: CH3COOC2H5 + NaOH CH3COONa +C2H5OH

Theory:

Plug flow reactor is characterized by the fact that the flow of the fluid through the
reactor is orderly with no element of fluid overtaking or mixing with any other element ahead
or behind. Actually, there may be lateral mixing of fluid in a plug flow reactor; however,
there must be no mixing or diffusion along the flow path. The necessary and sufficient
condition for plug flow is for the residence time in the reactor to be the same for all elements
of fluid.

In PFR the composition of the fluid varies from point to point along path;
consequently, the material balance for a reaction component must be made for a different
element of volume dV. Thus for reactant A, equation is

Input = output + disappearance of reactant by reaction + accumulation (since,

accumulation=0)

FA = (FA +dFA) + (-rA) dV

FA = input of A moles/time;

(FA + dFA) = output of A moles/time;

(-rA) dV = disappearance of A by reaction moles/time.

Also dFA = d[FAo(1-XA)] = - FAodXA

Therefore we get, FAod XA = (-rA) dV

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

dV

CA0, FA0 FA FA+dFA CAf, FAf

XAo=0,o XAf, f

dXA

dXA

Distance through reactor

Fig 1: Notation for a plug flow reactor

General equation is :

𝑋𝐴𝑓 dXA
 = V/o =VCAo/FAo =CAo∫0 (−rA )

𝑋𝐴𝑓 𝑑𝑋𝐴 𝐶𝐴𝑓 𝑑𝐶𝐴

For constant-density system, V/FAo =/CAo = ∫0 (−𝑟𝐴) = -1/CAo ∫𝐶𝐴0 (−𝑟𝐴)

Note : For systems of constant density (constant volume batch and constant density plug
flow ) the performance equation are identical,  for plug flow is equivalent to ‘t’ for the batch
reactor, and the equations can be used interchangeably .

For systems of changing density there is no direct correspondence between batch and
the plug flow equations and the correct equation must be used for each particular situation in
this case the performance equations can’t be used interchangeably .

Area= t = CAoV/FAo

-1/rA r-c curve for the reaction (constant-density system

only)

0 CA CAo

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Fig 2: Graphical representation of the performance equations for PFR

For the reaction,

CH3COOC2H5 + NaOH CH3COONa +C2H5OH

A+B products; M=CB0/CA0 (M=Reactant ratio)

-rA =- rB = kCACB ; when M=1, Then –rA= kCACB=kCA2

kindividual = (CAo – CA1)/τ×CA0×CA1 kavg = (k1+k2+k3+k4)/4

Procedure:

1. Prepare NaOH solution.

2. Prepare Ethyl Acetate solution of required normality.
3. Adjust the flow rate such that two flow rates are equal
4. After steady state collect samples.
5. Titrate the samples taken using phenolphthalein indicator.
6. Repeat the experiment & get two sets of readings.

Precaution:

1. Measure exact volume of water.

2. Use pure water.
3. Handle electronic weighing balance carefully.
4. Don’t disturb the equipment while taking reading.
5. Take care of pressure.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Observation table:

Sr Flow rate Volume of Burette Time

sample for reading
No. NaOH Ethyl acetate titration ml (min)

Calculation Table:

Sr no. CA 1/CA CA0 1/CA0 1/CA-1/CA0 T

Result:

The kinetics of saponification reaction between ethyl acetate & NaOH is found average given
by

k analytically =
k graphically =

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO. 4

Aim: To study the kinetics of saponification of ethyl acetate & NaOH using CSTR at room
temperature.

Apparatus: Pipette, burette, conical flask, beakers, measuring cylinder.

Chemicals: 0.1N Ethyl acetate, 0.1 N NaOH, 0.1 N HCl, Phenolphthalein indicator.

Reaction: CH3COOC2H5 + NaOH CH3COONa +C2H5OH

Theory:
In an ideal CSTR the contents in reactor are well mixed & have uniform composition
throughout. Thus exit stream has same composition as that of fluid within reactor.

