Chemical Reaction Engineering

LIST OF EQUIPMENTS

CHEMICAL REACTION ENGINEERING LABORATORY

Sr. No Equipment
1 Edibon plug flow reactor

2 Edibon batch reactor

3 Elettronica veneta CSTR

4 Elettronica veneta PFR

5 Elettronica veneta reactor

6 Elettronica veneta CSTR in series

7 Catalyzed plug flow reactor

8 Fixed bed reactor

9 Fluidized bed reactor

10 Hybrid reactor

11 Alkaline fading reaction unit

12 Hydrogenation reactor until

13 Pilot plant for sulphonation of benzene

14 Pilot plant for production of hexamethylene tetramine (HMT)

LIST OF EXPERIMENTS

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Chemical Reaction Engineering

Sr.No Experiment
1 To standardize a standard solution of sodium hydroxide and develop equation of
trendline.

2 Find the effect of initial molar concentration (CAo) of a key component for a
given reaction in the lab under the isothermal conditions (constant density
system) on the space time, conversion and space velocity of PFR.

3 To study the kinetics (n and k) of given reaction by using differential analysis.

4 To study the effect of volume of reaction mixture on conversion, space time and
space velocity for continuous reactor.

5 To compare the rate of given chemical reaction at room temperature with and
without agitation.

6 To find/investigate the effect of flow rate on conversion, space time and space
velocity in PFR.

7 To find the value of n and k for the given reaction by using integral analysis.

8 To study the kinetics of saponification reaction (i.e. K) at different temperatures

by using conduct metric method.

9 To study the effect of temperature on the rate of reaction in a batch reactor for a
given saponification reaction in the lab.

10 To study the effect of superficial air velocity on overall heat transfer co-efficient
for the air-steam system in a fluidized bed reactor.

11 Determine rate of conversion of hydrogen to ethane as a function of time in a

tubular flow reactor.

12 To study the effect of superficial air velocity on pressure drop in fixed and
fluidized bed conditions and compare their results.

13 To study the effect of superficial air velocity on overall heat transfer co-efficient
for the air-steam system in a hybrid reactor.

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Chemical Reaction Engineering

14 To determine the rate of reaction in the sulfonation of benzene on a pilot plant.

15 To plot conversion of formalin as a function of time.

16 Find out the activation energy for the hydrogenation of ethylene using magnesia-
copper oxide catalyst.

EXPERIMENT NO. 1

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Chemical Reaction Engineering

Object:

To standardize a standard solution of sodium hydroxide and develop equation of trend

line.

Apparatus:

Beaker, glass rod, conductivity meter, standard solution of NaOH, Cylinder.

Procedure:

1. Prepare standard solution (1 M or 0.1 M) of NaOH ( M= molarity).

2. For 1M solution of NaOH, weigh 40g of NaOH, put it in 1000ml cylinder, then add
water to make volume upto 1000ml.
3. Take 100/200ml of this standard solution in any suitable beaker and measure its
conductivity by conductivity meter.
4. Then add 10ml water each time in the same solution and measure the conductivity.
5. Take at least 10 readings.
6. For molarity of the solution each time use M1V1/n1 = M2V2/n2
7. Draw a graph between molarity (concentration) on x-axis and conductivity (mS, μS,
ppm or mg/L) on y-axis.

Observations And Calculations:

Sr. No Molarity (M) Conductivity (mS , μS, ppm)

Expected Trend (Graph):

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Chemical Reaction Engineering

Graph b/w conductivity and molarity

3.5

3
conductivity (mg/L, ppm)

2.5

1.5

0.5

0
0 0.5 1 1.5 2 2.5 3 3.5
Molarity ( M)

Theory:

The following topics should be covered by students

 Methods of concentration measurement of a solution.

 Conductivity and its units.
 Calibration of conductivity meter.
 Parameters which can be measured by conductivity meter.
 Other techniques for the measurement of concentration of solution.

