CHEE3005 – Semester 2 2018

REACTION ENGINEERING

Experiment 1 Lab Report

P08
Fatima Abdullah – 43717695
Christie Hadwen – 44373203
Lukas Rehm – 45015939
Leif Sharkey – 43171091
1 INTRODUCTION
1.1 Background
Reaction engineering is a commonly employed concept that enables understanding and
optimisation when determining process parameters. For many commercial applications reactors
can be largely categorised as; Plug Flow Reactor (PFR), Continuous Stirred Tank Reactor
(CSTR), Batch Reactor (BR) or various combinations, despite the many design variations
applied to satisfy production requirements. As such, reactors are identified by distinctly
comparable characteristics, for example, a PFR operates with a continuous flow of reactants
passing through a cylindrical geometry where length >> radius. Compared to a BR being a
closed system generally a tank, a CSTR is an open continuous system. In practice, Doran (2012)
states that the relative performance of batch, CSTR, and PFTR reactors can be considered from a
theoretical point of view in terms of the substrate conversions and product concentrations
achieved using vessels of the same size. Despite zero-order reactions, there is no difference
between the three reactors in terms of the overall conversion rate, thus, benefits associated with
particular reactor designs or modes of operation depend on the reaction kinetics. In summary,
performance of bioreactors depends on several key aspects of their design and operation such as,
configuration, size, mode of operation (batch versus continuous, parallel versus series),
processing conditions (i.e. temperature, pH, ect.).

1.2 Aim and Objective

The aim of this experiment is to investigate how changes in the volumetric flow rate and tau
effect the conversion of reactants in Equation 1. A theoretical model will compare this effect
across the three reactors outlined in Section 1.1. Further, investigation will assess the theoretical
space-time (tau) of the CSTR against the experimentally determined resonance time.
Equation 1:
𝑁𝑎𝑂𝐻 + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻
𝐴 + 𝐵 → 𝐶 + 𝐷
The investigation will conclude by outlining how and why differences, if any, may exist between
the theoretical and experimental resonance times and assessing optimisation strategies to
increase conversion within the given experimental parameters.
1.3 Assumptions
The following assumptions will be applied to the experimental data which will be used for
calculations in Section 3.
 Steady state operating conditions with a single homogenous reaction in the bulk fluid.
 Constant thermal and physical properties of fluid and material
 Negligible heat-loss to the environment and pressure drop across the reactor
 Negligible changes in kinetic and potential energy within the reactor and flowing fluid
 Negligible concentration gradients within reactor vessel tube (well micro-mixed)
 Constant volume
2 EXPERIMENTAL PROCEDURE
Before the experiment was commenced, the
reactants were checked to ensure a sufficient
amount of each were available. The pumps were
turned to ‘remote mode’ and the outlet tube of the
reactor was focused towards the reactor drain and
closed. The reactor rig was then switched on and
hot water flow to the reactor was set temperature
to 30 °C.
Both Pump 1 and Pump 2 were set to respective Figure 1: CSTR Experiment Setup
dial numbers for the desired flowrate following
the calibration data from the Lab Manual Appendix. Pumps were switched to manual mode and
started together; to prompt simultaneous feed of both reactants to the CSTR. Reactant flows were
observed with recording of conductivity and temperature commencing immediately once outflow
was observed. Recordings were every 30 seconds for four minutes then every two minutes after,
until steady state conductivity (repeat value ± 0.01 mS/cm) was maintained. This method was
repeated three times with both reactants flows 30mL/min, 50mL/min and 70mL/min.
3 CSTR EXPERIMENTAL & THEORETICAL RESULTS
Residence time and conversion were calculated based on the CSTR design equation.
Additionally, the conversion was calculated based on the experimental results. These are
displayed in Table 1. Full calculations can be seen in Appendix 1.
Table 1: CSTR Theoretical and Experimental Results
Mean Reactant Flow Residence Time Theoretical Experimental
Experimental
Experimental Rate (min) Conversion Conversion
Order
Temperature (˚C) (mL/min) τ XA XA
Run 1
28.55 50 16 0.69 0.86
Run 2
28.3 60 13.3 0.66 0.84
Run 3
28.5 70 11.4 0.64 0.83

The calculated and measured conversions were plotted against the residence time, as shown in
Figure 1.
 1
0.9
0.8

Conversion (XA)
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
10 11 12 13 14 15 16 17
Residence Time τ (min)

Calculated Measured Linear (Calculated) Linear (Measured)

Figure 1. Comparison of Calculated and Measured Conversion

4 PFR AND BATCH REACTOR THEORETICAL CALCULATIONS

Residence times and conversions were calculated based on the PFR and Batch Reactor design
equations provided in the Lab Manual and are displayed in Table 1. Full calculations for both
reactors are seen in Appendix 1.
Table 2: PFR and Batch Reactor Theoretical Results
Reactant PFR Batch Reactor
Experimental
Flow Rate
Order τ (min) XA τ (min) XA
(mL/min)
Run 1
50 16 0.986 16 0.986
Run 2
60 13.3 0.984 13.3 0.984
Run 3
70 11.4 0.981 11.4 0.981

