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PLUG FLOW TUBULAR REACTOR 1

OPERATION MANUAL

Introduction

Types of chemical reactors remain a highly discussed in chemical process industries


worldwide. The reactor is the place where chemical reactions take place. Hence it is arguably
the single most important part of any chemical process design. The design of a reactor must
be finely tuned so that its mechanisms suit the necessities of the process that is to be carried.
Depends on the nature of the materials in both the feed and the products, the reactors may
take a wide range of forms. This is why full comprehension of a reactor of a particular design
as well as its working mechanisms is very much vital to actually conduct a particular
chemical process.

In this experiment, the Plug Flow Tubular Reactor is used as it has been properly designed for
students experiment on chemical reactions in liquid phase under isothermal and adiabatic
conditions. Included in the unit is a jacketed plug flow reactor, individual reactant feed tanks
and pumps, temperature sensors and conductivity measuring sensor. By using this particular
unit, students will be capable to conduct the typical saponification reaction between acetate
and sodium hydroxide among the others reaction.

General Description

In the form of nylon tubing that has been would spirally on a glass support
cylinder.
The reactor tubing is high temperature and chemical resistant.
A stirrer motor is mounted on the top of reactor housing frame.
Stirrer motor is controlled on control panel.
The inlet for sodium hydroxide and ethyl acetate is provided beside the stirrer
motor and the inlet piping is of stainless steel.
The inlet piping after entering the glass support cylinder has been converted
into preheat coils with certain number of turns to increase the residence time of
the 2 chemicals inside the hot water bath.
Piping provided with compression joints at connection points for proper sealing
Reactor coil with reactants is heated by a water bath circulator unit.
An inlet and outlet line has been provided for the circulation of water into the
reactor and water bath.
Manual for reactor maintenance, safety and operation along with the
instructions manuals of various parts in the reactor is provided.
2 feeding tanks provided for the reacting chemicals
2 dosing pumps have been positioned beside the reactor housing frame for
feeding the liquid into reactor tubing coil.
Conductivity sensor has been provided to constantly monitor and if necessary
control the conductivity rate of the on-going experiment
A probe holder which is connected to the outlet line from the reactor tubing coil
in order to analyse the conductivity of the resulting solutions has been fixed on
the reactor housing frame.
Temperature monitoring and control system has been provided for the logging
of water temperature inside the water bath circulator and the temperature in the
product line.
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OPERATION MANUAL

Temperature transmission to signal conditioners & PC by K-type


thermocouples.
An elaborate control panel has been installed in the frame of the reactor to
control the equipment in the reactor and co-ordinate the inputs and outputs
from the PC.
Panel designed with power switch, emergency switch, TIC control switch,
water filling, stirrer and alarm light.
Panel displays temperature control value and conductivity value.
A user friendly but detailed software has been custom designed specifically for
the PFR data logging.
Software is loaded completely into the PC.
A CD ROM of the software will be provided to the customer for future
reference along with the appropriate manuals.
Work sheets for the data acquired are managed and the required graphs between
the constants or values measured are plotted.
PLUG FLOW TUBULAR REACTOR 3
OPERATION MANUAL

Description of Equipment Layout

Valve for Air Inlet

Dosing Pump 1 Dosing Pump 2


Conductivity
Sensor

Air Regulator

Stirrer
Sampling Point

Electrical
Control Panel
Reactor
Tubing Coil

Temp. Control
Water Bath
Tank

Waste Tank
Reactant Tank
Waste Tank Outlet
1&2
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OPERATION MANUAL
(6)

(5)
(8)

(7) (9)

(21)
(15)

(4)

(20)
(12)

(2) (3) (10)


(11) (18)
(13)

(1) (14)

(16) (17) (19)

(1) Reactant Tank


Size: 450 mm x 300 mm x 360 mm
Material: Polyvinyl Chloride (PVC)
Able to contain 2 type of chemicals seperately
Install below the reactor.

.
(2) Dosing Pump 1
Maximum Flow Rate: 360 ml/min
Impulse / minute: 118
Power: 65 W
Installed beside to the dosing pump 2.