Learning Outcomes:

EXPERIMENT NO. 2

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Chemical Reaction Engineering

Object:

Find the effect of initial molar concentration (CAo) of a key component for a given
reaction in the lab under the isothermal conditions (constant density system) on the space time
and space velocity of PFR.

Apparatus:

Plug flow reactor

Procedure:

Following points are allowed while performing the experiment.

1. Note the initial concentration CAo of the reaction mixture.

2. Switch on the reactor and let it achieve steady state.
3. After specific time note the final concentration CAf.
4. From the values of CAo and CAf calculate XA.
5. From this XA calculate volume (V), space time (τ) and space velocity (s).
6. Plot the following graph from the calculations:
 Graph between CAo and V.
 Graph between CAo and τ.
 Graph between CAo and s.

Observations And Calculations:

Sr.No CAo CAo CAf XA= 1- V ( liter) τ s=1/τ

(gmole/hr) (μS) (μS) (CAf/CAO) (min) (min-1)

Formulas used:

XA= 1-(CAf/CAO)

𝑋𝐴
𝑉 𝑑𝑋𝐴
=∫
𝐹𝐴𝑂 0 −𝑟𝐴

-rA = k CAo2 (1-XA)2

V/ CAoV0 = (1/(K CAo 2))(XA/(1-XA))

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Chemical Reaction Engineering

τ= V/V0

s = 1/τ

Graphs:

Graph between CAo and V.

V(L)

CA0 (gmol/L)

Graph between CAo and τ.

τ (min)

CA0 (gmol/L)

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Chemical Reaction Engineering

Graph between CAo and s.

s(min-1)

CA0 (gmol/L)

Theory:

The following topics should be covered by students

 Concept of space time and space velocity.

 Construction and working of PFR.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 3

Object:

To study the kinetics (n and k) of given reaction by using differential analysis.

Apparatus:

Batch reactor with and without agitator, glass rod, conductivity meter, standard solution
of NaOH and ethyl acetate, Cylinder.

Reaction:

CH3COOC2H5 + NaOH → CH3COONa + C2H5Na

Procedure:

1. Take 100ml standard solution (1 M or 0.1 M) of NaOH and 100ml of ethyl acetate in
separate beakers.
2. Note the conductivity of (0.1 M) NaOH solution by conductivity meter, it will be C A0
at time t=0.
3. Put these solutions in the batch reactor simultaneously with or without agitation, as the
reaction starts, note the conductivity after every 20 seconds and continue to do so until
a constant reading is obtained.
4. Plot conductivity Vs time and apply differential analysis by plotting tangents to this
curve and then find the values of “n” and “k” after plotting a graph between ln(-dCA/dt)
vs. lnCA.

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Chemical Reaction Engineering

Observations And Calculations:

Sr.No Time Conductivity Points on each Slope ln(--dCA/dt) ln(CA)

(min) (ppm) tangents -dCA/dt

Graph:

CA

(mg/L)

time (t)

ln -dCA/dt

ln CA

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Chemical Reaction Engineering

Theory:

The following topics should be covered by students

 Concept of differential analysis.

 Concept of order of reaction and rate constant.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 4

Object:

To study the effect of volume of reaction mixture on conversion, space time and space
velocity for continuous reactor.

Apparatus:

 CSTR
 PFR

Procedure:

1. First of all, switch on the CSTR and want till it achieves steady state. Then calculate
the initial concentration of the solution.
2. Then calculate the concentration at different intervals.
3. Then calculate the volume by collecting the solution.
4. Calculate the conversion, space time and space velocity.
5. Plot the graph between volume and conversion, volume and space time and volume and
space velocity.
6. Repeat the same procedure for PFR.

Observations And Calculations:

Sr.No CAo XA= 1- V ( liter) τ s=1/τ

(μS) (CAf/CAO) (min) (min-1)

Formulas used:
XA= 1-(CAf/CAO)
τ= V/V0
s = 1/τ

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Chemical Reaction Engineering

Graphs:

Graph between Vo and XA.

