Technion – Israel Institute of Technology The Department of Chemical Engineering

Laboratory of Chemical Engineering II – Winter 2017

Plug Flow Reactor Continuous Stirred Tank Reactor

(CEY, Armfield - ISSUE 15 July 2013) (CEM-MKII, Armfield - ISSUE 20, September 2013)

General overview

A. PFR:

Tubular reactors are often used when continuous operations are required. In a tubular reactor,
the feed enters at one end of a cylindrical tube and the product stream leaves at the other end.
Ideal Plug flow reactor (PFR) is a type of tubular reactor in which the composition of the fluid
varies from point to point along a flow path. It has no variation in concentration in the radial
direction and no mixing between differential elements of volume. For plug flow reactors all
fluid elements take the same length of time to travel from the reactor inlet to the reactor outlet.
Deviation from the ideal flow pattern can be caused by channeling of fluid, by longitudinal
mixing caused by vortices and turbulence, by recycling of fluid, or by creation of stagnant
regions in the vessel.

Reactors can be characterized by a number of parameters:

τ - the ratio between the useful reactor volume and the feed flow rate

RTD, E(t) - residence time distribution function

F(t) - the cumulative distribution function

t m or t - mean residence time

σ2 - variance

The RTD can be determined experimentally by tracer techniques or evaluated using

mathematical models. Tracer techniques use several perturbations in the inlet of the reactor and
wait for the reactor response. The most common perturbations used in a plug flow reactor are
Step change and Pulse change. The perturbations use tracer solutions containing a detectable
agent that can be measured/visualized and therefore followed. This allows a full comprehension
of the reactor behavior.
 The tubular CEY reactor is packed with glass beads. It has a RTD that is very similar to that of a
plug flow reactor, but with some axial dispersion. To describe the CEY reactor, a non-ideal
tubular reactor, the dispersion model can be used, in which an axial dispersion of material
exists as result of molecular and connective diffusion. The parameter that measures the extent of
axial dispersion is the vessel dispersion number, D . For small extents of dispersion the
ul
spreading tracer curve does not significantly change in shape as it passes the measuring point
(figure 1 and 2). The residence time data can be obtained by tracer experiments, so the
parameter in the model can be evaluated and predictions of conversion and exit concentrations
in non-ideal reactors can be made.

Figure 1: Residence time distribution curves for Figure 2: Effluent response curve for Pulse
Step experiment for dispersion model. (Adapted experiment for dispersion model. (Adapted
from reference No. 6) from reference No. 6).

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 Useful equations 3,6,8:

The RTD function E(t) can be determined directly from a Pulse experiment 3,6:

The cumulative distribution F(t) can be determined directly from a Step experiment for positive
change 3,8:

Cout is the concentration at the reactor outlet at time t and C0 is the feed tracer
concentration. When the step change is done by water, Fnegative(t)=1-Fpositive(t).

B. CSTR:

The continuous stirred tank reactor (CSTR) in the form of either a single tank or (more
often) tanks in series. It is used widely and is particularly suitable for liquid phase reactions.
Advantages include consistent product quality, straightforward automatic control and low
manpower requirements. In an ideal CSTR the reactor is perfectly mixed, so the concentration
of any substance in the effluent stream is identical to the concentration throughout the reactor.
The concentration of tracer in the effluent at any time t, is: )C0 is the
concentration of the input).4 When performing a step experiment and assuming the mean
residence time is equal to the space-time, the following equation should be used:
 t

C (t )  C0 1  e tm  .
 

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Make sure you understand the following prior to the lab: CSTR, PFR,  , E (t ) , F (t ) , tm ,  2 ,
Pulse and Step tracer experiment (ideal versus non-ideal reactors), the dispersion model and Peclet
number, relationship between conductivity and concentration, differences between CSTR and PFR.

References:
1. Fogler, H. Scott. "Elements of chemical reaction engineering", 3rd. ed., pp.11,
Prentice Hall PTR, New Jersy, (2001).
2. Ibid, pp. 57.
3. Ibid, pp. 812-823.
4. Ibid, pp. 829-830.
5. Ibid, pp. 877.
6. Ibid, pp. 885.
7. Hill, Charles G. Jr. “Introduction to chemical engineering kinetics and reactor design”,
pp.262-264, John Wiley & Sons, Canada, (1977).
8. Ibid, pp. 398-400.

