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Chemical Reaction Engineering LAB MANUAL

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0% found this document useful (0 votes)
89 views67 pages

Chemical Reaction Engineering LAB MANUAL

Uploaded by

kaviyas.21chem
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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You are on page 1/ 67

Rajiv Gandhi University of Knowledge Technologies

Department of Chemical Engineering


Chemical Reaction Engineering Lab
(CH3801)
Course Objectives:
• Operate lab equipments like CSTR, Batch, PFR reactors.
• Analyze the concentration versus time data and determine the specific rate
constant and the order of the reaction.
• Compare theoretical and experimental conversions in a CSTR and PFR.
• Estimate RTD and model parameters in a CSTR, PFR, packed bed and
CSTRin-series.

List of Experiments:
S.No Name of the experiment
1. CSTRS in series

2. Isothermal batch reactor


3. Isothermal CSTR
4. RTD studies in CSTR
5. RTD studies in PFR
6. Tubular reactor

Course Outcomes:
• Design the experiments to acquire the kinetic and RTD data.
• Analyze the experimental data to obtain the reaction rate expression
(reaction order and specific reaction rate constant).
• Attain competency in running the bench scale and pilot scale reactors.
ISOTHERMAL BATCH REACTOR-
Peristaltic Pump System
(With Data Logging Facility)
(CRE-907RH)
Foreword
Welcome to the fast growing family of K.C. product owners. We appreciate your interest in us
and thank you for buying our product.

You have chosen the finest quality product in the market which is produced using latest techniques
and has underwent strict quality control tests. It is a product that we are proud to build and you
are proud to own it.

Our products are easy to understand and operate. They are excellent for students who are trying to
gain practical knowledge through experiments.

However your comfort and safety are important to us, so we want you have an understanding of
proper procedure to use the equipment. For the purpose, we urge you to read and follow the step-
by-step operating instructions and safety precautions in this manual. It will ensure that your
favourite product delivers reliable, superior performance year after year.

This manual includes information for all options available on this model. Therefore, you may find
some information that does not apply to your equipment.

All information, specifications and illustrations in this manual are those in effect at the time of
printing. We reserve the right to change specifications or design at any time without notice.

Customer satisfaction is our primary concern. Feel Free to contact us for any assistance. So what
are you waiting for, roll up your sleeves and let us get down to work!

K.C. Engineers Pvt. Ltd.


Important
Important Information About This Manual

Reminder for Safety

Modification on Equipment:

This equipment should not be modified. Modification could affect its performance, safety or
disturbance. In addition damage or performance problems resulting from modification may not be
covered under warranties.

Precautions and Maintenance:

This is used to indicate the presence of a hazard that could cause minor or moderate personal injury
or damage to your equipment. To avoid or reduce the risk, the procedures must be followed
carefully.
Contents
1. Objective …………………………………… 1

2. Aim …………………………………… 1

3. Introduction …………………………………… 1

4. Theory …………………………………… 1

5. Description …………………………………… 3

6. Utilities Required …………………………………… 3

7. Installation procedure of software …………………………………… 4

8. Method of operating software …………………………………… 4

9. Experimental Procedure …………………………………… 4

10. Observation & Calculation …………………………………… 5

11. Nomenclature …………………………………… 6

12. Precautions & Maintenance Instructions …………………………………… 7

13. Troubleshooting …………………………………… 7

14. References …………………………………… 7

K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR


(With Data Logging Facility)
(Rev. 1)
ISOTHERMAL BATCH REACTOR (WITH DATA LOGGING
FACILITY)
1. OBJECTIVE:
To study of a non-catalytic homogeneous reaction in an isothermal batch reactor.

2. AIM:

• To study the progress of a chemicals reaction and determine the kinetic parameters.

• To determine the effect of temperature on reaction rate constant.

3. INTRODUCTION:
A batch reactor is a closed system with no input and output streams. A batch reactor can
operate under the following conditions :

• Isothermal (temperature of reaction mass remains constant).

• Perfectly mixed (composition of the reaction mixture is uniform through out).

• Constant volume (volume of the reaction mixture within the reactor remains
constant, there is no appreciable change in the density of reaction mass).

4. THEORY:

REACTION:

NaOH + CH3COOC2H5  CH3COONa + C2H5OH

(A) (B) (C) (D)

The above reaction is second order reaction (n = 2)

For second order reaction

− dC A
− rA =
dt

− r A = KC A2 …………………………………………(1)

K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR


(With Data Logging Facility)
Page No. 1 of 7 (Rev. 1)
Where − r A is rate of disappearance of A, C A is concentration of A at any time t, K is
rate constant.

