ALDOL CONDENSATION OF HMF AND ACETONE OVER Mg——Al LAYERED DOUBLE HYDROXIDES AND MIXED OXIDES

摘要

The main aim of the work is to synthesize six different types of calcined layered double hydroxides and use them as catalysts for aldol condensation of hydroxymethylfurfural and acetone.The three layered double hydroxides were Mg-Al in different ratios and the other three were Zn-Al,Ni-Al and Mg-Al-Zr.The first three catalysts were prepared by urea precipitation method and the final three catalysts were prepared by titration method while the pH is maintained at 9-10.All the six catalysts were calcined and the mixed oxides were reconstructed to form the calcined layered double hydroxides(CLDH).Both the LDH and CLDH were analysed by different techniques like thermal gravimetric analysis,scanning electron microscopy,Transmission electron microscopy,powder XRD,BET and elemental analysis.
　　Another part of the work was to use the CLDH as catalyst and examine the selective formation of mono condensation and di condensation product of HMF and acetone.The condensation was carded out with all the six catalysts under various experimental conditions in presence of different solvents.Among all the experiments conducted the most optimal catalyst was found to be Mg4Al-CO3-2CLDH which furnished mono condensed product selectively in good yield.The optimised solvent was found to be acetone.The conversion of the products was obtained by gas chromatography.The final product was analysed by spectroscopic techniques like proton NMR and C-13NMR.

目录

声明

Acknowledgments

Brief Introduction of Supervisor and Author

Table of Contents

Abstract

1．Introduction

1．1 Scope and Aim of the Thesis

1．2 Preparation of Catalysts

1．3 Analysis of the Synthesized Catalysts

1．4 Application of The Synthesised Catalysts in Aldol Condensation

2．Literature Survey

2．1 Introduction

2．2 Synthesis of Hydroxyl Methyl Furfural(HMF)

2．2．1 Synthesis of Fuel Intermediates and Transportation Fuel from HMF

2．3 Layered Double Hydroxides(LDH)

2．3．1 Synthesis of LDH

2．4 Materials Obtained from LDH

2．4．1 Mixed Metal Oxides

2．4．2 Rehydrated LDH

2．5 The Application Of LDH as Catalysts for Producing Biofuels

2．6 Aldol Condensation-Catalysed by LDH

3．Materials and Methods

3．1 Preparation of Catalyst

3．1．1 Preparation of Mg-Al LDH by Urea Preparation Method

3．1．2 Preparation of (4：1) of Zn-Al，Ni-Ai and Mg-Al-Zr(0．05) LDH by Thermodynamic Titration Method

3．1．3 Preparation of Layered Double Oxide(LDO)

3．1．4 Aldol Condensation Reaction of Hydroxyl Methyl Furan (HMF) and Acetone

3．2 Analytical Methods

3．2．1 BET(Brunauer Emmett Teller)

3．2．2 Temperature Programmed Desorption(TPD)

3．2．3 Thermo Gravimetric Analysis

3．2．4 Powder XRD

3．2．5 Scanning Electron Microscope

3．2．6 Transmission Electron Microscope(TEM)

3．3 Chemical Characterisation of the Catalysts

3．3．1 Gas Chromatography(GC)

3．3．2 NuclearMagnetic Spectroscopy(NMR)

4．Results and Discussion

4．1 Synthesis of the Layered Double Hydroxides

4．2 Thermal Decomposition of LDH

4．3 Reformation of The Mixed Metal Oxides to Layered Double Hydroxides

The FT-IR Spectra

4．4 The Surface Properties and Morphology

4．4．1 The Analysis of LDH by SEM

4．4．2 Elemental Analysis

4．4．3The Elemental Analysis of Zr-Mg-Al-LDO in Absence of Oxygen

4．4．4 The Analysis of LDH by BET and BJH

4．4．5 The Analysis of LDH by TPD

4．4．6 The Analysis of LDH By Powdered XRD

4．4．7 The Analysis of LDH by TEM

5．Conclusion

References

7．Appendix