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A. Equipment unit Overview – CEY Plug Flow Reactor

1. General:
The Armfield CEY Plug Flow Reactor is an example of an ideal tubular reactor. It is designed
to demonstrate the mechanism of chemical reactions and flow pattern in continuous flowing
systems. A tubular reactor packed with glass beads has a Residence Time Distribution that is
very similar to that of a plug flow reactor, but with some axial dispersion.
The unit consist of the following components, ordered by the material flow: two reagent
bottles and pumps 6 port injection valve  static premixer  reactor column  sensor
block with conductivity and temperature probes  drain.
Figures 3 and 4 present the Plug Flow Reactor Unit diagram. The conductivity and
temperature probes enable monitoring the reactions. In addition, all the experiments
performed in the CEY unit are followed visually by means of the reactor transparency and the
use of color indicators.

Reagent bottles
CEY reactor

Injection
valve

Figure 3: Front View of Plug Flow Reactor Unit

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 Figure 4: flow path from the reagent bottles to the 6-port injection valve.

2. Injection valve:
The injection valve has 6 ports and two positions. In one position adjacent ports are linked
together inside the valve so that there are 3 pairs of linked ports. Changing the position of the
valve links the alternate port pair together (figure 5). The function of the valve is to inject a
tracer solution (colorful solution) in a defined volume ratio. This is achieved by using a tracer
solution loop of defined lengths. When the injection valve is in the load position the tracer
solution loop is filled. Tracer solution passes out of the injection valve and it is recirculated.
Carrier liquid (water) is directed to the reactor. When the injection valve is switched to the
injection position the carrier liquid (water) push the tracer solution (dye) contained in the
loop I into the reactor.

Figure 5: Injection valve positions

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3. CEY reactor:
The plug flow reactor (figure 6) is an acrylic column with a total volume of 1 L. It is packed
with 3mm glass beads to give plug flow with axial dispersion and improve flow distribution.
At the bottom of the reactor a static premixer with a total volume of 1.6 mL is located. It is
packed with glass beads of 1.2 mm in diameter to thoroughly mix the reactants before
entering the reactor. To avoid movement of the glass beads there are four meshes, which are
located at the ends of the reactor column and the static premixer.
Temperature and conductivity probes are fitted into the sensor block which is located at the
top of the stand, so measurement of the materials exiting the column are monitored.

Figure 6: CEY Plug Flow Reactor Unit

4. The software (CEXC software):

The CEY reactor is controlled using a software which allows real-time monitoring and data
logging of all sensor outputs and control of the pumps. The Mimic Diagram screen in the
software shows all the sensor outputs, and controls for the pumps, according to the
experiment that is carry out (figures 7-8)

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 Pumps operation: Feed pump speeds are controlled using up/down arrows or typing the
flow (ml/min) in each window for each pump. Click on the appropriate POWER ON
symbol to start up the pumps.

 Data acquisition: Conductivity and temperature values will be monitored on the screen
and the data logged when ‘GO’ is clicked. Recorded results can be displayed in tabular

and graph format by pressing: .

Figure 7: Pulse experiment screen

Figure 8: Step experiment screen

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B. Equipment unit Overview –Continuous Stirred Tank Reactor

1. General:
The Armfield CEM MkII Continuous Stirred Tank Reactor is designed to demonstrate the
mechanism of a chemical reaction in this type of reactor as well as the effects of varying the
process conditions such as reaction temperature, reactor volume, stirring rate, feed rate etc.

The flow of materials is as follows. Two feed pumps, on the service unit, separately pump the
chemical reagents from the two feed bottles into the reactor through connectors in the base of
the reactor. As reagents are pumped into the reactor, the level increases until it finally
overflows the stand pipe and flows to the drain. The conductivity and temperature probes
enable monitoring the reactions. Figures 9-10 present the CSTR Unit diagram.

Hot water
circulator
Reagent bottles

Figure 9: CEM MkII Continuous Stirred Tank Reactor

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 Figure 10: CEM MkII Continuous Stirred Tank Reactor diagram

2. CEM reactor:
The CEM CSTR diagram is presented in figure 11. The reactor has a maximum volume of 2
Liters and minimum of 1 Liters.
A stainless steel coil inside the reactor provides the heat transfer surface for either heating or
cooling the chemical reactants for exercises above ambient temperature. A stirrer (turbine
agitator) works in conjunction with a baffle arrangement to provide efficient mixing and heat
transfer. Glands in the reactor lid house the conductivity and temperature sensors. The larger
of the two glands is for the conductivity probe. The glands are unscrewed by hand, the probes
inserted completely into the reactor until they rest on the reactor base and then the glands re-
tightened. The working volume of the reactor is determined by the height of the stand pipe,
which can be adjusted by loosening the hexagonal gland nut. A mark is etched onto the stand
pipe so that for maximum operating volume of the reactor, it should be aligned with the gland
nut. A stop prevents the stand pipe from being completely removed, and this also defines the
minimum working volume which is half the maximum volume.