The performance equation for the batch reactor is:

CA
dC A
t =− ∫
C Ao
−r A
……………………………………… (2)

Where t is time of reaction, C Ao is initial concentration of A, C A is concentration of A at

any time t.

Substitute the value of − r A in eqn (2) from eqn (1)

C
1 A dC A
K C∫Ao C A 2
t =− ……………………………………..(3)

On solving the above equation we get

CA
1  1 
t=  
K  C A  C Ao

1  C Ao −C A 
t=  
K  C A C Ao 
C Ao − C A
Rate constant, K =
t C Ao C A

(C Ao − C A )
Degree of conversion, X A =
C Ao

Also, a plot of t vs. XA/ (1-XA) shall yield a straight line for an assumed second order
reaction with slope = 1/(KCAo). From this slope rate constant, K can be calculated.

Effect of temperature on reaction rate constant is expressed in terms of

Arrhenius‘law

K = K o e − E / RT

K o is the frequency factor and E is called the activation energy of reaction, R is real gas
constant, and T is reaction temperature.

A plot of ln K vs 1/T on semilog paper yields a straight line with slope = -E/R

From this slope, activation energy, E can be calculated.


K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR
(With Data Logging Facility)
Page No. 2 of 7 (Rev. 1)
5. DESCRIPTION:
The set up consists of a reactor made up of Borosilicate glass fitted in a constant
temperature water bath. One stirrer is fitted for mixing the reactants in reactor and other
is fitted in water bath to keep the uniform temperature throughout in the bath. The
temperature of bath can be maintained from ambient to 80°C with the help of digital
temperature indicator cum controller. Product from the reactor is analyzed by electronic
sensor.

The present set-up has a facility to interface the system with computer which enables to
log the experimental data using computer. The educational software and data-logging
package has been developed for unit. This software is capable to tabulate the sample
readings according to the requirement of experiment under study and results obtained
can be compared.

6. UTILITIES REQUIRED:
6.1 Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket
with earth connection.

6.2 Water supply (Initial fill).

6.3 Floor Drain Required.

6.4 Computer system : Pentium IV with DVD drive, Windows 7,MS-office 7 version
pre loaded, One USB slot required in PC for DATA ACQUISITION CARD.

6.5 Laboratory glass ware:-

Beaker (500 ml) : 02 Nos.

6.6 Chemicals:-

Distilled water : 02 Lit

NaOH Pellets : 10 gm

Ethyl acetate : 15 ml

K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR


(With Data Logging Facility)
Page No. 3 of 7 (Rev. 1)
7. INSTALLATION PROCEDURE OF SOFTWARE:
Two DVDs are provided with the equipment. One DVD is of Device Driver and other
DVD of Operating Software. First, place the device driver DVD in DVD-ROM and wait for
5 to 10 seconds. A blue-colored window appears on the screen. Install the software as
per directions. When installation is finished, a shortcut would be created on the desktop
showing name as “NI-Max”. Restart the computer system. Fix USB Card in empty USB
slots. This ends the completion of loading of DAQ Card Driver. Now, take Operating
Software DVD and place in DVD-ROM. Open DVD and open folder “Isothermal Batch
Reactor.” and then double click on “Setup.exe”. Follow the instructions and do the
installation.
Go to desktop and double click on “NI-Max”. A window opens and looks at left side.
Follow the path as “My System”  “Devices and Interfaces”  Click on USB-6008:
“Dev1”, Right click and rename it as “049” and press “enter”. Now, it appears as USB-
6008: “049” .Close the window. After completion of installation “restart” the computer
system.

8. METHOD OF OPERATING SOFTWARE:


Open the EXE of selected condenser by clicking it from program Menu of main Menu
bar. Enter Password “kce” for the software and press “enter” or click “OK”. Click the
“Interface” button to open interface of the software. In the entire software, a “NEXT”
button is provided, at left front, which enables to go to next step. Another button named
as “BACK” is present. This facilitates to retrieve last step taken. An “EXIT” button, at
right bottom end, is present there. It may be used to exit at any session and finally,
stopping the software.
Note: In the absence of external hardware (USB-6008), the interfacing section may
not able to work.

