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ABSTRACT
In this work, a reactive distillation process for the production of a fuel additive has been
modelled, simulated and controlled using proportional-integral-derivative (PID) control
method. The fuel additive considered was isopropyl alcohol that was produced from the
reaction occurring between propylene and water, with diisopropyl ether as a side product.
In accomplishing the work, the ChemCAD model of the process was first developed using
SCDS Distillation Column #1 and the fluid package employed was UNIFAC property
model. The ChemCAD column had 15 stages where the feed stream for water was the 6th
stage and the one propylene was the 10th stage; the section of the column between the two
feed streams was the reaction section of the column. After simulating the developed
ChemCAD model to convergence, it was converted to dynamic type from which the
dynamic responses of the system were generated and used with the aid of MATLAB to
develop transfer function model having the reboiler duty, the reflux ratio and the
temperature of the bottom product as the input variable, the disturbance and the output
variables of the process, respectively. The obtained transfer function of the model was used
to develop both open-loop and closed-loop Simulink models for the process that were used
to carry out the open-loop and the closed-loop simulations of the process. The closed-loop
simulation was carried out with the desire of achieving a fuel additive product with a mole
fraction of 0.97. This was accomplished using a PID controller applied inferentially via the
product temperature and tuned by trial-and-error technique. It was observed from the results
obtained that isopropyl alcohol could be produced successfully from a reaction between
propylene and water using reactive distillation suppressing the associated side reaction. It
was also found out that it is possible to control the mole fraction of isopropyl alcohol
inferentially using bottom temperature because temperature and mole fraction have been
found to be dependent on each other. Finally, it has has been shown that a reactive
distillation has been controlled to give high purity of isopropyl alcohol of approximately
0.97 mole fraction as the bottom product in the developed reactive distillation column using
the PID controller with trial-and-error tuning technique.
Keywords: Fuel additive, reactive distillation, ChemCAD, MATLAB/Simulink,
proportional-integral-derivative.
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TABLE OF CONTENTS
CERTIFICATION …………………………………………………………………………………………………iv
DEDICATION……………………………………………………………………………………………………….v
ACKNOWLEDGEMENT ………………………………………………………………………………………vi
ABSTRACT…………………………………………………………………………………………………………vii
TABLE OF CONTENTS…………………………………………………………………………………….. viii
LIST OF FIGURES ………………………………………………………………………………………………..x
LIST OF TABLES …………………………………………………………………………………………………xi
CHAPTER ONE …………………………………………………………………………………………………….1
1.0 INTRODUCTION ………………………………………………………………………………………..1
1.1 Background of Study ……………………………………………………………………………………..1
1.2 Problem statement………………………………………………………………………………………….3
1.3 Aim and Objectives………………………………………………………………………………………..3
1.6 Significant of Study ……………………………………………………………………………………….4
CHAPTER TWO ……………………………………………………………………………………………………5
2.0 THEORETICAL BACKGROUND AND LITERATURE REVIEW……………………….5
2.1 Isopropyl Alcohol (IPA) …………………………………………………………………………………5
2.2 Properties of Isopropyl alcohol ……………………………………………………………………7
2.2.1 Physical properties of IPA ……………………………………………………………………8
2.2.2 Chemical properties of IPA…………………………………………………………………..8
2.3 Uses of isopropyl alcohol………………………………………………………………………………..8
2.4 Concept of Reactive Distillation Process…………………………………………………………10
2.5 Previous Study on Reactive Distillation of IPA………………………………………………..11
CHAPTER THREE……………………………………………………………………………………………….15
3.0 METHODOLOGY………………………………………………………………………………………15
3.1 Procedures for Model Development and Steady State simulation……………………….15
3.2 Procedures for Dynamics Simulation………………………………………………………………17
3.3 Procedures for Open loop Simulation of the Process…………………………………………18
3.4 Procedures for Process Controller Tuning ……………………………………………………….19
3.5 Procedures for Simulink Modelling and Closed Loop Simulation of the Process….20
CHAPTER FOUR…………………………………………………………………………………………………22
4.0 RESULTS AND DISCUSSION ……………………………………………………………………22
4.1 Process Steady State Results………………………………………………………………………….22
4.2 Process Dynamics results………………………………………………………………………………24
4.3 Open-Loop Response……………………………………………………………………………………27
4.4 Closed Loop Response………………………………………………………………………………….29
4.4.1 Servo closed-loop response……………………………………………………………………..30
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4.4.2 Regulatory closed-loop response ……………………………………………………………..31
CHAPTER FIVE…………………………………………………………………………………………………..33
5.0 CONCLUSION AND RECOMMENDATION……………………………………………….33
5.1 Conclusion ………………………………………………………………………………………………….33
5.2 Recommendation …………………………………………………………………………………………33
REFERENCES……………………………………………………………………………………………………..34
APPENDICES ……………………………………………………………………………………………………..37
APPENDIX A…………………………………………………………………………………………………..37
APPENDIX B …………………………………………………………………………………………………..38
APPENDIX C …………………………………………………………………………………………………..38
APPENDIX D…………………………………………………………………………………………………..39
x
LIST OF FIGURES
Figure 3.1:ChemCAD flowsheet for the production of isopropyl alcohol …………………….16
Figure 3. 2: Simulink open loop model of the process ……………………………………………….19
Figure 3. 3:Closed loop model of the process with PID controllers tuned with Cohen-Coon
and Ziegler-Nichols techniques……………………………………………………………………………….21
Figure 4 1: Dynamic response of the process in form of isopropyl alcohol mole fraction
against time ………………………………………………………………………………………………………….25
Figure 4 2: Dynamic response of the process in form of product temperature against time
……………………………………………………………………………………………………………………………26
Figure 4.4: Closed loop response for a isopropyl alcohol mole fraction of 0.97 (set-point
tracking) ………………………………………………………………………………………………………………31
Figure 4 5: Closed loop response to a unit step change in reflux ratio only (disturbance
rejection) ……………………………………………………………………………………………………………..32
xi
LIST OF TABLES