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 Figure 11: Diagram of the reactor unit

3. The CEM software and data logger:

The Continuous Stirred Tank Reactor is controlled using a software, which allows real-time
monitoring and data logging of all sensor outputs and control of the heater, stirrer and pumps.
The equipment is controlled from the Mimic Diagram screen in the software. This shows all
the sensor outputs, and includes controls for the pumps, stirrer and hot water Circulator. The
mimic diagram screen is presented in figure 12.

 Recorded results can be displayed in tabular and graph format by pressing: .

 Pumps, stirrer and hot water circulator operation: Click on the POWER ON symbol to
operate this systems. Feed pump speeds are controlled using up/down arrows or typing
the flow (ml/min) in each window for each pump (maximum 150 ml/min). The volumetric
ratio in which the reactants are mixed is defined by the relative flow rates of the two
pumps. The degree of mixing may be adjusted using the agitator speed control box on the
main screen of the software.

 Data acquisition: Conductivity and temperature values will be monitored on the screen
and the data logged when ‘GO’ is clicked.

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 Figure 12: Mimic diagram and software screen

Safety

It is essential to wear protective clothing, gloves and safety spectacles when handling chemicals
during the experiment.

While using the system it is possible that there will be some spillage and splashing - all users
should be made aware that they may be splashed while operating the equipment, and should
wear appropriate clothing and non-slip footwear.

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C. Experimental procedures

Three experiments will be carry out using the CEY PFR and the CEM CSTR units:
 Exercise A – PFR Flow pattern characterization by a step change.
 Exercise B – PFR Flow pattern characterization by a Pulse change.
 Exercise C – CSTR Flow pattern characterization by a step change
Final report requirements are detailed in the end of each experiment and are additional to those
published in the course website.

General preparations:
 Prepare 400 mL of a concentrated tracer solution containing 1 M Potassium Chloride and
0.1% (%w/v) of Indigo Carmine. Fill the indicated reagent bottle with 200 mL concentrated
tracer solution.
 Prepare 2 Liters of 0.1 M Potassium Chloride containing 0.01% (%w/v) of Indigo Carmine,
by a 10-fold dilution of 200 mL concentrated tracer solution. Fill the indicated reagent
bottle with the diluted tracer solution.
 Prepare 3 Liters of 0.1 M Potassium Chloride and fill the indicated reagent bottle.
 Fill two reagent bottles with 2 Liters of distilled water each.
 All the calculations should be prepared in advance to the lab and presented to the
teacher assistant.

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1. Exercise A - Flow pattern characterization by a step change:
1.1. Objective
To study the flow pattern characterization of a tubular reactor packed with glass beads.
This will be achieved using a model considering a plug-flow reactor with axial
dispersion and by determination of the RTD.
1.2. Method
The study of flow pattern in a reactor is done by using Step change tracer technique.
Colored tracer solution is used in order to make the propagation of the concentration
wave visible.
1.3. Chemicals
2 Liters of distilled water
2 Liters of 0.1 M Potassium Chloride containing 0.01% (%w/v) of Indigo Carmine
1.4. Procedure
 Start the software and choose the Step Experiment option.
 Position the reagent bottles: bottle 1 with the diluted tracer solution, and bottle 2
with distilled water. Make sure to refit the lids.
 Arrange the experimental assembly in accordance with Figure 13. Notice that T
connector that is supplied with the unit is connected.
 Take the feed pipe from the reagent bottle 1 and introduce it into reagent bottle 2, so
that both pumps pump the same solution into the reactor (water).

Figure 13: layout Step experiment

 Type the flow rate in the software 50ml/min in each window for each pump so that
the total flow rate of the solution entering the reactor will be 100ml/min.
 Switch on the pumps by pressing POWER ON.

