TABLE OF CONTENTS

Contents 1. Abstract 2. Introduction 3. Objectives 4. Theory 5. Materials and apparatus 6. Methodology 7. Results 8. Discussion 9. Conclusions 10. Recommendations 11. References 12. Appendix

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1.0 ABSTRACT This experiment is mainly conducted to know the effect of pulse input to the Continuous Stirred Tank Reactor (CSTR) in series and in the same time to know how the CSTR operated. in this experiment, it consist of three CSTR tank in series. Initially Tank 1 is filled with salt solution while tank 2 and Tank 3 is filled with deionized water.Then the pump P2 is switched on in order to fill all the three with

deionized water and the flowrate F1 is set to 150ml/min. Then, the deionized water is pumped for 10 minutes and the conductivity is recorded at stable low values. Then the pump P2 is switched off for 5 minutes and pump P! is switched on for 5 minutes. Then pump P1 is switched off and the pump P2 is switched on back and every three minutes, all the conductivity values for three reactors are recorded. Then graph of Conductivity values for all three reactors is plotted against Time. From the graph , it shows that the C(t) curve response similarly to the transient behaviour of CSTRs in series of pulse input as the experiment is carried out in pulse input manner. The residence time at which feed stay in each tank causes increasing, maximum and decreasing of its concentration in time interval. The residencetime distribution analysis can be done to describe this non-ideal reactor in terms of its efficiency.

2.0 INTRODUCTION

CSTR In Series (Model: BP 107) is designed to introduce students of Chemical Engineering on the dynamic behavior of reactors in series. The unit is based on the simplest classic case of a well-mixed, multi-staged process operation that basically consists of three reactors connected in series by piping. The solution in each reactor is well stirred and the concentration can be measured. Other equipments provided along with the unit including sump tanks, feed pumps and also instrumentation (Solution Engineering Sdn. Bhd.). Continuous stirred tank reactor (CSTR) is also known as flow reactor. In ideal continuous stirred tank reactor, mixing is complete and the reactant concentration and temperature are the same everywhere in the reacting mixture. Consequently, the composition of the exit stream is the same as that of the reactant mixture. As a result of mixing in a continuous stirred tank reactor, material that enters at one moment may be anywhere within the reactor at the next and may indeed be in the fluid leaving the exit stream. This effect is called by-passing means that the range of residence times is very large, though it is still possible to define a mean residence time. Several tank reactors are often operated in series or cascade as shown in figure below. In that way, the disadvantages of the relatively low reactant concentration on the one hand, and by-passing on the other, may be partially off-set. As the number of tanks increase in series, the performance of the complete system approaches that of a plug-flow reactor and, in the limit of an infinite number of tanks, becomes equal to it (Bamford, Tipper & Compton, 1985). Basically, CSTR is run at a steady state and its main feature is the complete uniformity of concentration and temperature throughout the reactor due to its perfect mixing. Other than that, the concentration and temperature of material leaving the tank must be the same as the material present inside the tank. Currently, CSTR is widely used in large-scale production, whereas the batch processing is preferred in case of small-scale operation. Moreover, continuous operations results in more consistent product properties and have a high productivity through the reduction of inactive periods such as filling, heating and cooling compared to the batch processing. Furthermore, the book also stated that it is necessary to understand the dynamic characteristics to ensure the successful operation of a continuous stirred tank reactor. The realistic process model can predict the dynamic behaviours of a plant. If there are any fault occurs in plant, therefore it may happen due to the discrepancy between model predictions and plant outputs (Jana, 2008).

3.0 AIMS To determine the concentration that response to a pulse input. To determine the effect of pulse input method towards the experiment. To understand the working mechanism of CSTR in series.

4.0 THEORY

CSTR, also known as Continuous-Stirred Tank Reactor is a type of reactor commonly used in industrial processing. This type of reactor, also referred as vat or back mix reactor is primarily used for liquid phase reaction, usually operated at steady state with continuous flow of reactant and product, and assumed to be perfectly mixed. Hence, there is no time dependence or position dependence of the temperature, the concentration or the reaction rate inside the CSTR. Every variable is the same at every point inside the reactor. Since the temperature and concentration are identical everywhere within the tank, therefore they are the same at the exit point as they are in the tank.

Figure 1 CSTR mixing patterns (Fogler, 2006)

General mole balance equation : Assume steady state, where : (1)

And well mixed, therefore : Rearranging the equation : (2) Deriving the equation :

(3) In reactor sizing, one can measure the size of desired reactor based on the given rate of reaction as a function of conversion X, -rA = f(X). As shown in the Levenspiel Plot below, the volume of a single desired CSTR is represented as the area under the curve.