(3) Dosing Pump 2


Maximum Flow Rate: 360 ml/min
Impulse / minute: 118
Power: 65 W
Installed the nearest to the reactor housing frame.
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OPERATION MANUAL

(4) Reactor Tubing Coil


Coil Length: 32.5m
Coil ID: 4 mm
Coil OD: 6 mm
Reactor Volume: 0.4 liter
Material: Nylon
High temperature and chemical resistance
Installed inside the glass support cylinder.
(5) Con 10 Conductivity Sensor
Thread Size: NPT
Maximum Pressure: 1.0MPa
Temperature Range: 0 ~ 100C
Used to detect the conductivity of the solutions in the product line.
Installed above reactor housing frame.
(6) Stirrer
Speed Range: Max. 100 rpm
Used to mix the water inside glass support cylinder.
Stirrer unit is installed above reactor housing tank and impeller is installed
inside the reactor housing frame.
(7) Glass Support Cylinder
Size: 240 mm x 400mm
Material: Glass
Install outside the reactor tubing coil
(8) Reactor Housing Frame
Size: 260 mm x 550mm
Material: Stainless Steel
Support glass support cylinder and reactor tubing coil
Installed beside both dosing pumps
(9) Overflow tube
Size: 12mm x 500mm
Used to exhaust the overflow water in the glass cylinder and water bath
circulator.
Installed inside the reactor.
(10) Level Sensor
Used to detect and maintain the water level
Prevent the heater operates in dry condition
Installed inside the temperature control water bath circulator.
(11) Heater
Power: 240 V
Maximum Temperature: 60C
Used to heat the water to reach the desired temperature and maintain the water
temperature.
Installed at the bottom of the water bath circulator

(12) Solenoid Valve


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OPERATION MANUAL

Once the water temperature is higher than desired temperature, solenoid valve
will open automatically to allow water from outside flowing into the water
bath circulator for cooling.
(13) Temperature Control Water Bath Circulator
Size: 220 mm x 250 mm x 150 mm
Material: Stainless Steel
Used to store the water for heating the solutions inside the reactor tubing coil.
Install at the bottom of reactor housing frame.
(14) Waste Tank
Size: 350 mm x 380 mm x 350 mm
Material: Polyvinyl Chloride (PVC)
Used to store all solutions coming from reactor
Install below reactor housing frame
(15) Air Regulator
Used to regulate the air flowing into the reactor tubing coil for clearing
solutions remained.
Installed beside doing pumps.
(16) Drain valve of reactant tank 1 (V1)
(17) Drain valve of reactant tank 2 (V2)
(18) Drain valve of reactor house tank (V3)
(19) Drain valve of production tank (V4)
(20) Ball valve for air flowing into inlet tubing 1 (V5)
(21) Ball valve for air flowing into inlet tubing 2 (V6)

Electrical Panel Control Description


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OPERATION MANUAL

3 4

5 6

7 8

(1) Temperature Indicator Control (TIC)


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OPERATION MANUAL

Show current temperature of water in water bath circulator. (Value in RED


colour)
Set the desired temperature for the on-going experiment. (Value in YELLOW
colour)
a. Press <<
b. Press or to set the desired temperature.
c. Press MODE to save the adjusted temperature.
Unit: Celcius (C)

(2) Conductivity Monitor


Show the conductivity value of the solutions inside the reactor tubing coil.
Unit: mS/cm
(3) Power Switch
Equipment main power switch
(4) Emergency Stop Button
Press to cut off the equipment power source
(5) TIC Control Switch
Switch on/off the heater inside water bath circulator.
(6) Water Filling
Fill up the water inside reactor.
(7) Stirrer Switch
Adjust the stirrer speed for stirring the solutions inside reactor.
(8) Alarm Light
The alarm light would be flashing and ringing when the water level below the
level sensor.

