多孔材料的合成与氨硼烷储氢应用
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摘要
本论文从多孔材料的定向设计合成出发，借助计算机模拟，成功以LTA分子筛拓扑结构为设计思想，研究基本结构基元和特定拓扑结构之间的关系，利用具有硅氧双四员环D4R的官能化立方硅烷I8OPS [(IPhSiO_(3/2))_8]模拟传统分子筛结构中的D4R，合成了类LTA拓扑结构的新型有机无机杂化骨架，为定向设计提供了新路线，并且成功为无机分子筛材料和有机多孔材料搭建桥梁（第二章）。
以定向设计为基本思路，我们合成了只由C，H轻元素组成的具有很低的骨架密度的有机多孔材料PAF-1，同时该材料具有预想的性质：很高的比表面和很大的孔容，并且热稳定性也普遍高于金属有机骨架。这种新材料的应用成为该论文的研究课题之一。在当今能源问题的大环境下，我们将该材料应用于燃料电池的储氢体系，利用其良好的纳米限域作用和低密度特点，可以明显提高氨硼烷的放氢性能（第三章）。
而以往报导的用于AB性能提高材料一般是同时利用纳米限域和催化作用，但是在PAF-1体系中，仅仅利用前者就能得到相同的性能提高。纳米限域和催化在AB性能的提高中之间的相互关系如何是一个值得探讨的问题，在下一章中，我们选用了不同金属中心的MOF-74结构作为研究对象，探索了纳米限域和催化在该体系中如何发挥作用，并且得到两者共同作用时能得到更好的结果的结论（第四章）。
本论文在有机无机骨架的定向合成以及氨硼烷的性能提高上进行了详细的研究和阐述，为多孔材料在储氢方面的应用提供了大量开创性的工作。
Porous materials have attracted the extensive attention due to its unique porestructure and separation, catalysis, adsorption, confinement properties. Especially, inrecent years, following the development of COFs, MOFs, PAFs materials, organicfunctional groups are introduced into the frameworks which provides widerdevelopment space to design and synthesis porous materials from inorganic moleculesieves to the organic porous material with practical applications.
This paper mainly focuses on how to build up the porous framework which hasthe specific topology of molecule sieve using the organic-inorganic hybrid buildingunit. And we also discussed nano-confinement and catalytic performances of PAFs,MOFs on hydrogen storage in AB system. A series of techniques were employed toimprove the total hydrogen storage and hydrogen dynamics. In summery, the workhas achieved the following results:
(1). Using silica double4-rings (D4R) functionalized cubic silane I8OPS[(IPhSiO3/2)8](octaphenylsilsesquioxanes, OPSs) as cubic nano building block,biphenyl groups were formed to alternate the T–O–T linkage between D4R in LTA orACO backbones of the new porous organic-inorganic hybrid framework of JUC-Z1.MAS, NMR and N2adsorption results show that the structure is likely to have LTAtopology. This strategy of utilizing I8OPS as a building block with Ullmann chemistryas a linking method may provide an approach for constructing a wide variety offunctionalized zeolitic porous organic frameworks that bridge COFs and zeolites.
(2). Using porous aromatic framework PAF-1as substrate to nano-confine ABmolecules can improve the amount of hydrogen and decrease the release temperaturewith no volatile by-products in dehydrogenation process. It started to dehydrogenateat very low temperature (around50oC) with the peak of77oC. Furthermore, about4wt%(AB) of hydrogen was evolved in the first25minutes at75oC which is2wt%ofsystem. Compared with other porous supports such as MOFs, the PAF-1has a verylow framework density because it is built up by light C and H elements. This couldsignificantly improve the hydrogen systemic gravimetric capacity and thus more feasible in practical applications.