Consider the reaction,

CH3COOC2H5 + NaOH CH3COONa +C2H5OH

Rate constant= k = (CA0-CA1)/ t×CA12

Where t is the residence time t =VR/V0

Conversion = XA = CA0 –CA1/CA0

Procedure:

1. Prepare NaOH solution.

2. Prepare Ethyl Acetate solution of required normality.
3. Adjust the flow rate such that two flow rates are equal
4. After steady state collect samples.
5. Titrate the samples taken using phenolphthalein indicator.
6. Repeat the experiment & get two sets of readings.

Precaution:

1. Measure exact volume of water.

2. Use pure water.
3. Handle electronic weighing balance carefully.
4. Don’t disturb the equipment while taking reading.
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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

5. Take care of pressure.

Observation table:

Sr. No. Flow rate Volume of Burette Time

sample for reading
NaOH Ethyl acetate titration (min)

Calculation Table:

Sr no. T XA (1-XA) (1-XA)2 XA/(1-XA)

Result:

The kinetics of saponification reaction between ethyl acetate &NaOH is found average given
by

Kanalytically=

Kgraphically=

Kavg=

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO. 5

Aim: To study the kinetics of saponification of ethyl acetate & NaOH using CSTR at 40oc.

Reaction: CH3COOC2H5 + NaOH > CH3COONa +C2H5OH

Chemicals: 0.1N Ethyl acetate, 0.1 N NaOH, 0.1 N HCl, Phenolphthalein indicator.

Theory:
In an ideal CSTR the contents in reactor are well mixed & have uniform composition
throughout. Thus exit stream has same composition as that of fluid within reactor.

A very important chemical engineering problem is a carrying out of chemical reactions under
controlled condition. Continuous process may take place in a continuous flow stirred tank
(CSTR), where reactant are fed in at a controlled rate & reacted product is drawn off
continuously. Or the reactants may be fed into a long tube (tubular reactor) & discharge product at
the end.

In spite of complexity, it is possible to study a simple reaction in a laboratory under some

conditions. This experiment studies the reaction kinetics of the saponification of ethyl acetate
in a CSTR.

The saponification reaction of ethyl acetate with sodium hydroxide can be represented by the
following stoichiometric equation.

CH3COOC2H5 + NaOH > CH3COONa +C2H5OH

Space time = VR/VO

The reaction is found to be second order & practically irreversible. The rate expression is

- r A = k CACB kmol/(m3/sec)

Rate constant= k = (CA0-CA1)/ t×CA12 =XA/ CA0 (1-XA)2

Conversion = XA = CA0 –CA1/CA0

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Procedure:

1. Prepare NaOH solution.

2. Prepare Ethyl Alcohol solution of required normality.
3. Adjust the flow rate such that two flow rates are equal
4. After steady state collect samples.
5. Titrate the samples taken using phenolphthalein indicator.
6. Repeat the experiment & get two sets of readings.

Precaution:

1. Measure exact volume of water.

2. Use pure water.
3. Handle electronic weighing balance carefully.
4. Don’t disturb the equipment while taking reading.
5. Take care of pressure.

Observation table:

Sr. Flow rate Volume of Burette Time

No. sample for reading
NaOH Ethyl Acetate titration (min)
(ml)
(ml)

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Calculation Table:

Sr no. T XA (1-XA) (1-XA)2 XA/(1-XA)

Result:
The kinetics of saponification reaction between ethyl acetate & NaOH is found average given
by

Kanalytically=

Kgraphically=

Kavg=

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO. 6

Aim: To verify the half life period of saponification reaction between ethyl acetate and
NaOH in isothermal batch reactor.

Reaction: CH3COOC2H5 + NaOH > CH3COONa +C2H5OH

Chemicals: 0.1N Ethyl acetate, 0.1 N NaOH, 0.1 N HCl, Phenolphthalein indicator.