Safety Considerations
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OPERATION MANUAL

1. The unit must be operated under the supervision of lab tutors who have been properly
trained to handle the unit.
2. Operation manual supplied with the unit must be carefully read and understood before
started operating the unit.
3. Follow the instruction stated in the operation manual carefully during experiment.
4. The unit should be in the stable condition without subjected to any shock, sudden
impact or vibration.
5. Always check and rectify any leak.
6. Leaking couplings or fittings should be carefully retightened. Replace any gaskets or
seals if necessary.
7. Do not touch the hot components of the unit.
8. Be careful when handling any chemicals. Wear the gloves if possible.
9. Make sure the system is sufficiently ventilated when working at atmospheric pressure.
10. Only properly trained staffs are allowed to carry out any servicing.
11. Before any servicing, shut down the whole operation and let the system to cool down
and be properly ventilated.
12. Do not operate heater in dry condition.
13. Shut down the unit after used.
14. Stop the experiment and unit immediately when there is any accident happened.
15. Do not set the temperature of heater over limit.
16. After each experiment, drain off any liquids from the reactor and make sure that the
reactor and tubings are cleaned properly. Flush the system with deionized water until
no trace of salt is detected.
17. Dispose all liquids from tanks immediately after experiments. Do not leave any
solution or waste in the tanks over a long period of time.
18. Wipe off any spillage from the unit immediately.

Summary of Theory

Plug Flow Tubular Reactor


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OPERATION MANUAL

This reactor is also known as tubular flow reactor which is usually used in industry
complementary to CSTR. It consists of a cylindrical pipe and is usually operated at steady
state. For analytical purposes, the flow in the system is considered to be highly turbulent and
may be modeled by that of a plug flow. Therefore, there is no radial variation in concentration
along the pipe.

In a plug flow 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.

In an ideal tubular flow reactor, which is called plug flow reactor, specific assumptions are
made regarding the extent of mixing:
(1) No mixing in the axial direction
(2) Complete mixing in the radial direction
(3) A uniform velocity profile across the radius

Tubular reactors are one type of flow reactors. It has continuous inflow and outflow of
materials. In the 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 stirring prevent complete
mixing of the fluid in the tube.

Rate of reaction and rate law

The rate at which a given chemical reaction proceeds can be expressed in several ways. It can
be expressed either as the rate of disappearance of the reactants, or the rate of formation of
products.
In the following reaction,
aA + bB cC + dD (1)

A and B are the reactants, while C and D are the products. a,b,c,d are the stoichiometric
coefficients for the respective species.

If species A is considered as the reaction basis, then the rate of reaction can be represented by
the rate of disappearance of A. It is denoted by the symbol rA. The numerical value of the
rate of reaction, -rA is defined as the number of moles of A reacting per unit time per unit
volue, and has the typical unit of mol/dm3s.

Similarly, the rate of reaction can be also represented by the rate of disappearance of another
species, such as rB and the rate of formation of a product, such as rC and rD. They can be
related in the following equation:

(2)

The chemical reaction rate is an intensive quantity and depends on temperature and
concentration. The reaction rate equation (or the rate law) is essentially an algebraic equation
involving concentration. It may be a linear function of concentration, or may be some other
types of algebraic equations. One of the most common general forms of this dependence is
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OPERATION MANUAL

the product of concentrations of the individual reacting species, each of which is raised to a
power, for example
(3)
where
k = rate constant
CA = concentration of A species
CB = concentration of B species
= stoichiometric coefficient of A
= stoichiometric coefficient of B

For a given reaction, the particular concentration dependence of the rate law must be
determined almost without exception from experimental observation. Although the functional
dependence may be postulated from theory, experiments are necessary to confirm the
proposed form.

The order of a reaction refers to the powers to which the concentrations are raised in the
reaction rate law. In equation (3), the reaction is order with respect to reactant A, and
order with respect to reactant B. The overall order of the reaction,
n=+ (4)

Conversion

Using the reaction shown in equation (1), and taking species A as the basis of calculation, the
reaction expression can be divided through by the stoichiometric coefficient of species A, in
order to arrange the reaction expression in the form,

(5)

The expression has now put every quantity on a per mole of A basis.
A convenient way to quantify how far the reaction has progressed, or how many moles of
products are formed for every mole of A consumed; is to define a parameter called
conversion. The conversion XA is the number of moles of A that have reacted per mole of A
fed to the system,

(6)

Because the conversion is defined with respect to the basis of calculation (species A), the
subscript A can be eliminated for the sake of brevity and let X = XA.

