CPE5005-B

Reaction Engineering

Tubular Reactor Lab experiment

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 Contents
• Background information to Tubular Reactors
• Aims of the tubular reactor experiment
• Experimental materials and set-up
• Saponification applications
• Experimental steps
• Data collection
• Data analysis
• Calculations
• Report

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Background information to Tubular Reactors
• Provide continuous inflow and outflow of materials (i.e. in continuous
processes).
• 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 prevents complete
mixing of the fluid in the tube:
• the properties of the flowing stream will vary from one point to
another, namely in both radial and axial directions.

Ideal tubular reactors referred to as a plug flow reactor (PFR).

Key assumptions:
 the fluid is perfectly (completely) mixed in the radial direction but no
mixing in the axial direction, i.e., the direction of flow
 the reactor has a fixed residence time: Any fluid (plug) that enters the
reactor at time t will exit the reactor at time t +τ , where τ is the
residence time of the reactor.
 a uniform velocity profile across the radius.

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 Aims

• introduce the concept of a tubular reactor operating under isothermal

conditions (i.e. constant temperature of 30oC in the reactor),

• determine the reaction rate constant (k) under isothermal conditions,

• effect of residence time (t) on conversion of reactants (X) at:

 Three different sets of reactants flowrates (50,70,90 cm3min-1), which
will give a different residence time (t) per different set of reactants
flowrates, therefore affecting the conversion of the key reactant (sodium
hydroxide) and that of the sodium acetate (product).

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 Experimental materials and set- up
• The reaction explored for the aims described above regard the saponification of 0.1 M Ethyl
Acetate (CH3COOC2H5) with 0.1 M Sodium Hydroxide (NaOH), producing ethanol (C2H5OH)
and sodium acetate (CH3COONa) :
CH 3COOC2 H5 + NaOH ® CH 3COONa +C2 H5OH
• Bottles of 2.5 litres of 0.1 M Ethyl Acetate (CH3COOC2H5) with 0.1 M Sodium Hydroxide
(NaOH) are already prepared for you. You should keep an eye on refilling the feeding bottles
to the reactor between switching to different flowrate runs as you need to avoid (i) the
discontinuity of the feed and (ii) create bubbles in the reactor, i.e. that can further hinder the
already “imperfect” mixing (see slide 3), also potentially leading to “missing” the steady state
conditions seen graphically through the software.
• Description of the materials, execution of the experiment at the three different flowrates of
the reactants, reactor and the theory of the aims (as seen in the previous slide) are found
between pages 5 and 7, as well as in Appendix A in the lab handbook for the “Tubular reactor”
on Canvas.

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 Experimental materials and set- up
conductivity probe and the temperature sensor

Hot water at 37oC surrounding

the reactants’ tube (reactor’s
jacket) Reactants & products at 30oC

Water input

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 Experimental materials and set- up
Reactor at 30oC

Peristaltic pump Unreacted reactants

feeding Sodium and formed products
Hydroxide

Water tank feeding

the reactor’s jacket
Reactants’
flowrate per set

Hot water at 37oC Peristaltic pump Peristaltic pump

surrounding the reactants’ feeding Ethyl Acetate Heating coil to keep the feeding Hot water at
tube (jacket) reactor’s temperature 37oC
constant

Armfield software interface for controlling the experimental parameters

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 Saponification applications

Both products of the studied saponification reaction find a wide range of

applications in the petroleum, textile, cosmetics, and paint industries.

e.g.

• saponification is used in the textile industry to remove insoluble calcium

salts;

• in the paint industry, it is used to intensify colors.

Also, used in the food industry as a tampon and protector:

 very significant role as tampon in haemodialysis.

In the leather industry, it is used in the neutralization of mineral acids.

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 Experimental steps

• Firstly you need to calculate the corrected flowrates to achieve 50,70 and 90
cm3min-1 per run based on the “Peristaltic pump calibration data” found in
appendix A in the lab handbook for the “Tubular reactor” on Canvas.
• The software is then initialised with the “experiment with heater” option being
selected.
• The water vessel, that feeds the jacket of the reactor is filled past the overflow level
to ensure that enough water is circulated.
• The Grant GD120 reactor jacket is then switched on and set to be at 37°C to result
in the constant temperature in the reactor.
• The concentrations of the reactant solutions are typed into the software interface,
once the temperature within the reactor reaches a steady point (of 30oC).

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 Experimental steps
• The pumps are activated by typing the desired flowrate into the software
interface. We start with the desired feeding flow rate at 50 cm3min-1 aka based
on the corrected calculation e.g. “52 cm3min-1”.

• Once the pumps are turned on, the data logger is started and the software logs
the conductivity of the reactants and products.

• The experimental data used for the calculations are at steady state: when the
data observed on the graph are seen to ‘level-off’ and conductivity begins to
decrease gradually indicates that steady state conditions were achieved and that
the first run is completed.

