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Huong-Thi-Thanh-Tong ; Tong, Huong Thi Thanh ; Huong, Thi Thanh Tong: Boron coordination and co-incorporation of Al, Ga in BEA borosilicate and dissolution of zeolite nanoparticles from large particles in organic solvent [...]. 2007
Inhalt
Acknowledgements
Contents
Abbreviations
Introduction
1.1 Zeolites
1.1.1 Zeolites and Historical Perspective
1.1.2 Zeolites and Molecular Sieve Materials
1.2 Beta Zeolites and Beta Borosilicates
1.2.1 Beta Zeolites
1.2.2 Beta Borosilicates
1.2.3 Applications
1.3 Zeolite Nanocrystals
1.4 Scope of this Thesis
Synthesis of Zeolites and Molecular Sieves
2.1 Organic Structure Directing Agents
2.1.1 Introduction
2.1.2 Removal of SDAs from the Zeotype Framework
2.1.2.1 Calcination
2.1.2.2 Extraction
2.1.3 SDAs for Beta Zeolite and Beta Borosilicate Synthesis
2.2 Hydrothermal Technique
2.2.1 Induction Period
2.2.2 Nucleation
2.2.3 Crystal Growth
2.3 Dry-Gel Conversion Technique
2.4 Post-Synthesis Modification
Colloidal Zeolite Nanocrystals
3.1 Synthesis of Zeolite Nanocrystals
3.1.1 Synthesis of Zeolite Nanocrystals from Clear Solution
3.1.2 Confined Space Synthesis
3.2 Application of Zeolite Nanocrystals
3.2.1 Preparation of Structure Materials
3.2.1.1 Supported Zeolite Films and Membranes
3.2.1.2 Zeolite Structures Synthesized by Application of Ze
3.2.2 Tailored Synthesis of Porous Solids
3.2.3 Other Applications of Zeolite Nanocrystals
3.3 Zeolite Nanoparticles Prepared in Organic Solvents
3.3.1 Organic Solvent
3.3.2 Nanoparticles in Organic Solvents
Nuclear Magnetic Resonance
4.1 Fundamentals of Nuclear Magnetic Resonance Spectrosco
4.2 Interactions in Nuclear Magnetic Resonance , ,
4.2.1 The Zeeman Interaction
4.2.2 Radiofrequency Interaction
4.2.3 Chemical Shift Interaction
4.2.4 Spin-Spin Coupling Interaction
4.2.5 Direct Dipole-Dipole Interaction
4.2.6 Quadrupolar Interaction
4.3 NMR Techniques
4.3.1 Magic Angle Spinning (MAS)
4.3.2 Multiple Quantum Magic Angle Spinning (MQMAS)
Experimental
5.1 Synthesis
5.1.1 *BEA Hydrothermal Synthesis
5.1.1.1 Beta Boronsilicates (B-*BEA)
5.1.1.2 Aluminum Beta Zeolites (Al-*BEA)
5.1.2 *BEA Dry-Gel Synthesis
5.1.3 MFI Synthesis
5.1.3.1 B-MFI
5.1.3.2 Si-MFI
5.2 Calcination and Dehydration
5.3 Ion Exchange
5.3.1 Ion Exchange with Na+, NH4+
5.3.2 Post Synthesis Modification
5.3.2.1 Deboronation
5.3.2.2 Post-Synthesis Exchange with Al3+
5.3.2.3 Post-Synthesis Exchange with Ga3+
5.4 Zeolite Dissolution
5.5 X-Ray Diffraction
5.6 Raman Spectroscopy
5.7 Scanning Electron Microscopy (SEM)
5.8 Atomic Force Microscopy (AFM)
5.9 Thermogravimetric and Differential Thermal Analysis (TG
5.10 Dynamic Light Scattering (DLS)
5.11 Nuclear Magnetic Resonance (NMR) Spectroscopy
Synthesis and Characterization of *BEA-Borosilicate
6.1 Beta Borosilicate Structure
6.1.1 Synthesis Methods
6.1.2 Crystallization Time
6.2 Thermal Analysis
6.3 NMR Spectroscopy
6.3.1 29Si MAS NMR Spectroscopy
6.3.2 1H MAS NMR Spectroscopy
6.3.3 11B MAS NMR Spectroscopy
Boron Coordination of *BEA-Borosilicate
7.1 Dehydration of *BEA-Borosilicate
7.1.1 11B NMR Spectroscopy
7.1.2 1H MAS NMR Spectroscopy
7.2 Hydration of *BEA-Borosilicate
7.2.1 11B NMR Spectroscopy
7.2.2 1H MAS NMR Spectroscopy
7.2.3 29Si MAS NMR Spectroscopy
7.3 Dehydration of Borosilicate after Hydration
7.3.1 11B NMR Spectroscopy
7.3.2 1H MAS NMR Spectroscopy
7.3.3 29Si MAS NMR Spectroscopy
7.4 Discussion
Post-Synthesis of *BEA-Borosilicate
8.1 Deboronation of *BEA-Borosilicate
8.1.1 Ion Exchange
8.1.2 Deboronation
8.1.3 Discussion
8.2 Post-Synthesis Exchange with Aluminum
8.2.1 Post-Synthesis Exchange in Aqueous Media
8.2.1.1 XRD Powder Patterns
8.2.1.2 MAS NMR Spectroscopy
8.2.2 Post-Synthesis Exchange in Ethanol Solvent
8.2.2.1 XRD Powder Patterns
8.2.2.2 MAS NMR Spectroscopy
8.2.3 Discussion
8.3 Post-Synthesis Exchange with Gallium
8.3.1 XRD Powder Patterns
8.3.2 MAS NMR Spectroscopy
8.3.3 Discussion
Dissolution of Zeolite Nanoparticles in Organic Solvents
9.1 Zeolite Nanoparticles in Organic Solvents
9.1.1 Microscale Zeolites
9.1.2 Zeolite Nanoparticles in Dimethylformamide (DMF)
9.1.3 Nanoparticles in Dimethylsulfoxide (DMSO)
9.2 Zeolite Nanoparticle Structure
9.2.1 X-Ray Diffraction
9.2.2 MAS NMR Spectroscopy
9.2.3 Raman Spectroscopy
9.3 Water and Cation Concentration Effects
9.3.1 Water Effect
Sodium Effect
9.4 Concluding Remarks
Summary and Outlook
Bibliography