Table 3 1: Cohen-Coon and Zeigler-Nichols tuning parameter expressions………………….20
Table 4 1: Column calculated parameters…………………………………………………………………22
Table 4 2: Column distillate stream properties………………………………………………………….22
Table 4 3: Column bottoms stream properties…………………………………………………………..23
Table 4.4: Controller parameters using Zeigler-Nichols and Cohen-Coon Tuning…………29
Table 4 5: Controller parameters (Trial and Error tuning)…………………………………………..30
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CHAPTER ONE
1.0 INTRODUCTION
1.1 Background of Study
Agreeing to statistics that has been provided from U.S Energy Information Administration
in 2007 annual report on rapid increase of demand for petroleum and gas production. World
demand for oil is projected to increase by 37% over 2006 levels by 2030. It is because the
oil is widely used in many industries such as transportation, manufacturing, polymers,
shipment and others. Transportation consumes major amount of the energy and increase
year by year. This growth has largely come from new demand for personal-use vehicles
powered by internal combustion engines. There is endless need to reduce carbon emissions
and problems encountered with biodiesel blends, such as fuel system corrosion, increased
fuel foaming and water separation. Fuel additives are compounds put together to increase
the quality and efficiency of the fuels used in motor vehicles through treatments. Cars and
trucks are predicted to cause the highest demand in the transportation approaching to 75%.
In other to reduce the consumption of fuel as well as improvement of gas produced during
combustion, isopropyl alcohol (IPA) is used as an additive in the fuel.
IPA is used in gasoline blending as an octane enhancer to improve hydrocarbon combustion
efficiency. It is primarily produced by combining water and propene in a hydration reaction.
It is also produced by hydrogenating acetone. In the conventional process, separate system
between reactor and separation units are used. This technology features a two-stage reactor
system of which the first reactor is operated in a recycle mode. With this method, a slight
expansion of the catalyst bed is achieved which ensures very uniform concentration profiles
within the reactor and can avoid hot spot formation. Undesired side reactions, such as the
formation of diisopropyl ether (DIPE) also can be minimized.
2
Nowadays, the search for a novel method to replace the conventional one has been a major
interest both in industry and academia. This novel method is learnt to give high conversion
of fuel additives economically (Giwa and Giwa, S.O., 2013), and it is know as “reactive
distillation”. Reactive distillation is a process in which the chemical reactor is also the still
(an apparatus used to distill liquid mixtures by heating to selectively boil and then cooling
to condense the vapor). Separation of the product from the reaction mixture does not need a
separate distillation step, which saves energy (for heating) and materials.
Furthermore, reactive distillation is a process that combines chemical reactions and physical
separations into a single unit operation. This process, as a whole, is not a new concept as
the first patent dates back to 1920. The initial publications on this process dealt with
homogeneous self-catalyzed reactions such as esterifications and hydrolysis, but
heterogeneous catalysis in reactive distillation is a more recent development. While the
concept existed much earlier, the first real- world of the system implementation of reactive
distillation took place only in the 1980s.
The relatively large amount of new interest in reactive distillation is due to the numerous
advantages it has over typical distillation. It can enhance reaction rates, increased
conversion, enhanced reaction selectivity. Also, heat integration benefits and reduced
operating costs are part of the benefits associated with reactive distillation. All these factors
contribute to the growing commercial importance of reactive distillation.
However, since heat transfer, mass transfer, and reactions are all occurring simultaneously,
the dynamics which can be exhibited by catalytic distillation columns can be considerably
more complex than found in regular columns. These results in an increase in the complexity
of process operations and the control structure installed to regulate the process.
3
1.2 Problem statement
The conventional method of isopropyl alcohol (a fuel additive) production is not only
ineffective in handling the side reaction involved in the process but also very costly because
many pieces of equipment (reactors, separators, etc) are required by it. The inefficiency of
this process to suppress those side reactions as well as its high cost are the major problems
identified it and to which solutions must to be proffered. One approach of solving this
problem is by developing a control algorithm that will be able to make the process behave
as desired.
1.3 Aim and Objectives
The aim of this project to carry out proportional-derivative-integral (PID) control of a
reactive distillation process for fuel additive (isopropyl alcohol) production. In order to
achieve this aim, the following objectives are set:
 developing ChemCAD model of the process,
 simulating the developed ChemCAD process model for both steady-state and dynamics
to generate dynamic response data,
 developing the process transfer functions with the aid of MATLAB using the generated
data,
 developing the Simulink mode of the process using the developed transfer function,
 carrying out the open-loop simulation of the transfer function in Simulink environment,
and
 applying an appropriate method to tune the controller and simulating the control system
of the process for both servo and regulatory cases.
4
1.5 Scope of Study
This work is limited to applying ChemCAD and MATLAB/Simulink to model, simulate
and control a reactive distillation process for fuel additive production.
1.6 Significant of Study
The successful completion of this work will provide the parameters required to be inputed
into a PID controller used for the control of a reactive distillation process in order to obtain
a very high purity of isopropyl alcohol, which is a fuel additive

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