9. EXPERIMENTAL PROCEDURE:

9.1 STARTING PROCEDURE:

9.1.1 Prepare 1L of N/10 sodium hydroxide solution by dissolving 4 gm of


sodium hydroxide in 1L of distilled water.

9.1.2 Prepare 1L of N/10 ethyl acetate solution by mixing 8.8 gm (or 9.8 ml) of
ethyl acetate in 1L of distilled water.

9.1.3 Put 400 ml sodium hydroxide and ethyl acetate in two 500 ml beaker.
K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR
(With Data Logging Facility)
Page No. 4 of 7 (Rev. 1)
9.1.4 Close all the valves.

9.1.5 Fill water in the water bath.

9.1.6 Fill ethyl acetate solution in the reactor.

9.1.7 Ensure that ON/OFF switches given on the panel are at OFF position.
o
9.1.8 Set the reaction temperature (ambient to (50-70) C) by increment,
decrement and set button of DTC.

9.1.9 Connect electric supply to the set-up.

9.1.10 Start the heater and stirrer of the bath and wait till constant temperature is
attained.

9.1.11 Fill sodium hydroxide into the reactor.

9.1.12 Start motor and stirrer of the reactor.

9.1.13 At regular intervals of 3-5 min record the conductivity of reactants in


computer interface..

9.1.14 Record the reaction temperature.

9.1.15 Repeat the experiment for different reaction temperature.

9.2 CLOSING PROCEDURE:

9.2.1 When experiment is over switch OFF the motor and stirrer of reactor.

9.2.2 Switch OFF the heater and stirrer of the water bath.

9.2.3 Drain the reactor and water bath by open their drain valves respectively.

10. OBSERVATION & CALCULATION:

10.1 DATA:
Initial concentration of NaOH in feed mixture CA0 = 0.1 mole/ltrs

K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR


(With Data Logging Facility)
Page No. 5 of 7 (Rev. 1)
10.2 OBSERVATION TABLE:

S. No. T (oC) t (min) CA(mole/L)

10.3 CALCULATIONS:
C Ao − C A
XA =
C Ao

C Ao − C A
K= (L/mole min)
tC AC Ao

CALCULATION TABLE: 1

S. No. t (min) XA K (L/mole min)

11. NOMENCLATURE:

Nom Column Heading Units Type


CA Concentration of unreacted NaOH in the reactor mole/L Measured

C Ao Initial concentration of NaOH in the feed mixture mole/L Calculated

K Rate constant for individual run L/ mole min Calculated


NNaOH Normality of NaOH in feed solution g eq /L Given
o
T Reaction temperature C Given
t Time min Measured
XA Degree of conversion * Calculated

* Symbols represent unitless quantity.

K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR


(With Data Logging Facility)
Page No. 6 of 7 (Rev. 1)
12. PRECAUTION & MAINTENANCE INSTRUCTIONS:
12.1 Measure the exact volume of water and weigh the chemicals.

12.2 Always use distilled water, good quality chemicals and standard solution for
titration.

12.3 Keep close all the drain valves while filling the reactant in reactor.

12.4 Handle the chemicals carefully.

12.5 Don’t ON heater switch before filling water in the water bath.

13. TROUBLESHOOTING:
13.1 If there is any leakage tight that part or fix it again after wrapping teflon tape.

13.2 If D.T.C do not display on display board it means sensor connection is not proper
(tight computer jacket).

13.3 If switch of the heater is ON but temperature can’t rise but panel LED is ON it
means bath heater had burned replace that.

14. REFERENCES:
14.1 Levenspiel, Octave (2001). Chemical Reaction Engineering. 3rd Ed. NY: John
Wiley & Sons. pp 27-29, 44, 92, 111.

14.2 Fogler H. Scoot (2008). Elements of Chemical Reaction Engineering. 4th Ed. ND:
Prentice-Hall of India Pvt. Ltd. pp 148-150, 152-155.

K.C. Engineers Pvt. Limited, Ambala ISOTHERMAL BATCH REACTOR


(With Data Logging Facility)
Page No. 7 of 7 (Rev. 1)
7

RTD STUDIES IN CSTR


Peristaltic Pump System

(CRE-914 RHb)
7

Foreword
Welcome to the fast growing family of K.C. product owners. We appreciate your interest in us
and thank you for buying our product.

You have chosen the finest quality product in the market which is produced using latest techniques
and has underwent strict quality control tests. It is a product that we are proud to build and you
are proud to own it.