XA

VO (L)

Graph between Vo and τ.

τ (min)

VO (L)

Theory:

 Construction and working of CSTR.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 5

Object:

To compare the rate of given chemical reaction at room temperature with or without
agitation.

Apparatus:

Batch reactor with stirrer, beaker, conductivity meter, standard solution of NaOH and
ethyl acetate, cylinder, stop watch, stirrer.

Procedure:

1. Take 100ml or as per required standard solution (0.1 M) each for NaOH and ethyl
acetate in a beaker.
2. Put these solutions in batch reactor simultaneously.
3. First the readings without agitation at room temperature and then with agitation at room
temperature from new solutions.
4. Plot graphs between concentration vs. time and rate of chemical reaction vs. time with
and without agitation.

Observations And Calculations:

Without agitation

Using k= 6.42 L/(gmol)(min)

Sr. No Time Conductivity Conc. -rA=kCA2

(min) (ppm) (mg/L)

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With agitation

Using k= 6.42 L/(gmol)(min)

Sr. No Time Conductivity Conc. -rA=kCA2

(min) (ppm) (mg/L)

Graphs:

Without
Conc. agitation

With
agitation

With
agitation

-rA
Without
agitation

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Chemical Reaction Engineering

Theory:

The following topics should be covered by students

 Concept of rate of reaction.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 6

Object:

To find/investigate the effect of flow rate on conversion, space time and space velocity
in PFR.

Apparatus:

Plug flow reactor

Procedure:

1. Note the initial concentration CA0 of the reaction mixture.

2. Switch on the reactor.
3. Set a specific flow rate and let the reactor achieve steady state.
4. After specific time note the final concentration CAF.
5. From the values of CA0 and CAF calculate conversion XA.
6. Also calculate space time (τ) and space velocity (s).
7. Plot the following graph from the calculations;
 Graph between V0 and XA.
 Graph between V0 and r.
 Graph between V0 and s.

Observations And Calculations:

Observations for pump 1:

Sr.No V0 CAf XA= 1- τ s=1/τ

(ml/min) (mS) (CAf/CAO) (min) (min-1)

Observations for pump 2:

Sr.No V0 CAf XA= 1- τ s=1/τ

(ml/min) (mS) (CAf/CAO) (min) (min-1)

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Chemical Reaction Engineering

Formulas Used:

XA= 1-(CAf/CAO)
τ= V/V0
s = 1/τ

Graphs:

XA

VO (mL/min)

τ (min)

VO (mL/min)

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Chemical Reaction Engineering

s (min)-1

VO (mL/min)

Theory:

The following topics should be covered by students

 Methods of concentration measurement of a solution.

 Conductivity and its units.
 Calibration of conductivity meter.
 Parameters which can be measured by conductivity meter.
 Other techniques for the measurement of concentration of solution.

Theory:

The following topics should be covered by students

 Construction and working of PFR

 Concept of space time and space velocity

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 7

Object:

To find the value of n and k for the given reaction by using integral analysis.

Apparatus:

Batch reactor with and without agitator, glass rod, conductivity meter, standard solution
of NaOH and ethyl acetate, cylinder.

Reaction:

CH3COOC2H5 + NaOH → CH3COONa + C2H5Na

Procedure:

1. Take 100ml standard solution (1 M or 0.1 M) of NaOH and 100ml of ethyl acetate in
separate beakers. Note the conductivity of (0.1 M) NaOH solution by conductivity
meter, it will be CA0 at time t=0.
2. Put 100ml each solution in a batch reactor in the lab simultaneously as the reaction
starts, note the conductivity (ppm,mg/L, mS, μS) by conductivity meter after every 20
sconds and prepare the following table.
3. Plot ln(CA0/CA) vs time for first order kinetics.
4. Plot (1/CA-1/ CA0) vs time with CA0=CB0 or 1/CA vs. time with “1/CA0” as an intercept;
if “CA0” is not known for 2nd order kinetics.
5. Plot ½[1/CA2-1/ CA02] vs. time for third order kinetics. If the above plots in 3,4 and 5
are perfect straight lines with more than (85-90)% of the data falling on this line,
integral analysis is correct, otherwise it fails.
6. For perfect straight line the order (n=1, 2, 3) will be known and from slope of this line
“k” can be found. Remember this method will give integral order only.