Mass Balance

In a plug flow reactor, reactants are fed to the reactor at the inlet and the products are
removed from the reactor at the outlet. The reaction takes places within the reactors as the
reacting mixtures moves through the pipe. In an ideal plug of reactor, the reacting mixture is
assumed to move as a plug and its properties are assumed to be uniformly distributed across
the cross section of the reactor.
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OPERATION MANUAL

FA = the molar flow rate of A in moles per time


FAo = the molar flow rate of A at the inlet in moles per time
FAf = the molar flow rate of A at the exit in moles per time
Vo = the volumetric flow rate at the inlet in volume per time
Vf = the volumetric flow rate at the exit in volume per time

Design equation for reactant A in the PFR is obtained by writing the mass balance for reactant
A over a deferential volume of the reacting mixture dV as follows:

Mass of A entering the volume dV per unit time = mass of A leaving the volume dV per
unit time + mass of A accumulated within the volume dV per unit time + mass of A
disappearing by the reaction within the volume dV per unit time

At steady state, no accumulation takes place. Therefore, at steady state, the above reduces to

FAMA = (FA + dFA)MA + (-rA)MAdV (7)

where

FA = the number of moles of A per unit time entering the differential volume dV
(FA + dFA) = the number of moles of A per unit time leaving the differential volume dV
MA = the molar mass of A
(-rA) = the molar rate at which A is disappearing because of the progression of the reaction

Note that the unit of rA os moles per volume per time and there for rA is multiplied by the
molar mass of A to get the reaction rate in compatible unit for the mass balance given by
equation (7)

Removing MA from equation (7) and rearranging it, we get the design equation for reactant A
in an ideal PFR operated at steady-state as follows:

= rA (8)

Working out in terms of the molar flow rate of A, FA:

The volume VPFR required to reduce the molar flow rate of A in the PFR from FAo mol/sec at
the entrance of the reactor to FAf mol/sec at the eit of the reactor can be evaluated by
integrating equation (8) as follows:

(9)

where (-rA) should be expressed as a function of FA.


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OPERATION MANUAL

Working out in terms of the concentration of A, CA:

Concentration CA in an ideal PFR is defined as follows:

(10)

Equation (10) gives FA = CA. Substituting which in (8), we get

= rA (11)

If the volumetric flow rate v is a constant then equation (11) yield

(12)

where
CAo = the respective concentrations of A at the entrance of the reactor
CAf = the respective concentrations of A at the exit of reactor
(-rA) should be expressed as a function of CA

Working out in terms of the conversion of A, xA:

Conversion of A in a PFR is defined by

(13)

which gives FA = FAo (1-xA). Substituting which in equation (8), we get

(14)

when integrated with the conditions xA = 0 at the entrance (where V=0) and xA = xAf at the
exit (where V = VPFR), gives

(15)

xAf = the conversion of A at the exit of the reactor


(-rA) should be expressed as a function of xA.
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OPERATION MANUAL

Introduction of Following Experiments

The stoichiometry of the saponification reaction between NaOH and EtOAc is:
NaOH + EtOAc NaOAc + EtOH

This reaction can be assumed to be second order overall, first order in each reactant, with the
following rate expression:
Rate = k2CNaOHcEtOAc

Where k2 = second order rate constant and CNaOH and CEtOAc are concentrations of NaOH and
EtOAc, respectively. The rate expression has the units [moles/(litre)(time)]. For these
experiments, the unit of time should be minutes.