Our products are easy to understand and operate. They are excellent for students who are trying to
gain practical knowledge through experiments.

However your comfort and safety are important to us, so we want you have an understanding of
proper procedure to use the equipment. For the purpose, we urge you to read and follow the step-
by-step operating instructions and safety precautions in this manual. It will ensure that your
favourite product delivers reliable, superior performance year after year.

This manual includes information for all options available on this model. Therefore, you may find
some information that does not apply to your equipment.

All information, specifications and illustrations in this manual are those in effect at the time of
printing. We reserve the right to change specifications or design at any time without notice.

Customer satisfaction is our primary concern. Feel Free to contact us for any assistance. So what
are you waiting for, roll up your sleeves and let us get down to work!

K.C. Engineers Pvt. Ltd.


7

Important
Important Information About This Manual

Reminder for Safety

Modification on Equipment:

This equipment should not be modified. Modification could affect its performance, safety or
disturbance. In addition damage or performance problems resulting from modification may not be
covered under warranties.

Precautions and Maintenance:

This is used to indicate the presence of a hazard that could cause minor or moderate personal injury
or damage to your equipment. To avoid or reduce the risk, the procedures must be followed
carefully.
7

Contents
1. Objective …………………………………… 1

2. Aim …………………………………… 1

3. Introduction …………………………………… 1

4. Theory …………………………………… 1

5. Description …………………………………… 3

6. Utilities Required …………………………………… 3

7. Experimental Procedure …………………………………… 4

8. Observation & Calculation …………………………………… 5

9. Nomenclature …………………………………… 6

10. Precautions & Maintenance Instructions …………………………………… 7

11. Troubleshooting …………………………………… 7

12. References …………………………………… 7

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-


Peristaltic Pump System
(Rev. 1)
7

RTD STUDIES IN CSTR


1. OBJECTIVE:
RTD studies in a CSTR.

2. AIM:
2.1 To plot the RTD curve for a CSTR using a pulse tracer.

2.2 To determine the dispersion number.

3. INTRODUCTION:
Real reactors do not satisfy the idealized flow patterns, back mix flow or plug flow
deviation form ideality can be due to channeling of fluid through the vessel, recycling of
fluid within the vessel or due to the presence of stagnant region or pockets of fluid in the
vessel. To predict the exact behavior of a vessel as a chemical reactor, RTD or stimulus
response technique is used.

4. THEORY:
The exit age distribution function of fluid leaving a vessel or RTD of fluid in a vessel is
called the E-CURVE. The normalized curve is such that

∫ Edt = 1
0
-------------- (1)

In stimulus-response experimentation the system is perturbed and then observes how


the system reacts or responds to this stimulus. The analysis of the response gives the
desired information. A pulse tracer input signal could be used as a stimulus.

The concentration - time curve for pulse signal at the vessel outlet is called the C-
CURVE. Considering steady-state flow of fluid through a closed vessel:

C=E ---------------- (2)

The mean age of the exit stream or mean residence time is:


τ = ∫ tEdt = ∑ tE∆t ---------------- (3)
0

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-


Peristaltic Pump System
Page No. 1 of 7 (Rev. 1)
7

τ=
∑ (t C )i i
---------------- (4)
∑C i

And the variance of the E or C distribution is


σ t2 = ∫ t 2 Edt − τ 2 = ∑ t 2 E∆t − τ 2 ---------------- (5)
0

∑ (t C ) −  ∑ (t C ) 
2 2

σ
i i i i
2
= ---------------- (6)
∑C  ∑ C 
t
i i

Variance, or a measure of the spread of the curve at time θ .

σ t2
σ θ2 = ---------------- (7)
τ2

Models are useful for representing flow in real vessels, for scale up, and for diagnosing
poor flow. We have different kind of models depending on whether

Flow is close to plug, mixed, or somewhere in between. For small deviations from plug
flow dispersion model is used. Suppose an ideal pulse of tracer is introduced

into the fluid entering a vessel. The pulse spreads as it passes through the vessel,

and to characterize the spreading this model, we assume a diffusion like process
superimposed on plug flow. We call this dispersion, the dispersion coefficient D
 D 
represents the spreading process.   is the dimensionless group characterizing
uL

the spread in the whole vessel.

For closed vessel

2
 D   D   −
uL

σθ 2
= 2  − 2   1 − e D
 ----------------- (8)
uL uL  

Ignoring the second term of the above equation we get.