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Chemical Reaction Engineering

Observations And Calculations:

Time Conc. CA0/CA ln(CA0/CA) 1/CA-1/ CA0 1/CA ½[1/CA2-1/ CA02]

(min) (CA)

Theory:

The following topics should be covered by students

 Concept of order and rate constant

 Concept of integral analysis

Graph:

ln(CA0/CA)

Time (t)

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Chemical Reaction Engineering

(1/CA)

Time (t)

1/CA-1/ CA0

Time (t)

½[1/CA2-1/ CA02]

Time (t)

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Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 8

Object:

To study the kinetics of saponification reaction (i.e. K) at different temperatures by

using conductometric method.

Apparatus:

Batch reactor, conductivity meter, standard solution of NaOH and ethyl acetate,
cylinder, stop watch.

Procedure:

1. First take data of previous experiment i.e. between time and conductivity.
2. Then calculate C0 – Ct for all the temperatures i.e. 35 0C, 45 0C, 55 0C and 65 0C.
3. After that calculate C0 – Ct for all the temperatures.
4. Find the value of k by using the formula
k= 1/0.01(C0 – Ct/ Ct – Cf) t
5. At the end calculate kavg for all these temperatures which are our objective function.

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 Chemical Reaction Engineering

Observations And Calculations:

At t= 35 0C

(C0 at t=0 sec/min)

(Cf at t where reading becomes constant)

Time Conductivity Conc. C0 – Ct Ct – Cf k= 1/0.01(C0 – Ct/ Ct – Cf) t

(min) mg/L or M
ppm

k1= (kavg) at 35 0C

Similar table should be prepared for temperature i.e. 35 0C, 45 0C, 55 0C and 65 0C and also
calculate the values for average “k” against each temperature i.e. k2,k3,k1.

Theory:

The following topics should be covered by students

 Concept of saponification reaction.

 Concept of Arrhenius law.
 Knowhow of activation energy, frequency factor and rate constant.
 Conductivity and its units.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 9

Object:

To study the effect of temperature on the rate of reaction in a batch reactor for a given
saponification reaction in the lab.

Apparatus:

Beaker, conductivity meter, standard solution of NaOH and ethyl acetate, cylinder,
heating source, stop watch, stirrer.

Procedure:

1. Use the table at different temperatures from experiment no. 8.

2. Find the rate of chemical reaction against each value of time for each temperature.
3. Plot rate of chemical reaction (-rA) vs. time at different temperatures to study the
dynamics of the chemical reaction on the same plot.
4. Also plot concentration vs. time graph for different temperatures on the same plot.
5. Finally plot the relationship between (-rA) vs. temperature to see the effect of
temperature on rate of reaction i.e. -rA= f(T).

Observations And Calculations:

Considering reaction 2nd order i.e. n=2

Sr. no Temperature Conc. k -r1 = kCA2

(°C) (M)

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Graphs:

Rate of
reaction

Temperature

Theory:

The following topics should be covered by students.

 Concept of Arrhenius law.

 Knowhow of activation energy, frequency factor and rate constant.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 10

Fluidized bed reactor

Object:

To study the effect of superficial air velocity on overall heat transfer co-efficient for the
air-steam system in a fluidized bed reactor.