Figure 2 Levenspiel Plot of CSTR

(University of Michigan,retrieved from internet 2013)

As for the reactor in series, one can design a sequence of CSTR desired based on the same equation of rate of reaction as a function of conversion given, provided that there are no side streams by defining the overall conversion at any point.

Figure 3 CSTR in series (University of Michigan ,retrieved from internet 2013) Mole balance on Reactor 1 : In Out + Generation = 0 FA0 FA1 + rA1V1 = 0 FA0 FA0 (1-X1) + rA1V1 = 0 FA0 FA0 + FA0X1 + rA1V1 = 0 Rearrange the equation :

Mole balance on Reactor 2 : In Out + Generation = 0 FA1 FA2 + rA2V2 = 0 FA0 (1-X1) FA0 (1-X2) + rA2V2 = 0 FA0 FA0X1 - FA0 + FA0X2 + rA2V2 = 0 Rearrange the equation :

Introducing tracer such as salts in CSTR will help in the analysis of the transient behaviours of the series by the means of step or pulse input. The value of conductivity indicates the progression of the tracer throughout the CSTR in series. When a tracer is introduced into the reactor by step input method, the tank in series will experience a transient behaviour as shown in the figure below.

Figure 4 Transient behaviour in CSTR series to the step input (Fogler, 2006)

Meanwhile, when a tracer is introduced into a reactor by pulse input, the transient behaviour in the CSTR in series differs from the step input due to the diminishing concentration. The transient behaviour of pulse input is illustrated in figure below.

Figure 5 Transient behaviour in CSTR series to the pulse input (Fogler, 2006)

5.0 MATERIALS AND APPARATUS

1. Distillation water. 2. Sodium Chloride. 3. Continuous reactor in series. 4. Computerize system.

6.0 METHODOLOGY

In this experiment, the effect of the Pulse Input is determined by monitoring the tracer by measuring the conductivity value for all three reactors.

1. The two of the three tank which are tank 2 and tank 3 are filled up with 20L of deionozed water. 2. The salt solution in tank 1 is prepared by laboratory assistant. 3. The deionized water from tank 2 is flow to the reactor 1 when the three way valve (V3) is set at position 2. 4. The pump 2 is switched on to fill up all three reactors with deionized water. 5. The flow rate of (Fl1) is set to 150ml/min by adjusting the needles valve (V4) and the stirrers 1,2 and 3 are switched on. 6. Then, the deionized water is pumped for about 10 minutes until the conductivity reading for all three reactors stable at low values. 7. The conductivity value is recorded at t0. 8. Next, the pump 2 is switched off after 5 minutes. The valve (V3) is switched to position 1 and the pump 1 is switched on. The timer is started. 9. After the pump1 is operated for 5 minutes, the pump 1 is switched off and the three ways valve (V3) is switched back to position 2. Then, pump 2 is switched on. 10. The conductivity values for each reactor is recorded for every three minutes and continued until reading for the three reactors are closed to the starting value recorded. 11. The pump 2 is switched off and the valve (V4) is closed. 12. Lastly, all the liquids in reactors is drained by opening the valves V5 and V6.

7.0 RESULT

In this experiment, we are using Continuous Stirred Tank Reactor. The conductivity value are recorded with time interval 3 minutes. The data are tabulated in the table below :-

Table 7a: Conductivity values of each reactor respective to time Time (min) 0.0 3.0 6.0 9.0 12.1 15.0 18.0 21.3 24.0 27.0 30.0 33.0 36.0 39.0 42.0 45.0 48.0 51.0 54.0 58.1 61.0 64.0 67.0 QT1 (ms/cm) 7.5268 8.4162 5.8439 4.6100 3.1803 2.4443 1.7285 1.2790 0.9236 0.6776 0.5105 0.3844 0.2325 0.1801 0.0908 0.0720 0.0270 0.0226 0.0405 0.0345 0.0000 0.0055 0.0208 QT2 (ms/cm) 0.4563 2.7169 3.7695 4.2771 4.2715 3.9312 3.5582 2.9489 2.5648 2.0718 1.8267 1.4188 1.1744 0.8827 0.7239 0.5756 0.4307 0.3004 0.3032 0.1809 0.1512 0.1359 0.0564 QT3 (ms/cm) 0.0000 0.4343 1.1176 2.5784 2.6335 3.0936 3.2392 3.2730 3.1100 2.9065 2.6750 2.4362 2.1096 1.8843 1.5854 1.3517 1.1383 0.9156 0.8062 0.5616 0.4175 0.4068 0.3033