D σ θ2
= ----------------- (9)
uL 2

Defining the reduced time as:

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-


Peristaltic Pump System
Page No. 2 of 7 (Rev. 1)
7

t
θ = ----------------- (10)
τ

Exit age distribution at time i

Ci
Ei = ----------------- (11)
∑ C i ∆t
Exit age distribution at time θ

E θ = τ × Ei ----------------- (12)

Plot a graph between θ vs Eθ.

5. DESCRIPTION:
The setup consists of one feed tank through which water is fed to the borosilicate
reactor. A peristaltic pump is provided to measure flow and circulation of feed. The flow
rate can be adjusted by operating the speed variation knob of pump. The continuous
stirred tank reactor made of borosilicate glass is provided for understanding the RTD
characteristics. A pipette is used for dozing the tracer into the C.S.T.R.

6. UTILITIES REQUIRED:
6.1 Electricity supply: Single phase, 220 V AC, 50 Hz, 5-15 Amp. Combined socket
with earth connection.

6.2 Water supply (Initial fill)

6.3 Floor drain required.

6.4 Laboratory glassware required:-

Burette (50 ml) : 01 No.

Conical flasks (250 ml) : 01 No.

Pipette (20 ml) : 01 No.

Measuring cylinder (250 ml) : 01 No.

6.5 Chemicals:-

N/10 NaOH : 200 ml

Concentrated H2SO4 : 100 ml

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-


Peristaltic Pump System
Page No. 3 of 7 (Rev. 1)
7

Phenolphthalein indicator : Few drops

7. EXPERIMENTAL PROCEDURE:

7.1 STARTING PROCEDURE:

7.1.1 Close all the valves.

7.1.2 Open the lid of feed tank and fill the feed tank with water.

7.1.3 Close the lid of feed tank.

7.1.4 Connect electric supply to the set up.

7.1.5 Switch ON the mains ON/OFF switch.

7.1.6 Switch on the peristaltic pump.

7.1.1 By operating Auto/Manual switch and speed variation pot water is passed
into the reactor.

7.1.7 Fill N/10 sodium hydroxide in burette.

7.1.8 Switch ON the stirrer and wait till the water comes out from the outlet.

7.1.9 Fill the concentrated H2SO4 (10 ml or 20 ml) in the pipette.

7.1.10 Input concentrated H2SO4 into the system with the help of pipette.

7.1.11 At regular time intervals (say 30 sec for high water rate, 1 min for low
water rate), collect 20 ml sample from the outlet in measuring cylinder.

7.1.12 Transfer the sample solution in conical flask.

7.1.13 Titrate the sample solution, using phenolphthalein as an indicator against


N/10 sodium hydroxide (add NaOH from burette).

7.1.14 Repeat the experiment for different RPM (before changing the flow rate,
drain the reactor first).

7.2 CLOSING PROCEDURE:

7.2.1 When experiment is over stop the flow of feed by closing the pump.

7.2.1 Switch OFF the stirrer.

7.2.2 Switch OFF the power supply.

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-


Peristaltic Pump System
Page No. 4 of 7 (Rev. 1)
7

7.2.3 Drain the reactor and feed tank by open their drain valves respectively.

8. OBSERVATION & CALCULATION:

8.1 DATA:
Working volume of reactor VR = ____ Lit
Volume of sample V2 = 20 ml
Normality of NaOH used for titration N1 = 0.1 g eq/L

8.2 OBSERVATION TABLE:

S.No. ti (min) N (RPM) V1 (ml)

8.3 CALCULATIONS:
V 1N 1
N 2= (g eq/L)
V2

N2
Ci= (mole/L)
2

Vo = N × 0.15 (LPH)

V R * 60
τt = (min)
Vo

∆t = t i −t i −1 (min)

CALCULATION TABLE:1

S.No. ti (min) Ci (mol/lit) ti Ci ti2 Ci ∆t (min) Ci ∆ t

∑C i ∑t i C i ∑t i
2
Ci

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-


Peristaltic Pump System
Page No. 5 of 7 (Rev. 1)
7

∑t i C i
τ = (min)
∑C i
 ∑ t i2 C i 
σ t2 =   −τ 2
 ∑ Ci 
 

σ t2
σ θ2 =
τ2

D σθ
2

=
uL 2

Ci
Ei =
∑ C i ∆t
t
θ=
τ

Eθ = τ × E i

CALCULATION TABLE:2

θ Ei Eθ

Plot a graph between θ vs Eθ .