The apparatus in this experiment is:


1. Plug flow tubular reactor

The apparatus of Back Titration:


1. Conical flask
2. Measuring Cylinder
3. pH indicator
4. Beakers
5. Burette
6. Retort Stand
7. Stop watch
8. Droplet

Chemicals to be used are:


1. 0.1 M Sodium Hydroxide, NaOH
2. 0.1 M Ethyl Acetate, Et(Ac)
3. 0.1 M Hydrochloric Acid, HCl (Optional: for titration)
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OPERATION MANUAL

Standard Operation Procedures

General Start-up Procedures

1. Prepare the following solutions:


a) 15 liter of sodium hydroxide, NaOH (0.1 M) in reactant tank 1.
b) 15 liter of ethyl acetate, Et(Ac) (0.1 M) in reactant tank 2.
2. Ensure that all valves are initially closed.
3. Turn on the power for the control panel.
4. Ensure there is no any liquid inside the reactor tubing. Otherwise, open valve V5 and
V6 and adjust the air regular as small as possible to pump the air into it as long as
there is enough to clear the remained solutions inside reactor tubing before closing the
valve V5 and V6 again.
5. Connect the plastic water hose between water inlet solenoid valve and tap water
which is open to HALF only.
6. Set the desired temperature for the following experiment on the Temperature Indicator
Control (TIC) panel.
7. Turn on the TIC Control switch and keep pushing the water filling button (green
colour button) to fill up the water into the reactor until just below the overflow tube.
8. Switch on the stirrer to 100 rpm.
9. Switch on the computer and click the corresponding software.
10. Switch on pump P1 and pump P2 and adjust both pump to obtain highest possible
flow rate into the reactor by keying in the flow rate value into both blank of pumps P1
(360 ml/ min) and P2 (390 ml/min) into the computer and run it. Switch off them after
the chemicals coming into the reactor tubing coil.
11. The unit is now ready for experiment.

General Shut-Down Procedures

1. Set the temperature lower than that during experiment on the TIC.
2. Keep the cooling water to continue flowing.
3. Switch off pumps P1, P2. Switch off stirrer.
4. Switch off heater once the reactor to cool down to room temperature.
5. Turn off the power for the control panel.
6. Open valve V5 and V6 and adjust the air regulator as small as possible to pump the air
into it as long as there is enough to clear the remained solutions inside reactor tubing
coil before closing the valve V5 and V6 .
7. Open disposal valve V3 to drain any liquid from reactor into waste tank.
8. Keep the solutions for subsequent experiment. Otherwise, open valves V4 to drain all
solutions from waste tank. And also, open valves V1 and V2 to drain the remained
chemicals from reactant tanks to barrels for storage respectively.
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OPERATION MANUAL

Experimental Procedures

i. Preparation of Calibration Curve for Conductivity vs. Conversion

The reaction to be studied is the saponification reaction of ethyl acetate, Et(Ac) and sodium
hydroxide, NaOH. Since this is second order reaction. The rate of reaction depends on both
concentrations of Et(Ac) and NaOH. However, for analysis purposes, the reaction will be
carried out by using equimolar feeds of Et(Ac) and NaOH solutions with the same initial
concentrations. This ensures that both concentrations are similar throughout the reaction.

NaOH + Et(Ac) Na(Ac) + EtOH

The following procedures will calibrate the conductivity measurements of conversion values
for the reation between 0.1 M ethyl acetate 0.1 M sodium hydroxide:
Procedures:
1. Prepare the following solutions:
a. 1 liter of sodium hydroxide, NaOH (0.1 M)
b. 1 liter of sodium acetate, Na(Ac) (0.1 M)
2. Determine the conductivity and NaOH concentration for each conversion values by
mixing the following solution:
a. 0% conversion: 100 mL NaOH
b. 25% conversion: 75 mL NaOH + 25 ml Na(Ac)
c. 50% conversion: 50 mL NaOH + 50 ml Na(Ac)
d. 75% conversion: 25 mL NaOH + 75 ml Na(Ac)
e. 100% conversion: 100 mL Na(Ac)

Analysis and Discussion:


1. Record all data in the sample table in Appendix A.
2. Plot the calibration curve of conductivity vs. conversion. Determine the slope and y-
axis intercept.

ii. Experiment: Saponification of Et(Ac) and NaOH in Plug Flow Reactor

Title: Determine the effects of residence time on the saponification of NaOH and EtOAc by
using a Plug Flow Reactor.