Theory:

Half Life Period:

half life period is defined as the time taken for half of reaction to be completed that is the
time in which the concentration of reactant is reduced to half of its original value is called
half life period of reaction.

Expression for half life period of a reaction of 2nd order will be as follows:

𝟏
T1/2 =
𝒌 𝑪𝑨𝟎

Isothermal Batch Reactor :

A batch reactor is closed system with no input and output streams. A batch reactor can
operate under conditions like isothermal (temperature of reaction mass remains constant),
perfectly mixed (composition of reaction mixture is uniform throughout), and constant
volume (volume of reaction mixture within the reactor remains constant, there is no
appreciable change in density of reaction mss).

Procedure:

1. Prepare the solution of ethyl acetate and NaOH.

2. Run reaction for time interval time.
3. Titrate unreacted NaOH with HCl.
4. Plot time vs concentration and find the value of k.
5. At steady state take sample at regular interval.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

6. Allow reaction for some time and collect sample.

7. Samples are taken at regular time interval.
8. Verify the result using the formula.

Precaution:

1. Use pure water, Measure the exact volume of water.

2. Handle electronic weighing balance carefully.
3. Don’t disturb the equipment while taking reading.
4. Take care of pressure.

Observation table:

Sr. No. Volume of Volume of Volume of Burette Time K

sample from HCl sample Reading lit/(mol)(min)
reactor (ml) (ml) from (min)
filtration (ml)
(ml)

Result:
The half life period for saponification reaction between ethyl acetate and NaOH in batch
reactor is verified and is found as _____________.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO. 7

Aim: - To study the comparison between PFR and MFR.

Plug Flow Reactor:-

In a 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 prevent 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.
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
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
Steady-state Plug Flow Reactor
In a plug flow reactor the composition of the fluid varies from point to point along a flow
path ; consequently, the material balance for a reaction component must be made for a
differential element of volume dV. Thus for reactant equation becomes
input = output + disappearance by reaction + accumulation (=0)

Performance Equation is:-

𝑉 𝜏 𝑋 𝑑𝑋 𝑉 𝑋 𝑑𝑋
=𝐶 = ∫0 𝐴𝑓 −𝑟𝐴 or = 𝐶𝐴𝑜 ∫0 𝐴𝑓 −𝑟𝐴
FAO 𝐴𝑂 𝐴 υO 𝐴

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Advantages and Disadvantages of PFR:-

Usage Advantages Disadvantages

1. Large Scale 1. High 1. Undesired

Conversion thermal
per Unit gradients may
Volume exist

2. Low 2. Poor
2. Fast Reactions operating temperature
(labour cost) control

3. Continuous 3. Shutdown
3. Homogeneous Operation and cleaning
Reactions may be
expensive

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

4. 4. Good heat
Heterogeneous transfer
Reactions

5. Continuous
Production

6. High
Temperature

Mixed flow reactor: -

This type of reactor consists of one or more cylindrical tanks. Normally the tanks are
arranged with their axes vertical, although this is not essential. The stirring of the contents of
each tank is affected by an agitator which is mounted on a shaft inserted through the vessel
lid. In addition, the tank is fitted with the auxiliary equipment necessary to maintain the
desired reaction temperature and pressure conditions. The well-stirred tank reactor is used
almost exclusively for liquid phase reactions, although instances of gaseous reactions have been
reported. In normal operation, a steady continuous feed of reactants is pumped into the vessel and
since there is usually negligible density change on reaction, an equal volume of the reactor contents is
displaced through an overflow pipe situated near the top of the vessel.
A type of reactor is used very commonly in industrial processing is a stirred tank operated
continuously. The MFR is normally at steady state and is usually operated so as to be quite
wellmixed. The temperature and concentration are identical everywhere within the reaction vessel
they are the same at the exits point as they are elsewhere in the tank. The continuous stirred-tank
reactor (CSTR), also known as back mix reactor, is a common ideal reactor type in chemical
engineering. Perfect mixing is assumed in case of Ideal CSTR.
In a perfectly mixed reactor, the output composition is identical to the composition of the
material inside the reactor, which is a function of residence time and rate of reaction. The
ideal CSTR model is often used to simplify engineering calculations and can be used to
describe research reactors. In practice it can only be approached, in particular in industrial
size reactors. Continuous stirred tank reactors are used very commonly in industrial
processes. For this type of reactor, mixing is complete, so that the temperature and the
composition of the reaction mixture are uniform in all parts of the vessel and are the same as
those in the exit stream.