9. NOMENCLATURE:

Nom Column Heading Units Type


Ci Concentration of H2SO4 in sample mole/L Calculated
D/uL Dispersion number * Calculated
Ei Exit age distribution at time i * Calculated
Eθ Exit age distribution at time θ * Calculated
N1 Normality of NaOH used for titration g eq/L Given
N2 Normality of H2SO4 in sample solution g eq/L Calculated
ti Time min Measured
K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-
Peristaltic Pump System
Page No. 6 of 7 (Rev. 1)
7

V1 Volume of NaOH used for titration ml Measured


V2 Volume of sample ml Given
Vo Volumetric flow rate LPH Calculated
VR Working volume of reactor Lit Given
τ Experimental mean residence time min Calculated
τt Theoretical mean residence time min Calculated
θ Reduced time * Calculated
σθ Variance at time θ * Calculated
2
σt Variance at time t min Calculated
∆t Average time difference min Calculated
N Speed of peristaltic pump RPM Measured

* Symbols are unitless

10. PRECAUTION & MAINTENANCE INSTRUCTIONS:


10.1 Measure the exact volume of water and weight of chemicals.

10.2 Always use distilled water, good quality chemicals and standard solution

for titration.

10.3 Keep close all the drain valves while filling the reactant in feed tanks.

10.4 Flow should not be disturbed during the experiment.

10.5 Handle the chemicals carefully.

11. TROUBLESHOOTING:
11.1 If there is any leakage tight that part or fix it again after wrapping Teflon tape.

12. REFERENCES:
12.1 Levenspiel, Octave (2001). Chemical Reaction Engineering. 3rd Ed. NY: John
Wiley & Sons. pp 293-294, 299-301, 305.

12.2 Fogler H. Scoot (2008). Elements of Chemical Reaction Engineering. 4th Ed. ND:
Prentice-Hall of India Pvt. Ltd. pp 871-873, 879, 887-888.

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN CSTR-


Peristaltic Pump System
Page No. 7 of 7 (Rev. 1)
RTD STUDIES IN PFR
(STRAIGHT TUBE TYPE–Peristaltic
Pump System)
CRE-(904RHb)
Foreword
Welcome to the fast growing family of K.C. product owners. We appreciate your interest in us and
thank you for buying our product.

You have chosen the finest quality product in the market which is produced by using latest
techniques and has underwent strict quality control tests. It is a product that we are proud to
build and you are proud to own it.

Our products are easy to understand and operate. They are excellent for students who are trying to
gain practical knowledge through experiments.

However your comfort and safety are important to us, so we want you have an understanding of
proper procedure to use the equipment. For the purpose, we urge you to read and follow the step-
by-step operating instructions and safety precautions in this manual. It will ensure that your
favourite product delivers reliable, superior performance year after year.

This manual includes information for all options available on this model. Therefore, you may find
some information that does not apply to your equipment.

All information, specifications and illustrations in this manual are those in effect at the time of
printing. K.C. reserves the right to change specifications or design at any time without notice.

Customer satisfaction is our primary concern. Feel Free to contact us for any assistance. So what
are you waiting for, roll up your sleeves and let us get down to work!

K.C. Engineers Pvt. Ltd.


Important
Important Information About This Manual

Reminder for Safety

Modification on Equipment:

This equipment should not be modified. Modification could affect its performance, safety or
disturbance. In addition damage or performance problems resulting from modification may not be
covered under warranties.

Precautions and Maintenance:

This is used to indicate the presence of a hazard that could cause minor or moderate personal injury
or damage to your equipment. To avoid or reduce the risk, the procedures must be followed
carefully.
Contents
1. Objective …………………………………… 1

2. Aim …………………………………… 1

3. Introduction …………………………………… 1

4. Theory …………………………………… 1

5. Description …………………………………… 3

6. Utilities Required …………………………………… 3

7. Experimental Procedure …………………………………… 4

8. Observation & Calculation …………………………………… 5

9. Nomenclature …………………………………… 7

10. Precautions & Maintenance Instructions …………………………………… 7

11. Troubleshooting …………………………………… 7

12. References …………………………………… 8

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
(Rev. 1)
RTD STUDIES IN PFR
(STRAIGHT TUBE TYPE)

1. OBJECTIVE:
RTD studies in a Plug flow reactor.

2. AIM:
2.1 To plot the RTD curve for a PFR using a pulse tracer.

2.2 To determine the dispersion number.

3. INTRODUCTION:
In plug flow, the concentration of reactant decreases progressively through the system
and in mixed flow the concentration drops immediately to a low value. Because of this
fact, a plug flow reactor is more efficient than the mixed flow reactors for reaction whose
rates increases with reactants condition.

