本研究旨在設計與製備以應用為目的之新型態孔洞材料。於本論文中所研究及討論之材料，可依種類及合成策略將其分為兩類。其一為利用雙功能結構導向試劑合成由沸石奈米層板組成之階層性沸石材料。本實驗室設計與開發出新型三節式結構導向試劑，其由中央疏水之聚丙氧基鏈串連兩端親水之結構導向官能基所組成。實驗結果顯示此三節式結構導向試劑能有效地調控沸石奈米層板的堆疊以及交錯成長，進而得到具有不同形貌的階層性沸石材料。此外，我們發現具有高比例交錯成長形貌之 silicalite-1 奈米層板擁有高比例之網狀矽醇基，其最有可能位在奈米層板之交錯處。此類型之silicalite-1 奈米層板於氣相 Beckmann rearrangement 上展現相當高以及穩定的活性與選擇性。我們更進一步地利用三節式結構導向試劑之聚丙氧基鏈與石墨烯表面間的疏水作用力，以石墨烯作為載體引導沸石奈米層板於其表面進行成長。同時我們也設計另一雙節式結構導向試劑，其一端由芘構築而成，利用芘與石墨烯間之 𝜋-𝜋 作用力以達同樣目的。在另一方面，我們利用本實驗室所發展之無模版法合成介孔鈦矽酸鹽，該材料係利用三乙醇胺穩定鹼性環境下之鈦物種，並利用 pH 值下降促使其與矽酸鹽物種進行共同縮反應，進而得到最後的介孔鈦矽酸鹽材料。該材料可同時進行痲瘋果油的酯化與轉酯化反應以得到高品質之生質柴油，且展現相當好之催化活性。

The thesis aims to design and prepare novel porous materials toward catalytic and other applications. Two synthetic strategies were developed to prepare distinct types of materials. Inspired by the synthesis of hierarchical zeolites comprising nanosheets using bifunctional structure-directing agents (SDAs), we developed a series of triblock SDAs featuring a polypropylene oxide (PO) linker between two heads of structure directing groups. Experimental results suggested that branching and stacking of zeolite nanosheets could be rationally controlled by using the designed triblock SDAs. Moreover, the highly-branched silicalite-1 nanosheets catalysts possessing significant amount of nest-like silanols which were generated most likely at the junctions of well-organized nanosheets/nanoplates exhibited excellent and stable activity for the vapor-phase Beckmann rearrangement and high lactam selectivity. We further employed the hydrophobic interaction between the PO linker of triblock SDA and the surface of graphene flakes to direct the restricted growth of zeolite nanosheets on graphene flakes. For the same purpose, a diblock SDA composed of a moiety of pyrene was synthesized to utilize the strong 𝜋-𝜋 interaction between pyrene and graphene. Alternatively, we developed a surfactant-free synthesis of nanoporous titanosilicates via the homogeneous cocondensation of silicate species and triethanolamine-stabilized titanium induced by a pH-drop of the highly alkaline synthesis solution. The thus prepared materials showed high catalytic activity for simultaneous esterification and transesterification of non-edible Jatropha oil for the production of high-quality biodiesel fuel.

Abstract i
Acknowledgements iii
Abbreviations iv
Table of Contents viii
List of Figures x
List of Tables xviii
Chapter 1 General Introduction 1
1.1 Classification of porous materials 1
1.1.1 Zeolites 1
1.1.2 Mesoporous materials 6
1.2 Acidity of zeolites and their catalytic applications 12
1.3 Hierarchical zeolites 15
1.3.1 Hierarchical zeolites comprising nanosheets 22
1.4 Aims of the study 31
Chapter 2 Morphology Control of Hierarchical MFI Zeolites Comprising Nanosheets 33
2.1 Background 33
2.2 Experimental section 35
2.3 Results and discussion 44
2.3.1 Hierarchical silicalite-1 octahedra 44
2.3.2 Effect of PO linker 52
2.3.2.1 TEOS as silica source 53
2.3.2.2 Sodium silicate as silica source 64
2.3.3 Effect of additive 70
2.4 Summary 82
Chapter 3 Catalytic Studies of Hierarchical Silicalite-1 on Vapor-phase Beckmann Rearrangement 84
3.1 Background 84
3.2 Experimental section 86
3.3 Results and discussion 88
3.3.1 Vapor-phase Beckmann rearrangement over hierarchical silicalite-1 octahedra 88
3.3.1.1 The reusability of silicalite-1 octahedra 94
3.3.2 Effect of hierarchical structure 95
3.3.2.1 The reusability of hierarchical silicalite-1 catalysts 99
3.4 Summary 103
Chapter 4 The Preparation of Zeolite Nanosheets on Graphene 105
4.1 Background 105
4.2 Experimental section 107
4.3 Results and discussion 111
4.3.1 Triblock SDA N3PO68N3 111
4.3.2 Diblock SDA N3Py 117
4.4 Summary 121
Chapter 5 Surfactant-free Synthesis of Nanoporous Titanosilicates as Solid Acid Catalysts for Biodiesel Fuel Production 122
5.1 Background 122
5.2 Experimental section 126
5.3 Results and discussion 130
5.3.1 Characterizations of nanoporous titanosilicates 130
5.3.2 Synthesis of Jatropha BDF over nanoporous titanosilicates 141
5.3.3 Synthesis of high-quality Jatropha BDF 148
5.4 Summary 151
Chapter 6 Conclusion and Perspectives 152
References 157
List of Publications 173

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