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  Water should be streamed in the system. Continue to stream water until you make
sure that there is no leakage from either the connections or probe box, , no
bubbles seen in the tubing, and the conductivity measurement corresponds to
that of distilled water.
 Switch off the pumps by re-pressing POWER ON.
 Take the feed pipe from the reagent bottle 2 and introduce it into reagent bottle 1, so
that both pumps pump the same solution into the reactor (tracer solution).
 Set data collection of conductivity at 3 seconds intervals using the software by
opening the “Sample” menu”  “Configure”.
 Switch on the pumps by pressing POWER ON and start the data logger program by
pressing ‘GO’ . Recorded results can be displayed in tabular and graph format

by pressing: .
 Measure the time it takes the solution to reach the reactor (column) and the time it
takes from the exit of the reactor until the detector. The recorded times will allow
estimation of the reactor space time and the space time in the connection tubes.
 Tracer solution should be streamed in the system and collection of data should
continue until steady state conditions are reached in the reactor with the conductivity
measurement corresponding to the solution concentration. This takes approximately
30 minutes.
 Once steady state is reached, turn off the peristaltic pump by re-pressing POWER
ON and change the tubes from vessel 1 to vessel 2 with water and turn on the pump
again.
 Switch on the pumps by pressing POWER ON and start the data logger program by
pressing ‘GO’. Take note of the time in system clock at which this change has
been done – it is important for the data analysis following.
 When the conductivity logged is approximately 0.001 mS and stable, stop the
experiment and the pump.
 Save the data obtained in XLS format.
 Repeat this procedure with different flow rate - 75 mL/min for each pump.
Open a new sheet in the recorded result table by clicking “Sample””Next
Results”.
1.5. Final report requirements
 Perform all calculations for each flow rate separately, and compare between them
afterwards.
 Plot the Step change graph of F(t) by using the experimental conductivity data. Make
sure to refer as time=0 to the measurement that was taken when the Step change has
been done and reached the reactor inlet, by eliminating the tubing time (i.e. when

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 water entered the reactor instead of the tracer solution). Explain the use in the
conductivity values in the equations.
 Calculate the F(t) values according to the dispersion model:
o Note that the theoretical model is for a positive step change, were in the
current experiment water were used to perform the change.
uL
o t * and are unknown and will be found through the model equation using the
D
uL
solver function of EXCEL. Make up a table in the data file with t * and .
D
o At this point Plot a column with RTD function F(t) for each time point by
uL
including a reference to t * and cells in the equation, although they are
D
unknown at this stage.
o In order to use the solver function, set in the SQD cell of your table the function
SUMXMY2 selecting the columns of the experimental F(t) and the model
equation, which means will sum the squares of the differences between these two
columns (experimental and model curves).
o Then, go to the Solver function and in “set target cell” select SDQ cell; in “Equal
to” select “Min” with value 0.1, which means minimization of this value. In “by
changing cells” select the cells of the two missing variables on the table built.
uL
o Press Solve bottom, t * and will be found, as well as the unknown columns.
D
o Plot the Step change graph of the model equation vs. time on the same graph you
have plotted the experimental data and compare them. Explain their shape and the
source for the difference between them.
o Plot the Step change graph of the experimental data on the same graph for both
flow rates (50 and 75 ml/min) and compare them. Explain the difference between
them by using the values of the Pe numbers and residence times in each flow rate.

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2. Exercise B - Flow pattern characterization by a Pulse change:
2.1. Objective
To study the flow pattern characterization of a tubular reactor packed with glass beads.
This will be achieved using a model considering a plug-flow reactor with axial
dispersion and by determination of the RTD.
2.2. Method
The study of flow pattern in a reactor is done by using the Pulse change tracer
technique. Colored tracer solution is used in order to make the propagation of the
concentration wave visible.
2.3. Chemicals
2 Liters of distilled water
200 mL of 1 M Potassium Chloride containing 0.1% (%w/v) of Indigo Carmine
2.4. Procedure
 Start the software and choose the Pulse Experiment option.
 Position the reagent bottles: bottle 1 with the concentrated tracer solution, and bottle
2 with distilled water.
 Arrange the experimental assembly in accordance with the Figure 14. Notice that T
connector supplied with the unit is not necessary in this case.