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 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Three stages of the continuous operation of a CSTR can be modeled.

1. from beginning to overflow
2. from overflow to steady state
3. Steady state operation

The first and second stages are transient and they produce differential equations. The third
stage is represented by a steady state model which contains algebraic equations.

Performance Equation is:-

𝑉 𝜏 ∆𝑋 𝑋 1 𝑉 𝑉𝐶𝐴𝑜 𝐶𝐴𝑂 𝑋𝐴
= = −𝑟𝐴 = −𝑟𝐴 or 𝜏=𝑆=υ = =
𝐹𝐴𝑂 𝐶𝐴𝑂 𝐴 𝐴 O FAO −𝑟𝐴

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Advantages and Disadvantages of MFR:-

Usage Advantages Disadvantages

1. Large Scale 1. Low 1. Undesired

Conversion thermal
2. Slow per Unit gradients may
Reactions Volume exist

3. 2. Low 2. Poor
Homogeneous operating temperature
Reactions (labor) cost control

4. Continuous 3. Continuous 3. Shutdown

as well as as well as and cleaning is
Batch Batch expensive
Production Operation
4.For +ve
5. High 4. Low heat order the
Temperature transfer volume of PFR
coefficient is more so PFR
is less efficient

Result: - In this way the comparison between PFR and MFR studied.

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO. 8

Aim: To study the design of PFR

Apparatus: Plug flow reactor, Pipette, Burette, Conical flask, Beakers, Measuring cylinder.

Chemicals: 0.2N Ethyl Acetate, 0.1N NaOH, 0.2N HCl, 0.4N NaOH, phenolphthalein
indicator.

Reaction: CH3COOC2H5 + NaOH CH3COONa +C2H5OH

Theory: The reaction involved is

CH3COOC2H5 + NaOH CH3COONa +C2H5OH

A+ B R+S

CA0= 0.1 mol/lit (CA0= 0.2/2) CR0=0

CB0= 0.2 mol/lit (CB0=0.4/2) CS0=0

We will intentionally take NaOH in excess to the extent of double, this to shift the
equilibrium towards right so that 100% conversion can be achieved according to the Le-
chateleir’s principle.

With this idea we are sure that no ethyl acetate will remain un reacted that being limited
reactant. Where as half of NaOH will remain un reacted because that was taken double based
on this fact, this un reacted NaOH can be estimated first by putting the sample into 0.2 N
HCL (quench). This is done to ensure the ceasing of reaction, if any chance some ethyl
acetate has remain un reacted.

Necessarily while conducting experiment related with design of rector, we will not go for a
reaction 2A→R (i. e CA0=CB0) rather we will go for the reaction A+B → R+S (i.e
CA0≠CB0)

We have decided to go for CA0=0.1 mol/lit, CB0=0.2 mol/lit (i.e value of m=

CB0/CA0=0.2/0.1=2)

Volume of PFR is given by

V/FA0= KCAO2(M-1) × ln((M-XA)/M(1-XA))

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Preparation of reactant solution

1) Ethyl acetate – In order to prepare 0.1 mol/lit we will have to prepare 0.2 mol/lit so
that after mixing it becomes 0.1 mol/lit

Ethyl acetate in 2.5 lit solution= (2.5×2)/1 =0.5 mol

= 0.5 mol × 88 = 44 gm = 44/ 0.9 = 49 ml

Measure 49 ml of ethyl acetate in glass measuring jar .Pour it into the plastic measuring
jar and add water till total become 2.5 lit.