Objective

1. To carry out a saponification reaction between sodium hydroxide (NaOH) and ethyl
acetate (Et(Ac)) in a Plug Flow Reactor(PFR).
2. To measure the conversion of ethyl acetate in saponification as a function of design
parameters in a PFR.
3. To determine the reaction rate constant and the rate of reaction of saponification
reaction in a PFR.
4. To observe the effect of residence time on conversion of ethyl acetate.
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OPERATION MANUAL

Procedure
1. Perform the general start-up procedures as in Standard Operation Procedures.
2. Set the temperature as 30C on Temperature Indicator Control (TIC).
3. To begin a plug flow reaction experiment, key in the flow rate of 50 ml/min to both
blank of pumps P1 and P2 into the computer and run it. Ensure both flow rates are the
same. Record the flow rate.
4. Start the pump 1 and 2 at the same time before starting the timer immediately.
(Computer: adjust the Set Time Record as 60s and click Start Record)
5. After 3 minutes, start monitoring the outlet conductivity value until it does not change
over time. This is to ensure that the reactor reaches the steady state. (You can record
the outlet conductivity value at the 5th minute if the value is still not stable)
6. Record the outlet conductivity value. (You just can start monitoring and recording the
outlet conductivity value after 2-3 minutes in order to make the solution remained
inside the reactor tubing coil during previous experiment has been cleared out.)
7. Calculate the concentration of NaOH exiting the reactor and extent of conversion
from the calibration curve.
8. Optional. Collect 50ml of sample near the opening of production line. Carry out the
back titration procedure manually to determine the concentration of NaOH in the
reactor and extent of conversion.
9. Repeat the experiment from step 2 to 8 for different residence times by increasing the
feed flow rates of NaOH and Et(Ac) to about 100, 150, 200, 250 and 300 ml/min.
Make sure flow rates of both pumps to be equal.
10. Perform the general shut-down procedures as in Standard Operation Procedures.

Back Titration Procedures


1. Fill up the burette with 0.1 M NaOH solution.
2. Pour 10 mL of 0.25 M HCl in a flask.
3. Add 50 mL samples collected from the experiment at every controlled flow rate (50,
100, 150, 200, 250 and 300 mL/min) into 10 mL HCl to quench the saponification
reaction.
4. Drop 3 drops of phenolphthalein into the mixture of sample and HCl.
5. Titrate the mixture with NaOH until it turns light pink.
6. Record the amount of NaOH titration.

Result

Volume of reactor tubing coil: 0.4 L


Concentration of NaOH in the reactor, CNaOH : 0.1 M
Concentration of NaOH in the feed vessel, CNaOH : 0.1 M
Concentration of HCl quench, CHCl : 0.25M (0.01L) (if applicable)
Volume of sample, Vs : 0.05L (if applicable)
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OPERATION MANUAL

Table 1
Flowrate of Flowrate of Total Minimum Maximum Average Volume of
P1 (ml/min) P2 (ml/min) Flowrate of Outlet Outlet Outlet NaOH (if
Solutions, t0 Conductivit Conductivit Conductivit applicable)
y (mS/cm) y (mS/cm) y (mS/cm)

Table 2

Residence time, (min) Conversion, X (%) Reaction Rate Rate of Reaction, -rA
Constant, k(L.mol/min) (mol.L/min)
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OPERATION MANUAL

Analysis and Discussion


1. Use the sample graph in Appendix for data collection.
2. Find out the residence time , conversion X, reaction rate constant k, rate of reaction
rA
3. Plot a graph of conversion vs residence time.