5 DISCUSSION
The experimental conversion in the CSTR is highest for the lowest flowrate of 50 ml/min as
shown in Table 1. This low flowrate increases the residence time, allowing the reaction to
proceed further toward completion. Upon increasing the flowrate to 60 ml/min and 70 ml/min,
the experimental conversion decreased to approximately 0.86 and 0.84, respectively.
As seen in Figure 1 and Table 1, the experimental conversions of CSTR were all significantly
greater across every flowrate compared with the theoretical conversions. The calculated
conversions were found by using the ideal CSTR model, which has many underlying
assumptions. However, these begin to break down in practical operation. Therefore, achieving
theoretical conversion would mean attempting to satisfy some of those assumptions outlined in
Table 3.
Table 3: Factors contributing to differences between experimental and calculated CSTR
conversions

Ideal Case Real Case

Micro-mixed  The mixing will not be perfect resulting in areas of different
concentrations.
 There will be inherent noise related to the pump's operation, these
Steady State fluctuations mean that at any given point it is unlikely to be perfectly
steady state. However, the average should show a steady state.
 There will be a small amount of liquid that does not mix and comes out
unreacted.
No Bypass
 There will also be a distribution of residence times as the particles take
different paths out of the reactor
Constant Volume  The stirring may result in areas stagnation. These stagnation areas will
effectively cause changes in volume.

The experimental conversions for the CSTR are higher than the calculated theoretical
conversion, which is likely due to incomplete mixing. This would cause areas of high
concentration, which would therefore have a higher yield.
A comparison of calculated reactor conversions using the same residence time found that
conversion for the PFR and batch were consistently the highest for all three residence times. In a
CSTR, the likelihood of reactants undergoing conversion decreases as the reaction progresses.
The products are formed and simultaneously mixed through the reactor volume, diluting the feed
and contributing to lower conversion values. The formation of dead zones (areas of no mixing)
and bypass streams also limit CSTR to lower conversions compared to the other two designs.

As expected, the batch and plug flow reactors yield the highest theoretical conversion of
approximately one. Since there is no flow in a batch reactor, the reactants are left in the vessel
undisturbed and react for time t until the material is removed. There are also no flow
disturbances to cause large variation in output conversion. This is the same with the PFR,
assuming no back mixing within the reactor.

The PFR consistently gave higher conversion values than the CSTR. Theoretical conversion in a
PFR should be higher than a CSTR as the reactants are not diluted and actively mixed with the
products. Thus, at the beginning of the reaction the plug flow contains presumably pure reactant.
As the plug moves along the tubular reactor reactant concentration decreases while product
concentration increases. In an ideal scenario, the product formation does little to hinder the
conversion.
While the PFR and batch reactors yield the same theoretical conversion, experimental conversion
will likely differ between the two for several reasons related to experimental set-up and operating
conditions.

When reporting on errors for this experiment which are presumed to affect results they can be
divided into two sub-classes categorised as:
Uncertainties – applicable to:
 The calibration curve used to find flow rates required for each experimental tau calculation.
 Reading the conductivity of the reactor fluid and adjusting dials for desired flowrate.

Inconsistencies – applicable to:

 Temperature control and stability of both the reactants entering the reactor and the net reactor
temperature.

Mitigating uncertainties is difficult as these are usually in-grained within the results by-way of
the operator. Best practice is applying a confidence interval to the results, however, this is out of
scope for this report. Nonetheless, inconsistencies can generally be addressed and the above
mentioned could be reduced via pre-heating the reactants before they were sent to the reactor and
accounting for the exothermic reaction of the reactor (Green and Perry, 2007).

6 SUMMARY AND CONCLUSION

After undertaking this experiment and investigating experimental reactor conversions at different
flowrates, it has become evident that experimental values can significantly deviate from
theoretical values. This can be directly attributed to the fact that concentration gradients are
present within the reactor which limits and in-turn resists the driving force of the reaction to
reach equilibrium. Comparisons of reactor types revealed that the CSTR yielded the lowest
conversions due to product build-up whereas the batch reactor and PFR had the greatest yield of
products if sufficient reaction time was allowed. They showed that maximum conversion within
time constraints was possible due to the continuous feed of reactants. Increasing accuracy of
modelling these experimental results mathematically would require reviewing some of the initial
assumptions which would add another layer of complexity to the formulas used in previous
sections.
It was found that theoretically, the batch and PFR would be the most favourable based on their
high yields, however the theoretical values calculated may differ depending on operating
conditions. Therefore, further testing into experimental yields of both batch and PFR should be
conducted to verify this conclusion.
7 APPENDICES
7.1 Appendix 1: CSTR Calculations
7.1.1 Residence Time
Reactor Volume = 1600 mL
For 50 mL/min flowrate:
𝑉 1600 𝑚𝐿
𝜏= = = 16 𝑚𝑖𝑛
𝜐𝑇 50 + 50 𝑚𝐿
𝑚𝑖𝑛
For 60 mL/min flowrate:
𝑉 1600 𝑚𝐿
𝜏= = = 13.33 𝑚𝑖𝑛
𝜐𝑇 60 + 60 𝑚𝐿
𝑚𝑖𝑛
For 70 mL/min flowrate:
𝑉 1600 𝑚𝐿
𝜏= = = 11.429 𝑚𝑖𝑛
𝜐𝑇 70 + 70 𝑚𝐿
𝑚𝑖𝑛
7.1.2 Rate Constant (units L mol−1 min−1)
Calculate k (rate constant) for each experimental temperature based on provided plot.
1
At T=28.55˚C, 𝑥 = 𝑇 = 0.0033, ln(𝑘) = −5010.6 ∗ 0.003 + 18.818 = 2.21, 𝑘 = 9.117.
1
At T=28.3˚C, 𝑥 = 𝑇 = 0.00331, ln(𝑘) = −5010.6 ∗ 0.0031 + 18.818 = 2.196, 𝑘 = 8.992.
1
At T=28.5˚C, 𝑥 = 𝑇 = 0.0033, ln(𝑘) = −5010.6 ∗ 0.003 + 18.818 = 2.21, 𝑘 = 9.117.