70.3 73.0 76.2 79.0 86.0 90.0 93.0 96.0 99.3

0.0000 0.0000 0.0000 0.0301 0.0000 0.0000 0.0000 0.0272 0.0000

0.0515 0.0231 0.0344 0.0675 0.0002 0.0167 0.0000 0.0186 0.0000

0.1952 0.1838 0.1212 0.1516 0.0856 0.0494 0.0529 0.0499 0.0000

Then, the data are plotted in the graph below :-

9 8 7 6 Conductivity (ms/cm) 5 QT1 (ms/cm) 4 3 2 1 0 0 -1 20 40 60 Time (min) 80 100 120 QT2 (ms/cm) QT3 (ms/cm)

Figure 7b: Graph of Conductivity versus Time

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8.0 DISCUSSIONS

Based on the graph plotted from the conductivity values of salt tracer in outlet of each continuously stirred tank reactors (CSTRs) in series, the trend mimic the graph of concentration vs time for CSTR series in pulse input. At low concentration of salt tracer, the outlet conductivity values is as similar as the concentration of salt passing through the outlet (Fogler, 2006). In a pulse input, an amount of tracer N0 is injected in single, sudden shot into the reactor in shortest time possible. The tracer then reside in the reactor for certain times and flow through the outlet (Fogler, 2006). The salt tracer that passed along the feed stream will be detected by the conductivity probe thus provide conductivity values. The conductivity values is equal to the concentration of salt tracer in the stream of low concentration of tracer.

In each reactor in series in pulse input, the concentration of tracer response by increasing by function of time, t. Then, it achieved peak concentration at certain time interval before dropped to concentration=0. However, first reactor registered steeper concentration in function of time graph, C(t) curve rather than second and third reactor. This is due to the lesser time of tracer that reside in reactor 1 before passing out rather than in reactor 2 and 3. The time in which tracer reside in the reactor is quantified by E(t).

The quantity E(t) is called as residence-time distribution function. The function is used to describe quantitatively how much time feed have spent in the reactor (Fogler, 2006). However, E(t) is not measured as the purpose of the experiment only to describe how much degree do the concentration response to pulse input CSTRs in series.

In pulse input, the problems usually arise on obtaining a reasonable pulse at a reactors entrance. As the reactor behaviourally different from the ideal model of CSTR, the time at which the tracer injected must be as short as possible so that the amount of dispersion between the point of injection and the entrance of tracer into reactor can be considered negligible (Fogler, 2006). The concentration-time curve plotted for each CSTR also has a long tail. These are problems as it is connected to large inaccuracies. To fix this, it is better to extrapolate the tail and analytically continue the calculation (Fogler, 2006).

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9.0 CONCLUSIONS

In conclusions the end of the experiments, students will know the effect of pulse input in CSTR.From the graph plotted, we can observe that the C(t) curve response similarly to the transient behavior of CSTRs in series of pulse input as the experiment is carried out in pulse input manner. The residence time at which feed stay in each tank causes increasing, maximum and decreasing of its concentration in time interval. The residence-time distribution analysis can be done to describe this non-ideal reactor in terms of its efficiency.

10.0 RECOMMENDATIONS Based on the experiments conducted it is highly suggested for students to: To do the start-up procedure every time they want to start a new experiments to make sure all the flow are regulated at the exact conditions to provide good reading of results To use another type of solution instead of deionized water that will increase the specific conductivity of the water in the reactors .The concentration of sodium chloride will be low enough so that specific conductivity will be linearly related to the concentration of sodium chloride. To make sure the flow rate of the flow is maintain to provide maximum flow of reaction hence give the best conductivity reading

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11.0 REFERENCES

1. R.G Compton, C.H Bamford, C. F. H. Tipper (1985), Kinetics and Chemical Energy, Elsevier Science Publishers. 2. Amiya K. Jana (2008), Chemical Process Modelling & Computer Simulation, Prentice Hall. 3. H. Scott Fogler (2006), Elements of chemical Reaction Engineering Fourth Edition, published by Pearson Education Inc. 4. University of Michigan (retrieved from internet 2013), Continuous Stirred Tanks Reactors http://www.umich.edu/~elements/asyLearn/bits/cstr/ 5. Solteq Engineering (internet 2013), Equipment for Education and Research, Continuos Stirred Tanks Reactor 6. Mathlab Central (internet 2013),Continuos Stirred Tanks Reactor http://www.mathworks.com/matlabcentral/fileexchange/32040-mpc-tutorial-iv-statespace-mpc-with-input-increment/content/html/ssmpctutorial.html

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12.0 APPENDIX

Figure 13a The set up apparatus of CSTR in series

(Solteq Engineering, internet 2013)

Figure13b Effect of Step Change Input

(Solteq Engineering, internet 2013)

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Figure 13c Effect of Pulse Input

(Solteq Engineering, internet 2013)

Figure 13d: CSTR in series (Mathlab Central, internet 2013)

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