(3). MOFs has good catalytic effect due to the metals in the structure relative tothe aromatic frameworks of PAFs materials in the thermal decomposition of AB. Weused NiCo-MOF-74as bi-metal catalyst and nano-confinement substrate. The amountof released hydrogen and rate were much higher than that of the single metalNi-MOF-74and Co-MOF-74systems. Studies have found that Ni is better catalyst toimprove hydrogen releasing speed, and Co is easier to keep the structural stability ofMOF-74. It provides a new method to selective utilize nano-confinement and catalyticproperties.
以定向设计为基本思路，我们合成了只由C，H轻元素组成的具有很低的骨架密度的有机多孔材料PAF-1，同时该材料具有预想的性质：很高的比表面和很大的孔容，并且热稳定性也普遍高于金属有机骨架。这种新材料的应用成为该论文的研究课题之一。在当今能源问题的大环境下，我们将该材料应用于燃料电池的储氢体系，利用其良好的纳米限域作用和低密度特点，可以明显提高氨硼烷的放氢性能（第三章）。
而以往报导的用于AB性能提高材料一般是同时利用纳米限域和催化作用，但是在PAF-1体系中，仅仅利用前者就能得到相同的性能提高。纳米限域和催化在AB性能的提高中之间的相互关系如何是一个值得探讨的问题，在下一章中，我们选用了不同金属中心的MOF-74结构作为研究对象，探索了纳米限域和催化在该体系中如何发挥作用，并且得到两者共同作用时能得到更好的结果的结论（第四章）。
本论文在有机无机骨架的定向合成以及氨硼烷的性能提高上进行了详细的研究和阐述，为多孔材料在储氢方面的应用提供了大量开创性的工作。
Porous materials have attracted the extensive attention due to its unique porestructure and separation, catalysis, adsorption, confinement properties. Especially, inrecent years, following the development of COFs, MOFs, PAFs materials, organicfunctional groups are introduced into the frameworks which provides widerdevelopment space to design and synthesis porous materials from inorganic moleculesieves to the organic porous material with practical applications.
This paper mainly focuses on how to build up the porous framework which hasthe specific topology of molecule sieve using the organic-inorganic hybrid buildingunit. And we also discussed nano-confinement and catalytic performances of PAFs,MOFs on hydrogen storage in AB system. A series of techniques were employed toimprove the total hydrogen storage and hydrogen dynamics. In summery, the workhas achieved the following results:
(1). Using silica double4-rings (D4R) functionalized cubic silane I8OPS[(IPhSiO3/2)8](octaphenylsilsesquioxanes, OPSs) as cubic nano building block,biphenyl groups were formed to alternate the T–O–T linkage between D4R in LTA orACO backbones of the new porous organic-inorganic hybrid framework of JUC-Z1.MAS, NMR and N2adsorption results show that the structure is likely to have LTAtopology. This strategy of utilizing I8OPS as a building block with Ullmann chemistryas a linking method may provide an approach for constructing a wide variety offunctionalized zeolitic porous organic frameworks that bridge COFs and zeolites.
(2). Using porous aromatic framework PAF-1as substrate to nano-confine ABmolecules can improve the amount of hydrogen and decrease the release temperaturewith no volatile by-products in dehydrogenation process. It started to dehydrogenateat very low temperature (around50oC) with the peak of77oC. Furthermore, about4wt%(AB) of hydrogen was evolved in the first25minutes at75oC which is2wt%ofsystem. Compared with other porous supports such as MOFs, the PAF-1has a verylow framework density because it is built up by light C and H elements. This couldsignificantly improve the hydrogen systemic gravimetric capacity and thus more feasible in practical applications.
(3). MOFs has good catalytic effect due to the metals in the structure relative tothe aromatic frameworks of PAFs materials in the thermal decomposition of AB. Weused NiCo-MOF-74as bi-metal catalyst and nano-confinement substrate. The amountof released hydrogen and rate were much higher than that of the single metalNi-MOF-74and Co-MOF-74systems. Studies have found that Ni is better catalyst toimprove hydrogen releasing speed, and Co is easier to keep the structural stability ofMOF-74. It provides a new method to selective utilize nano-confinement and catalyticproperties.
引文
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