2) NaOH solution : In order to prepare 0.2 mol/lit we will go for preparing 0.4 mol/lit so
that after mixing it become 0.2 mol/lit
NaOH required = (2.4 ×0.4)/1 = 1 mol
= 1×40 = 40 gm
Weight accurately 40 gm NaOH on electronic weighing balance, and go on adding the
water till total becomes 2.5 lit.

Calculation of volumetric flow rate of ethyl acetate :

Using above design equation calculate FA0 for given size of reactor then volumetric flow rate
of ethyl acetate

= (FA0 ×88 ) / (0.9×1000) LPH

Procedure:

1) Prepare 0.2 N, 2.5 lit ethyl acetate solution, 0.4 N ,2.5 lit NaOH solution , 0.1 N HCL
as a quench and 0.1 N NaOH for titration of sample
2) Pour reactant solution in to the feed tank
3) Ensure the absolute emptiness of the reactor
4) Close the drain valve of reactor if open
5) Pressurised both the feed tank upto 0.5 kg/cm2.
6) Open the knob of both the rotameters simultaneously.
7) Adjust ethyl acetate flow rate as calculated above theoretically keep same flow rate of
the NaOH solution ( Because initially prepared NaOH solution is double in
concentration than ethyl acetate. Therefore with equal flow rate we will get CB0/CA0
=2)
8) Calculate the residence time of the reactor with total operating flow rate as follows
T=(V/µ)×60 min
Where V = volume of reactor
µ= total volumetric flow rate
Start the stop watch the movement the flow is put on in to the reactor , verify if the
reactor overflows exactly after the time equal to T or not. The movement reactor start
overflowing draw the sample and titrate it to estimate un reacted NaOH

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Observation Table:

Run No. Flow rate of Flow rate of Vol. of Vol.of Burette

ethyl acetate NaOH (LPH) Sample for quench reading
(LPH) titration (ml) (ml)
(ml)
1.
2.
3.

Conclusion:

Result:

Vendor supplied PFR of following dimension

Dia= 1 inch = 2.54 cm

Length= 4 feet 2 inch = 50 inch = 50×2.54 = 127 cm

V= (π/4) × 2.542 ×127= 643 cc = 0.643 lit

Vendor has supplied the PFR of volume 0.643 lit, we have compared it practically and it has
found to be ______________.

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO.9

Aim: To study the design of isothermal batch reactor.

Apparatus: Reactor vessel with stirrer, conical flasks, Burette, Pipette.

Chemicals: 0.2N ethyl acetate, 0.4N NaOH, 0.1N HCl, 0.1 N NaOH phenolphthalein
indicator.

Reaction: CH3COOC2H5 + NaOH > CH3COONa +C2H5OH

Theory: The design of the batch reactor is given by

t= 1/ KCAO2 × ln((M-XA)/M(1-XA))

Principally if we draw the sample after carrying out the reaction after sometime and put the
fractional conversion obtained at that time in above design equation and time obtained from
the equation if this time tally’s with the actual experimental time then we can conclude that
given size of batch reactor is ok.

Procedure:

1. Prepare half litre each of 0.2N ethyl acetate and 0.4N NaOH and pour it into the batch
reactor.
2. Keep the reaction mixture in the reactor for 30min.
3. Calculate concentration by using kinetic expression for second order by putting t= 30
min and note.
4. Workout for sample by usual procedure and calculate the concentration obtained
experimentally
5. If concentration as calculate theoretically , matches or tallies with the concentration of
obtained experimentally then the said design of reactor is correct.

Observation table:

Sr.no. Vol.of Vol. of HCL Vol. of Vol.of NaOH

sample from solution Sample for
reactor titration

1.

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Conclusion:

Result:

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

EXPERIMENT NO.10

Aim: To study the design of CSTR

Apparatus: CSTR , Pipette, Burette, Conical flask, Beakers, Measuring cylinder.

