Thesis Contents

Brief Biography of the Author vii

Acknowledgments x

Nomenclature xi

1 Introduction 1

1.1 Background 1

1.2 Motivation and Significance of this Work 3

1.3 Thesis Outline 5

2 Historical Overview 7

2.1 Pertinent Research 7

2.2 Reactive Distillation 7

2.3 ETBE Synthesis 10

2.4 Modelling Techniques 11

2.5 Operability and Controllability Issues 13

2.6 Summary 16

3 Steady State Simulation 18

3.1 Reaction Chemistry 18

3.2 Reactive Distillation Model 22

3.3 Primary Model Validation 29

3.4 ETBE Simulations 30

4 Design Issues I - Understanding Reactive Distillation 34

4.1 Operating Variables and Interactions 34

4.2 Column Topography 43 ยง Design Issues II - Design Methods 54

5.1 Feasibility of a Reaction-Separation 54

5.2 Proposed Design Strategy for Hybrid Reactive Distillation 65 6 Design Issues m * Integrated Plants 70

6.1 ETBE Synthesis Routes 71

6.2 Process Selection 79

6.3 Process Optimisation 96

6.4 Overall Summary of Findings on Design Issues 102

7 Dynamic Simulation 105

7.1 Problem Formulation 105

7.2 Reactive Distillation Dynamic Model 108

7.3 Steady State Solution of the Dynamic Model 113

7.4 Process Dynamics and Transient Responses 114

8 Multiplicity 121

8.1 Input Multiplicity 121

8.2 Output Multiplicity 127

8.3 Pseudo-Multiplicity 141

8.4 Analysis of a Column for Multiple Steady States 145

8.5 Transitions Between Parallel Steady States 146

8.6 Operability Issues 155

9 Control Issues I - Open-Loop and One-Point Control 160

9.1 Basic Process Objectives 160

9.2 Degrees of Freedom Analysis 162

9.3 Open-Loop Control 163

9.4 One-Point Control 165

10 Control Issues II - Advanced Control 179

10.1 Two-Point Control 179

10.2 Control to Counteract Output Multiplicity 197

10.3 An Integrated Control Scheme 206

10.4 Overall Summary of Findings on Process Dynamics and Control Issues 222

11 Experimental Equipment 225

11.1 Pilot Plant Objectives 225

11.2 Design Basis and Expected Operating Conditions 226

11.3 Reactive Distillation Column 230

11.4 Ancillary Equipment 236

11.5 Feed and Product Systems 238

11.6 Instrumentation 240

11.7 Control System 242

11.8 Installation in the Laboratory 244

11.9 Costs 244

12 Experimental Tests 247

12.1 Equipment Tests 247

12.2 Pilot Plant Simulations 257

12.3 Operating Procedures 260

12.4 Total Reflux Tests 265

13 Conclusions and Recommendations 268

13.1 Conclusions 268

13.2 Recommendations 271

14 Cited Literature 272

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