Observations and Calculations:

Packing size =

Thermal conductivity of Aluminum (tube material) = K = 250 KW/mK

Thickness of reactor tube =s= 00016m

Diameter of reactor tube =d= 0.0762

Cross-sectional area of reactor tube = A= (π/4) d2 = 0.785 x (0.0762)2 = 0.00456 m2

Density of air = PM/RT

Superficial air velocity = volumetric flow rate/ cross-sectional area of reactor tube

Mass flow rate= volumetric flow rate x density

Conductive heat transfer coefficient = hcond = K/s =0.25/0.0016 = 16.25W/m2.K

Specific heat of air = Cp=1.006 Kj/kg.K

Heat = Q= mCP∆T

Surface area = As = πdl = 3.14 x 0.0762 x 0.3048 =0.073 m2

Convective heat transfer coefficient = hconv = Q/As∆T

Overall heat transfer coefficient= U= hcond + hconv

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Sr. Volumetric Superficial Mass Q=mCP∆T ∆T hconv U

No Flow rate Air flow rate (kW) Tsteam-Tair =Q/As.∆T (W.m2.K)
(L/min) velocity of air (K) (W/m2.K)
(m/sec) (kg/sec)

Theory:

The following topics should be covered by students

 Concept of fluidization.
 Concept of fluidized bed reactor
 Knowhow of superficial air velocity, heat transfer coefficient and Fourier Law.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 11

Object:

Determine rate of conversion of hydrogen to ethane as a function of time in a tubular

flow reactor.

Equipment:

Tubular flow reactor, stop watch.

Procedure:

1. Prepare the experimental set-up for the proposed experiment.

2. Pre-set the temperature of hot water bath so that it gives a constant reactor wall
temperature throughout the experiment.
3. Fix the feed flow rate and allow it to pass through the reactor before allowing the hot
water to pass through the jacket.
4. Note down the flow rate of feed (gm-moles/sec) and hot water flow rate (cm3/sec)
5. Keep noting the product composition, reactor wall temperature and fixed bed
temperature and hot water inlet and outlet temperatures after every five minutes until
steady state reaches. At this moment, finally record all the parameters.
6. Increase the flow rate of the feed and repeat the procedure.
7. Tabulate the data, as given in table (1).
8. Plot the conversion of hydrogen (yai – yao) as a function of time.

Table (1)
Consumption of hydrogen in reaction as a function of time

Volume of reactor = cm3

0
Reactor wall temperature = C

Mole fraction hydrogen in feed, yai =

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Feed rate, F Time, t Mole Mole Catalyst bed

Run (gm- fraction fraction of temperature
No. moles/sec) hydrogen in hydrogen T
product consumed
min sec stream, in reaction, 0C K
yao (yai-yao)
01 (Fixed 0
throughout 5
the run) 10
15
20
02 (Fixed 0
throughout 5
the run) 10
15
20

Theory:

The following topics should be covered by students

 Concept of catalytic tubular reactor.

 Concept of hydrogenation reaction.

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO. 12

Fluidized bed reactor

Object:

To study the effect of superficial air velocity on pressure drop in fixed and fluidized
bed conditions and compare their results.

Observations and Calculations:

Packing size=

Thermal conductivity of Aluminum (tube material) = K = 250 kW/m.K

Thickness of reactor tube= 0.0016m

Diameter of reactor tube= d= 0.0762m

Cross-sectional area of reactor tube =A= (π/4)d2 = 0.785 x (0.0762)2 = 0.00456 m2

Density of air= 1.006 KJ/kg.K

Superficial air velocity = volumetric flow rate/cross-sectional area of reactor tube

Pressure drop= Pg/gch

For fixed bed

Sr.no Volumetric Superficial air Difference in Pressure drop

flow rate velocity height (kgF/m2)
(L/min) (m/sec) (m)

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For fluidized bed

Sr.no Volumetric Superficial air Difference in Pressure drop

flow rate velocity height (kgF/m2)
(L/min) (m/sec) (m)

Theory:

The following topics should be covered by students

 Concept of fluidization.
 Concept of fluidized bed reactor
 Concept of fixed bed reactor
 Understanding of pressure drop

Learning Outcomes:

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Chemical Reaction Engineering

EXPERIMENT NO.13

Hybrid Reactor

Object:

To study the effect of superficial air velocity on overall heat transfer co-efficient for the
air-steam system in a hybrid reactor.