Chemicals: 0.2N Ethyl Acetate, 0.1N NaOH, 0.2N HCl, 0.4N NaOH, phenolphthalein
indicator.

Reaction: CH3COOC2H5 + NaOH CH3COONa +C2H5OH

Theory: The reaction involved is

CH3COOC2H5 + NaOH CH3COONa +C2H5OH

A+B → R+S

CA0= 0.1 mol/lit CR0=0

CB0= 0.2 mol/lit CS0=0

We will intentionally take NaOH in excess to the extent of double, this to shift the
equilibrium towards right so that 100% conversion can be achieved according to the Le-
0chateleir’s principle.

With this idea we are sure that no ethyl acetate will remain unreacted that being limited
reactant. Where as half of NaOH will remain unreacted because that was taken double based
on this fact,this unreacted NaOH can be estimated first by putting the sample into 0.1 N HCL
(quench). This is done to ensure the ceasing of reaction, if any chance some ethyl acetate has
remain unreacted.

Necessarily while conducting experiment related with design of rector, we will not go for a
reaction 2A→R (i.e CA0=CB0) rather we will go for the reaction A+B → R+S (i.e
CA0≠CB0)

We have decided to go for CA0=0.1 mol/lit, CB0=0.2 mol/lit (i.e value of m=

CB0/CA0=0.2/0.1=2)

V/FA0= XA / KCAO2 × (1-XA)×(M-XA)

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ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Preparation of reactant solution

1) Ethyl acetate – In order to prepare 0.1 mol/lit we will have to prepare 0.2 mol/lit so
that after mixing it becomes 0.1 mol/lit

Ethyl acetate in 2.5 lit solution= (2.5×2)/1 =0.5 mol

= 0.5 mol × 88 = 44 gm = 44/ 0.9 = 49 ml

Measure 49 ml of ethyl acetate in glass measuring jar .Pour it into the plastic measuring
jar and add water till total become 5 lit.

2) NaOH solution : In order to prepare 0.2 mol/lit we will go for preparing 0.4 mol/lit so
that after mixing it become 0.2 mol/lit
NaOH required = (5 ×0.4)/1 = 2 mol
= 2×40 = 80 gm
Weight accurately 80 gm NaOH on electronic weighing balance, and go on adding the
water till total becomes 5 lit.

Calculation of volumetric flow rate of ethyl acetate :

Using above design equation calculate FA0 for given size of reactor then volumetric flow rate
of ethyl acetate

= (FA0 ×88 ) / (0.9×1000) LPH

Procedure:

1) Prepare 0.2 N, 5 lit. ethyl acetate solution, 0.4 N 5 lit NaOH solution , 0.1 N HCL as a
quench and 0.1 N NaOH for titration of sample
2) Pour reactant solution in to the feed tank
3) Ensure the absolute emptiness of the reactor
4) Close the drain valve of reactor if open
5) Pressurised both the feed tank upto 0.5 kg/cm2.
6) Open the knob of both the rotameters simultaneously.
7) Adjust ethyl acetate flow rate as calculated above theoretically keep same flow rate of
the NaOH solution ( Because initially prepared NaOH solution is double in
concentration than ethyl acetate. Therefore with equal flow rate we will get CB0/CA0
=2)
8) Calculate the residence time of the reactor with total operating flow rate as follows
T=(V/µ)×60 min
Where V = volume of reactor
µ= total volumetric flow rate
Start the stop watch the movement the flow is put on in to the reactor , verify if the
reactor overflows exactly after the time equal to T or not. The movement reactor start
overflowing draw the sample and titrate it to estimate un reacted NaOH

34
ChED
 Chemical Reaction Engineering- I (Seventh Sem. IVth yr.)

Observation table:

Sr.no. Vol.of Vol. of HCL Vol. of Vol.of NaOH

sample from solution Sample for
reactor titration

1.

Conclusion:

Result:

Vendor has supplied the CSTR of volume approx 3 lit, we have compared it practically and it
has found to be _______

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ChED