7.1.3 Calculate CA0

𝜐𝐴 𝐶𝐴 50 ∗ 0.1
𝐶𝐴0 = = = 0.5 𝑚𝑜𝑙/𝐿
𝜐𝐴 + 𝜐𝐵 50 + 50

7.1.4 Theoretical conversion using CSTR design equation

𝑋𝐴
𝜏=
𝑘 ∙ 𝐶𝐴0 (1 − 𝑋𝐴 )2
𝑋𝐴
16 = → 𝑋𝐴 = 0.692
9.117 ∗ 0.5(1 − 𝑋𝐴 )2
𝑋𝐴
13.33 = → 𝑋𝐴 = 0.6665
8.992 ∗ 0.5(1 − 𝑋𝐴 )2
𝑋𝐴
11.429 = → 𝑋𝐴 = 0.6475
9.117 ∗ 0.5(1 − 𝑋𝐴 )2
7.1.5 Experimental conversion using CSTR design equation
0.00975 − Λ
𝐶𝐴 = 𝐶𝐴0 − 𝐶𝐴0 ( )
0.00975 − 0.0035
𝐶𝐴0 − 𝐶𝐴
𝑋𝐴 =
𝐶𝐴0
For 50 mL/min:
0.00975 − 0.00435
𝐶𝐴 = 0.5 − 0.5 ( ) = 0.0068 𝑚𝑜𝑙/𝐿
0.00975 − 0.0035
0.05 − 0.0068
𝑋= = 0.864
0.05
For 60 mL/min:
0.00975 − 0.00449
𝐶𝐴 = 0.5 − 0.5 ( ) = 0.00792 𝑚𝑜𝑙/𝐿
0.00975 − 0.0035
0.05 − 0.00792
𝑋= = 0.8416
0.05
For 70 mL/min:
0.00975 − 0.00457
𝐶𝐴 = 0.5 − 0.5 ( ) = 0.00856 𝑚𝑜𝑙/𝐿
0.00975 − 0.0035
0.05 − 0.00856
𝑋= = 0.8288
0.05
7.2 Appendix 2: PFR Calculations
7.2.1 Residence Time
The same residence times for the CSTR experiments were used.
7.2.2 Calculate CA0
𝜐𝐴 𝐶𝐴 50 ∗ 0.1
𝐶𝐴0 = = = 0.5 𝑚𝑜𝑙/𝐿
𝜐𝐴 + 𝜐𝐵 50 + 50

7.2.3 Theoretical conversion using PFR design equation

𝑋𝐴
𝜏=
𝑘 ∙ 𝐶𝐴0 (1 − 𝑋𝐴 )
𝑋𝐴
16 = → 𝑋𝐴 = 0.778
9.117 ∗ 0.5(1 − 𝑋𝐴 )
𝑋𝐴
13.3 = → 𝑋𝐴 = 0.984
8.992 ∗ 0.5(1 − 𝑋𝐴 )
𝑋𝐴
11.4 = → 𝑋𝐴 = 0.981
9.117 ∗ 0.5(1 − 𝑋𝐴 )
7.3 Appendix 3: Batch Reactor Calculations
7.3.1 Calculate CA0
𝜐𝐴 𝐶𝐴 50 ∗ 0.1
𝐶𝐴0 = = = 0.5 𝑚𝑜𝑙/𝐿
𝜐𝐴 + 𝜐𝐵 50 + 50

7.3.2 Theoretical conversion using Batch Reactor design equation

𝑋𝐴
𝜏=
𝑘 ∙ 𝐶𝐴0 (1 − 𝑋𝐴 )
𝑋𝐴
16 = → 𝑋𝐴 = 0.986
9.117 ∗ 0.5(1 − 𝑋𝐴 )
𝑋𝐴
13.3 = → 𝑋𝐴 = 0.984
8.992 ∗ 0.5(1 − 𝑋𝐴 )
𝑋𝐴
11.4 = → 𝑋𝐴 = 0.981
9.117 ∗ 0.5(1 − 𝑋𝐴 )

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