Observations And Calculations:

Packing size =

Thermal conductivity of Aluminum (tube material) = K = 250 Kw/mK

Thickness of reactor tube =s= 00016m

Diameter of reactor tube =d= 0.0762

Cross-sectional area of reactor tube = A= (π/4) d2 = 0.785 x (0.0762)2 = 0.00456 m2

Density of air = PM/RT

Superficial air velocity = volumetric flow rate/ cross-sectional area of reactor tube

Mass flow rate= volumetric flow rate x density

Conductive heat transfer coefficient = hcond = K/s =0.25/0.0016 = 16.25W/m2.K

Specific heat of air = Cp=1.006 Kj/kg.K

Heat = Q= mCP∆T

Surface area = As = πdl = 3.14 x 0.0762 x 0.3048 =0.073 m2

Convective heat transfer coefficient = hconv = Q/As∆T

Overall heat transfer coefficient= U= hcond + hconv

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Sr. Volumetric Superficial Mass Q=mCP∆T ∆T hconv U

No Flow rate Air flow (kW) Tsteam-Tair =Q/As.∆T (W.m2.K)
(L/min) velocity rate of (K) (W/m2.K)
(m/sec) air
(kg/sec)

Theory:

The following topics should be covered by students

 Concept of hybridization and hybrid reactor.

 Understanding of heat transfer coefficient

Learning Outcomes:

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EXPERIMENT NO. 14

Object:

To determine the rate of reaction in the sulfonation of benzene on a pilot plant.

Procedure:

1. Operate the plant at a temperature of 90 0C until steady state reaches. At this point,
analyze the sample of reaction mixture for Xa, XW and XS.
2. Allow the plant to cool to atmospheric temperature and make it ready for the next run.
3. Operate the plant at temperature of 95 0C, 100 0C and 105 0C and collect sample at
completion of reaction.
4. Analyze the samples in the laboratory and find out the values of Xa, XW and XS.
5. Tabulate the data.
6. Use the formula to calculate the rate of reaction.

Observations And Calculations:

𝑅𝐿 1 1
= 118 (𝑋𝑎 − 2 𝑋𝑤 + 4 𝑋𝑠 )−9.239+5349/𝑇
𝐶𝑎

Concentration of H2SO4 = Ca = (moles/liter)

Run no. Temperature (0C) Absolute Mole fractions

temperature Xa Xw Xs
(K)

Theory:

The following topics should be covered by students

 Concept of sulfonation reaction.

 Understanding of plate columns, heat exchangers, decanter, drier, centrifugal pump

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Learning Outcomes:

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EXPERIMENT NO. 15

Object:

To plot conversion of formalin as a function of time.

Procedure:

1. Take 50 gm sample of formalin solution before adding it to the reactor.

2. Calculate formalin in the sample (w1).
3. Operate the plant as discussed in section (3.6).
4. Take sample of reaction mixture after 30 minutes of addition of ammonia to the reactor.
5. Analyze the sample for unconverted formalin (w2).
6. After this, take samples of the reaction mixture (50 gm) after every 10 minutes till the
reaction is complete and analyze the samples for unconvted formalin.

Observations and Calculations:

1. From the analysis of each run, calculate the amount of formalin converted to HMT as
w3 (w3= w1 – w2).
2. Complete table (1) and plot the data as percent formalin converted to HMT as a function
of time.

Table (1)

Conversion of formalin as a function of time

Time Weight of Weight of formalin Weight of Percent

(min) sample (gm) unconverted (gm) formalin formalin
w1 w2 converted (gm) converted
w3= w1 – w2 (w3/w1) x 100

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Theory:

The following topics should be covered by students

 Properties and uses of hexamethylene tetramine.

 Concept of heating and cooling methods in a chemical reactor.

Learning Outcomes:

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