Figure 14: layout Pulse experiment

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  Empty water remnants from the flow path of pump 1 to avoid dilution of the tracer
solution. Make sure to place the corresponding tubes in another container to prevent
dilution of the reagents.
 Verify the directional position of the six port injection valve so that water is pumped
into the reactor and tracer solution is being recirculated. , i.e. the loading position.
The loop will contain the colored solution. (When switching the injection valve from
one position to another, turn the handle of the valve until it clicks to be sure that
connections between ports have been done properly. Otherwise, ports will be
blocked, pressure will increase and pipe will split plashing with the solution
contained.)
 Set data collection of conductivity to 3 seconds on the software from the “Sample”
menu”  “Configure”.
 Place the tracer tubes back in the reagent bottle.
 Type the flow rate in the software 50ml/min in each window for each pump.
 Switch on the pumps by pressing POWER ON.
 Once a steady state is reached (no bubbles in the reactor and conductivity
corresponding to that of distilled water) and the loop has been loaded with tracer –
stop the pumps.
 Switch the injection valve position to injection position. Then, start data acquisition
by pressing ‘GO’. At the same time switch on the water pumps by pressing POWER
ON. Take note of the time at which this has been done. The solution inside the loop
(tracer) will be injected into the reactor.
 Take note of the time the solution takes to reach the reactor (column). The recorded
time will allow estimation of the reactor space time and the space time in the
connection tubes.
 Finish the experiment when the conductivity is approximately 0.001mS
 Click again ‘POWER ON’ to finish the experiment. Stop data logging.
 Repeat this procedure with different flow rate - 75 mL/min for each pump.
Open a new sheet in the recorded result table by clicking “Sample””Next
Results”.
2.5. Final report requirements
 Perform all calculations for each flow rate separately, and compare between them
afterwards.



 Calculate C (t )dt , residence time and the variannce according to the experimental
0

data. In order to solve the definite integrals, use an approximation based on the
trapezoidal rule technique. Note: in case the base line of the graphs isn't 0, you
should eliminate this time points when performing the calculations, and relates only

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 to the values in the peak area. Non-zero values can change the RTD function and
affect the calculated values.
 Plot the Pulse change graph of E(t). Make sure to refer as time=0 to the
measurement that was taken when the Step change has been done and reached the
reactor inlet, by eliminating the tubing time (i.e. when tracer solution entered the
reactor instead of the tracer solution).
 Compare between the calculated values and the experimental data.
2
 Calculate the ratio . Use the disperssion model formula and use the EXCEL solver
tm2
function to find Peclet number. The formula should refer to a cell indicated as Peclet
number. When using the Solver function, select in “set target cell” the cell
2
containing the formula; in “Equal to” type the value generated for the ratio ; and
tm2
In “by changing cells” select the cell of the missing Peclet number.
 Press Solve, and Peclet number will be found.
 Plot the Pulse change graph of the two flow rate on the same graph. Explain their
shape and the source for the difference between them. Relate to the residence time
and Peclet numbers.

The trapezoidal rule technique:

The trapezoidal rule technique can be used for approximating definite

integrals, according to the following steps:

1. For each time point i, calculate the function inside the integral by
insert a formula in a new column in the Excel datasheet.
2. For each two time points, I and i+1, plot the “mean point” column,
which is the area of the trapezoidal between this two time points and
the function. For example, if the function is E(t), then:

.
3. Plot the “accumulative sum” of the mean points. This is how the integration is performed



using the sum of the different trapezoids: E (t )dt .
0
In details, for each time point i, the accumulative sum is the sum of the “mean point” from
time point 0 until time point t=i.

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3. Exercise C - CSTR:
3.1. Objective
Study the flow pattern in CSTR.
3.2. Method
The study of the residence time in a reactor is done by using a Step change with a
tracer solution.
3.3. Chemicals
2 Liters of distilled water
3 Liters of 0.1 M Potassium Chloride.
3.4. Procedure
 Start the software and choose the experiment with heater option.
 Fill and Position the reagent bottles.
 Arrange the experimental assembly. Make sure the CSTR feed tubes are connected
properly to the pumps.
 Gently transfer the conductivity and temperature sensors to the CSTR.
 Set the reactor stirrer to a speed of 50% and press ‘Power on’ button to start it up.
 Start the water feed pump by setting the pump speed control to 100 ml/min in order
to fill the reactor to the overflow as quickly as possible. When the reactor is full and
the conductivity is below 0.05mS, stop the feed pump. If the conductivity is high,
continue streaming water until the values drop.
 Set the data collection interval to 3 seconds press GO to start data acquisition and
immediately start the KCl solution feed pump by setting the pump speed to 100
ml/min. The conductivity of the reactor contents will begin to increase.
 After approximately 30 min, stop the pump and drain the reactor completely.
 At the end of the experiment fill the reactor with water again in order to clear the
reactor of KCl residue and Empty the reactor.
3.5. Final report requirements

C 
 Plot  vs. time and explain the shape of the graph. Compare it to the graphs
C0  0
obtained during the step change in the PFR.
 The residence time tm should be found graphically, by the equation given in the
theoretical section and applying ln function on it.
 Compare the resulted residence time value to the theoretical result obtained from the
Vreactor

formulation: Flowrate . Explain the differences.

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