Real reactors do not satisfy the idealized flow patterns, back mix flow or plug flow
deviation from ideality can be due to channeling of fluid through the vessel, recycling of
fluid within the vessel or due to the presence of stagnant region or pockets of fluid in the
vessel.

To predict the exact behavior of a vessel as a chemical reactor, RTD or stimulus


response technique is used.

4. THEORY:
The exit age distribution function of fluid leaving a vessel or RTD of fluid in a vessel is
called the E-CURVE. The normalized curve is such that

∫ Edt = 1
0
---------------- (1)

In stimulus-response experimentation the system is perturbed and then observes how


the system reacts or responds to this stimulus. The analysis of the response gives the
desired information. A pulse tracer input signal could be used as a stimulus.

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 1 of 8 (Rev. 1)
The concentration - time curve for pulse signal at the vessel outlet is called the C-
CURVE. Considering steady-state flow of fluid through a vessel:

C=E ---------------- (2)

The mean age of the exit stream or mean residence time is:


τ = ∫ tEdt = ∑ tE∆t ---------------- (3)
0

τ=
∑ (t C )i i
---------------- (4)
∑C i

And the variance of the E or C distribution is


σ t2 = ∫ t 2 Edt − τ 2 = ∑ t 2 E∆t − τ 2 ---------------- (5)
0

∑ (t C ) −  ∑ (t C ) 
2 2

σ
i i i i
2
= ----------------- (6)
∑C  ∑ C 
t
i i

Variance, or a measure of the spread of the curve at time θ .

σ t2
σ θ2 = ----------------- (7)
τ2

Models are useful for representing flow in real vessels, for scale up, and for diagnosing
poor flow. We have different kind of models depending on whether

flow is close to plug, mixed, or somewhere in between. For small deviations from plug
flow dispersion model is used. Suppose an ideal pulse of tracer is introduced

into the fluid entering a vessel. The pulse spreads as it passes through the vessel,

and to characterize the spreading this model, we assume a diffusion like process
superimposed on plug flow. we call this dispersion, the dispersion coefficient D
 D 
represents the spreading process.   is the dimensionless group characterizing
uL

the spread in the whole vessel.

For open vessel

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 2 of 8 (Rev. 1)
2
 D   D 
σθ 2
= 2  − 8  ----------------- (8)
uL uL

Solving the above equation we get.

D − 1+ 1+ 8σ θ
2

= ----------------- (9)
uL 8

Defining the reduced time as:

t
θ = ----------------- (10)
τ
Exit age distribution at time i

Ci
Ei = ----------------- (11)
∑ C i ∆t
Exit age distribution at time θ

E θ = τ × Ei ----------------- (12)

Plot a graph between θ vs Eθ.

5. DESCRIPTION:
The set up consists of feed tank through which reactant, fed to the reactor.Peristaltic
pump is provided to measure the flow and circulation of feed. The flow rate can be
adjusted by operating the speed variation knob of pump. The concentration of feed and
the product coming out from the reactor are analyzed by chemical titration.

For understanding the RTD characteristics, a special arrangement to inject tracer into
the reactor, using a syringe is provided.

6. UTILITIES REQUIRED:
6.1 Water supply (Initial fill)

6.2 Floor drain required.

6.3 Laboratory glassware required:-

Burette (50 ml) : 01 No.


Conical flasks (250 ml) : 01 No.

Syringe (20 ml) : 01 No.

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 3 of 8 (Rev. 1)
Measuring cylinder (250 ml) : 01 No.

6.4 Chemicals:-

N/10 NaOH : 200 ml

Concentrated H2SO4 : 100 ml

Phenolphthalein indicator : Few drops

7. EXPERIMENTAL PROCEDURE:

7.1 STARTING PROCEDURE:

7.1.1 Close all the valves.

7.1.2 Open the lid of feed tank and fill the feed tank with water.

7.1.3 Connect electric supply to the set up.

7.1.4 Switch ON the mains ON/OFF switch.

7.1.5 Switch on the peristaltic pump.

7.1.6 By operating Manual switch and speed variation knob water flows thru the
reactor.

7.1.7 Fill N/10 sodium hydroxide in burette. .

7.1.8 Fill the concentrated H2SO4 (10 ml or 20 ml) in the syringe.

7.1.9 Place the syringe at the tracer inlet.

7.1.10 Wait till the water comes out from the outlet.

7.1.11 Push the syringe into the system.

7.1.12 At regular time intervals (say 30 sec for high water rate, 1 min for low
water rate), collect 20 ml sample from the outlet, in measuring cylinder.