Result (For Reference ONLY)


Volume of reactor tubing coil: 0.4 L
Concentration of NaOH in the reactor, CNaOH : 0.1 M
Concentration of NaOH in the feed vessel, CNaOH : 0.1 M
Concentration of HCl quench, CHCl : 0.25M (0.01L) (if applicable)
Volume of sample, Vs : 0.05L (if applicable)

Flowrate of Flowrate of Total Minimum Maximum Average Volume of


P1 (ml/min) P2 (ml/min) Flowrate of Outlet Outlet Outlet NaOH (if
Solutions, t0 Conductivit Conductivit Conductivit applicable)
y (mS/cm) y (mS/cm) y (mS/cm)
50 50 100 8.15 8.37 8.26

100 100 200 8.45 8.65 8.55

150 150 300 8.6 9.0 8.8

200 200 400 9.02 9.15 9.09

250 250 500 9.06 9.24 9.15

300 300 600 9.38 9.54 9.46

Table 2
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OPERATION MANUAL

Residence time, (min) Conversion, X (%) Reaction Rate Rate of Reaction, -rA
Constant, k(L.mol/min) (mol.L/min)
4 94.83 45.8559 1.2257 x 10-3

2 91.15 51.49718 4.0334 x 10-3

1 87.98 54.89601 7.9314 x 10-3

1.333333333 84.30 53.69427 13.2351 x 10-3

0.8 83.54 63.44168 17.1884 x 10-3

0.666666667 79.60 58.52941 24.3576 x 10-3

Sample of Calculations

For flow rates of 50 ml/min,

Total flow rate, V0 = Flow rate of NaOH + Flow rate of Et(Ac)


= 50 mL/min NaOH + 50 mL/min Et(Ac)
= 100 mL/min
= 0.1 L/min

Hence, = 4 min

Calculate other residence times in the same way, and varying the flow rates.

Conversion (For Calibration Curve)

From the calibration curve, straight line equation is

y= - 0.1269x + 1.9965

x = Conductivity
y = Conversion

For the flow rate of 50 ml/min, conductivity is 8.26 mS/cm. Thus the value of conversion is:
y = -0.1269x + 1.9965
= -0.1269(8.26) + 1.9965
= 0.9483

Conversion (Optional: For Titration)


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OPERATION MANUAL

For flow rates of 50 ml/min:

Moles of reacted NaOH, n1= Concentration NaOH x Volume of NaOH titrated


= 0.1 M x L
= mole (Answer)

Moles of unreacted HCl, n2 = Moles of reacted NaOH


= n1
= mole (Answer)

Volume of unreacted HCl, V1 =

= L (Answer)

Volume of HCl reacted, V2 = Total volume of HCl V1


= 0.01 L V1
= L (Answer)

Moles of reacted HCl, n3 = Concentration of HCl x V2


= 0.25 M x
= mole (Answer)

Concentration of unreacted NaOH

CNaOH unreacted =

=
= M (Answer)

Xunreacted =

=
= (Answer)

Xreacted = 1 - Xunreacted

Conversion for flow rate 50 mL/min,

Xreacted x 100%
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OPERATION MANUAL

Calculate other conversions in the same way, and varying the flow rates.
Reaction Rate Constant, k

For flow rates of 50 ml/min:

V0 = Total inlet flow rate


= 0.1 L/min

VTFR = Volume for reactor


= 0.4L

CAO = inlet concentration of NaOH


= 0.1 M

X = 0.9483

= 45.8559 L.mol/min

Calculate other reaction rate constants in the same way, and varying the flow rates.

Rate of Reaction, -rA

-rA = k (CA0)2(1-X)2

For flow rates of 50 ml/min:


-rA = (45.8559) (0.1)2(1-0.9483)2
= 1.2257 x 10-3 mol.L/min

Calculate other rate of reactions in the same way, and varying the flow rates.
PLUG FLOW TUBULAR REACTOR 23
OPERATION MANUAL

Appendix: Calibration Curve of Plug Flow Tubular Reactor

Conversion Solution Mixture Concentration Conductivity


0.1 M NaOH 0.1 M Na(Ac) of NaOH (M) (mS/cm)
0% 100 mL - 0.1 15.77
25% 75 mL 25 mL 0.075 13.65
50% 50 mL 50 mL 0.05 11.92
75% 25 mL 75 mL 0.025 9.78
100% - 100 mL 0 7.86