• Make sure that you save the data of each flowrate run before you move on to the
following flowrate run, by giving a unique name to the saved file.
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 Experimental steps

• The piping is cleaned by passing water via the pumps through the reactor’s
tubing to ensure no left overs from the “50 cm3min-1” (1st run) are found when
the 70 (2nd run) and 90 cm3min-1 (3rd run) tests are started.

• Also, the piping needs to be primed (filled in) with the 0.1 M Ethyl Acetate
(CH3COOC2H5) and 0.1 M Sodium Hydroxide (NaOH) before the second and
third runs start.

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 Data collection
• After finishing all three runs (at 50,70 and 90 cm3min-1) you can export all data
per run, to an excel file.

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 Data analysis
Please, pay attention to the respective values you choose from the collected data to
calculate for :

L to be used in 1 calculation

Lc to be used in c1 calculation

L0= L0 = 0.195[1 + 0.0184(T - 294)] 0 to be used in 1 and c1 calculations

∞= 0

c∞= 0 if b0≥0

c∞= b0 if b0<0

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 Data analysis
Error analysis

Instrumentation and equipment used, carry inaccuracies in their measurements and

operations given:

o Temperature probe ±oC or % accuracy

o Conductivity probe ±Siemens/min or % accuracy

o Peristaltic pump ±cm3min-1 or % accuracy

Such inaccuracies perpetuate to our calculations leading to errors (%) in calculations.

These errors should be determined and calculated in your data analysis and calculations.

Same analysis should be made in your professional activities as instrumentation and

equipment in the industry will have the same effect or even when testing a new process at
lab scale.

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 Calculations
Data recording at steady state (taking approximately 25- 30 minutes
after the beginning of the each run at the three, different flowrates
for the reactants).
Note:
1. In the recorded data, the conductivities (L, Siemens/ cm) of
sodium hydroxide (NaOH) and sodium acetate (CH3COONa)
should be related to the concentrations of sodium hydroxide (0,
1 of NaOH) at times zero (0) and “t” and sodium acetate ( c1, c∞
of CH3COONa) at times “t” and “∞” : see equations on pages 10
and 11 in the lab handbook for the “Tubular reactor” on Canvas.
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 Calculations
2. Then, you use 0, 1 of NaOH and c1, c∞ of CH3COONa to
calculate the conversion of NaOH (X) and that of CH3COONa
(Xc) : see equations on page 11 in the lab handbook for the
“Tubular reactor” on Canvas.

3. Correction: on page 10 in the lab handbook for the “Tubular

reactor” on Canvas a0 and b0 refer to the initial concentrations (in
the feed) 0 and b0 of NaOH and CH3COOC2H5 respectively.

4. Plotting X/(1-X) vs time will give you km ; therefore the

reaction rate constant k could be calculated.

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 Calculations
5. Effect throughput (aka different flowrates tested) on conversion
can also been determined as explicitly described on pages 12 and
13 in the lab handbook for the “Tubular reactor” on Canvas.

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 Report
The report structure could be as follows:

• Contents

• List of tables

• List of figures

• List of equations

• Introduction

• Background information (e.g. uses in the industry for both the (continuous) plug flow
reactor and the reaction under study including their literature review. Also, for example
what the expected order is, the rate constant of the particular reaction in a plug flow
reactor under the same experimental conditions of pressure and temperature).

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 Report
• Experiment

 Methodology (please, try to avoid copying and pasting available information as e.g.
found in the lab handbook)

 Process Flow Diagram (PFD)

 Experimental set-up and procedure (please, try to be concise)

 Health and safety considerations

• Results

 Sample calculations based on the equations provided in the lab handbook (please,
present your calculated outcomes in figures, graphs and tables as necessary).

 Please, include here your error analysis as described earlier to further support your
discussion (following section of the report).

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 Report
• Analysis and Discussion

 What is your analysis based on the calculated results for k, overall mass balance,
throughput (graphs, tables, figures) as presented in the “Results” section?

 Could you enhance and support your discussion based on relevant literature?

• Sustainability

 What are the parameters that need to be considered for the sustainability of a process by
using a plug flow reactor?

 How could the tested operation become sustainable e.g. based on “effect of throughput
on conversion”?

• Conclusions

• Appendix

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 Report
• References

 Please, make sure you use a wide range of sources to support your report at different
sections: do not use only websites; you can use instead, textbooks, lecture notes,
scientific articles etc.

 Please, also do not use only one reference in a paragraph or a section; you should show
you are well informed.

 Finally, use the Harvard referencing system to write your references and cite them
accordingly in your report ( discussion, background information etc. as well as any
figures taken from the literature). If you present a table or a graph taken from the
literature and you have not produced it, you should refer to it as a “figure” and cite the
reference used.

Good Luck!
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 Thank you

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