Catalysts for transesterification

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Table of contents

Table of Contents
General introduction
Chapter 1. Transesterification reactions
1.1. Application of transesterification
1.1.1. Application of transesterification in liquid phase
1.1.2. Application of transesterification in gas phase
1.2. Catalysts for transesterification
1.2.1. Solid acid catalysts
1.2.2. Solid base catalysts
1.3. Preliminary work
1.4. Magnesium silicates
1.5. Aims and objectives
Chapter 2. Role of magnesium silicate hydrate formation
2.1. Introduction
2.2. Choice of reaction conditions
2.2.1. Data from literature
2.2.2. Thermodynamic study
2.2.3. Test with the chosen conditions
2.2.4. Experimental setup
2.3. Catalysts preparation and activities tests
2.3.1. Catalysts preparation
2.3.2. Catalytic performance of magnesium silicates
2.4. Characterisation of acido-basic properties
2.5. Structural characterization of magnesium silicates samples
2.5.1. X-ray spectroscopies
2.5.2. Scanning electron microscopy
2.5.3. 29Si and 25Mg NMR study
2.5.4. Diffuse reflectance infrared Fourier transform spectroscopy characterization
2.5.5. Conclusion on the characterization of the magnesium silicates samples
2.6. Discussion: a bifunctional catalyst
2.7. Kinetic study
2.7.1. Deactivation behaviour of catalyst
2.7.2. Calculation of the order of reaction in ethyl acetate
2.7.3. Interpretation of reaction order in ethyl acetate
2.8. Influence of the nature of the reactants
2.9. Conclusion
Chapter 3. Role of water on reactivity of commercial magnesium silicate
3.1. Introduction
3.2. Role of thermal pretreatment
3.2.1. Experimental procedure
3.2.2. Catalytic performances and TGA analysis
3.3. Characterizations of the pretreated magnesium silicate
3.3.1. DRIFTS analysis
3.3.2. The transmission FTIR spectra of adsorbed CO
3.3.3. 1H NMR analysis
3.3.4. Calorimetry analysis
3.4. Discussion of the structural characterizations and role of water
3.5. Conclusions
Chapter 4. Phyllosilicates
4.1. Introduction
4.1.1. Classification of phyllosilicates
4.1.2. Structure of phyllosilicates
4.2. Preparation of catalysts
4.3. Characterisation of the phyllosilicates
4.3.1. X-ray spectroscopy analysis
4.3.2. Nitrogen sorption analysis
4.4. Catalytic test of phyllosilicates
4.5. Kinetic study
4.5.1. Deactivation behaviour of catalyst
4.5.2. Calculation of the order of reaction in ethyl acetate
4.6. Role of thermal treatment
4.6.1. Catalytic performance and TGA measurement
4.6.2. Characterisation of laponite after pretreatment at different temperatures
4.7. Conclusion
General Conclusion and Outlook
Appendices
Appendix I. Transesterification reaction
Appendix II. Acido-basic properties study: MBOH conversion
Appendix III. X-ray Diffraction (XRD)
Appendix IV. X-ray spectroscopies
i. X-ray Fluorescence spectroscopy (XRF)
ii. X-ray Photoelectron Spectroscopy (XPS)
Appendix V. Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) ..130
i. Infrared and diffuse reflection
ii. Experimental implementation
Appendix VI. Fourier Transform Infrared spectroscopy (FTIR) measurement of adsorbed CO
Appendix VII. Measurement of specific surfaces
i. Principle
ii. Procedure
Appendix VIII. Thermogravimetric analysis
Appendix IX. Calorimetry
Appendix X. Nuclear Magnetic Resonance (NMR) study
Appendix XI. Scanning Electron Microscopy (SEM)