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OPERATION MANUAL
Introduction
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.
PLUG FLOW TUBULAR REACTOR 2
OPERATION MANUAL
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
PLUG FLOW TUBULAR REACTOR 4
OPERATION MANUAL
(6)
(5)
(8)
(7) (9)
(21)
(15)
(4)
(20)
(12)
(1) (14)
.
(2) Dosing Pump 1
Maximum Flow Rate: 360 ml/min
Impulse / minute: 118
Power: 65 W
Installed beside to the dosing pump 2.
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)
3 4
5 6
7 8
Safety Considerations
PLUG FLOW TUBULAR REACTOR 9
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
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.
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
PLUG FLOW TUBULAR REACTOR 11
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.
PLUG FLOW TUBULAR REACTOR 12
OPERATION MANUAL
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
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)
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)
(10)
= rA (11)
(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
(13)
(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)
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.
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.
PLUG FLOW TUBULAR REACTOR 16
OPERATION MANUAL
Experimental Procedures
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.
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)
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.
PLUG FLOW TUBULAR REACTOR 17
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.
Result
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)
PLUG FLOW TUBULAR REACTOR 19
OPERATION MANUAL
Table 2
PLUG FLOW TUBULAR REACTOR 20
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
Sample of Calculations
Hence, = 4 min
Calculate other residence times in the same way, and varying the flow rates.
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
= L (Answer)
CNaOH unreacted =
=
= M (Answer)
Xunreacted =
=
= (Answer)
Xreacted = 1 - Xunreacted
Xreacted x 100%
PLUG FLOW TUBULAR REACTOR 22
OPERATION MANUAL
Calculate other conversions in the same way, and varying the flow rates.
Reaction Rate Constant, k
X = 0.9483
= 45.8559 L.mol/min
Calculate other reaction rate constants in the same way, and varying the flow rates.
-rA = k (CA0)2(1-X)2
Calculate other rate of reactions in the same way, and varying the flow rates.
PLUG FLOW TUBULAR REACTOR 23
OPERATION MANUAL