7.1.13 Transfer the sample solution in conical flask.

7.1.14 Titrate the sample solution, using phenolphthalein as an indicator against


N/10 sodium hydroxide (add NaOH from burette).

7.1.15 Repeat the experiment for different RPM (before changing the flow rate,
drain the reactor first).

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 4 of 8 (Rev. 1)
7.2 CLOSING PROCEDURE:

7.2.1 When experiment is over stop the flow of water by closing the pump.

7.2.2 Switch OFF the power supply.

7.2.3 Drain the feed tank and reactor by open their drain valves respectively.

8. OBSERVATION & CALCULATION:

8.1 DATA:
Working volume of reactor VR = ____ Lit
Volume of sample V2 = 20 ml
Normality of NaOH used for titration N1 = 0.1 geq/L

8.2 OBSERVATION TABLE:

S.No. ti (min) V1 (ml) N (RPM)

8.3 CALCULATIONS:
V 1N 1
N 2= (g eq/L)
V2

N2
Ci= (mole/L)
2

Vo = N × 0.15 (LPH)

VR * 60
τt = (min)
Vo

∆t = t i −t i −1 (min)

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 5 of 8 (Rev. 1)
CALCULATION TABLE: 1

S.No. ti (min) Ci (mol/lit) ti Ci ti2 Ci ∆t (min) Ci ∆t

∑C i ∑t i C i ∑t i
2
Ci

∑t i C i
τ = (min)
∑C i
 ∑ t i2 C i 
σ t2 =   −τ 2
 ∑ Ci 
 

σ t2
σ θ2 =
τ2

D − 1+ 1+ 8σ θ
2

=
uL 8

Ci
Ei =
∑ C i ∆t
t
θ=
τ

Eθ = τ × E i

CALCULATION TABLE: 2

θ Ei Eθ

Plot a graph between θ vs Eθ .

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 6 of 8 (Rev. 1)
9. NOMENCLATURE:

Nom Column Heading Units Type


Ci Concentration of H2SO4 in sample mole/L Calculated
D/uL Dispersion number * Calculated
Ei Exit age distribution at time i * Calculated
Eθ Exit age distribution at time θ * Calculated
N1 Normality of NaOH used for titration g eq/L Given
N2 Normality of H2SO4 in sample solution g eq/L Calculated
ti Time min Measured
V1 Volume of NaOH used for tritation ml Measured
V2 Volume of sample ml Given
Vo Volumetric flow rate LPH Calculated
VR Working volume of reactor Lit Given
τ Experimental mean residence time min Calculated
τt Theoretical mean residence time min Calculated
θ Reduced time * Calculated
σθ Variance at time θ * Calculated
σt Variance at time t min Calculated
N Speed of peristaltic pump RPM Measured
∆t Average time difference min Calculated

* Symbols are unitless quantity.

10. PRECAUTION & MAINTENANCE INSTRUCTIONS:


10.1 Always use distilled water, good quality chemicals and standard solution for
titration.

10.2 Keep close all the drain valves while filling water in the feed tank.

10.3 Flow should not be disturbed during the experiment.

10.4 Handle the chemicals carefully.

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 7 of 8 (Rev. 1)
11. TROUBLESHOOTING:
11.1 If there is any leakage tight that part or fix that again after wrapping teflon tape.

12. REFERENCES:
12.1 Levenspiel, Octave (2001). Chemical Reaction Engineering. 3rd Ed. NY: John
Wiley & Sons. pp 267, 293-294, 297, 299-301, 305.

12.2 Fogler H. Scoot (2008). Elements of Chemical Reaction Engineering. 4th Ed. ND:
Prentice-Hall of India Pvt. Ltd. pp 871-873, 879, 885-886.

K.C. Engineers Pvt. Limited, Ambala RTD STUDIES IN PLUG FLOW REACTOR (Straight Tube Type)
PERISTALTIC PUMP SYSTEM
Page No. 8 of 8 (Rev. 1)

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