中微双孔分子筛的纳米制备、结构建模及构-效关系研究
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摘要
由于沸石分子筛受限于自身的微孔孔道,在参与化学反应过程中存在巨大的传质阻力,而有序中孔分子筛虽然将孔径尺寸扩展到了中孔范围,但其孔壁结构无定形,导致了有序中孔分子筛的水热稳定性较差、酸催化活性较低,无法满足工业催化反应的需要,因此,开发兼具沸石分子筛的强酸催化活性和可降低传质阻力的中孔结构的新型中微双孔分子筛对于处理复杂气体组分吸附与分离、大分子传递与输送以及大分子多级反应等方面具有重要的意义。鉴于此,本文综合运用多种实验技术及分子模拟技术,开展中微双孔分子筛的纳米制备、结构建模以及构-效关系等方面的研究。
本文创新地将水热合成法用于限制域生长,以三维有序介孔碳为硬模板,成功制备了一系列具有不同晶相结构和相同三维高度有序中孔结构的3DOm-i分子筛(3DOm-i LTA, 3DOm-i MFI, 3DOm-i BEA, 3DOm-i FAU, 3DOm-i LTL),并通过控制反应条件实现3DOm-i分子筛的硅铝比及孔结构在一定范围内内自由调变。
本文采用超声溶解的方法对水热合成出的3DOm-i分子筛进行了拆卸,制备了单分散的沸石纳米晶体,并创新地将密度梯度离心方法用于沸石纳米晶体的分离与提纯;本文还通过BEA纳米晶体与Silicalite-1纳米晶体、Au纳米晶体相互复合,制备出新型的沸石/沸石、沸石/纳米金复合材料,有望将双重酸活性位、酸活性位/金属活性位之间的协同作用应用于特定的催化反应,实现双重/多重活性位的协同催化。
本文采用限制域生长的方法,研究新类型的分子筛材料——片层状MFI分子筛,在有限空间内的生长,成功制备了具有中空结构、外壳为层状MFI的分子筛微球,这是目前对片层状MFI分子筛形貌控制的首次报道。
本文采用沸石纳米微晶自组装的方法成功制备了中微双孔分子筛ZSM-5-MCM-41,并采用分子建模技术首次建立起具有稳定结构的原子级模型,并运用该结构模型研究了ZSM-5-MCM-41对气体的吸附性能。
本文以双亲性表面活性剂P123为模板制备出高质量的中微双孔分子筛SBA-15,并通过建立其原子级结构模型从微观层面研究SBA-15微/中孔结构对气体吸附的影响。
本文创新地采用介观动力学模拟方法研究了双亲性表面活性剂P123在中微双孔分子筛SBA-15形成过程中的致孔机理,深入研究了有机模板剂、硅酸物种的电荷效应以及它们之间的电荷匹配作用对SBA-15介观相结构的影响;此外,通过模拟温度对模板剂P123聚集结构的影响,找寻出了一种温控的方法调节SBA-15微/中孔结构,可望指导实验定向合成具有特定微/中孔搭配的中微双孔分子筛SBA-15。
本文从分子工程学的角度出发,开发和制备了多种兼具沸石分子筛的酸催化活性和可降低传质阻力的中孔结构的中微双孔分子筛,并将分子模拟技术与实验技术相结合,从微观层面上研究了中微双孔分子筛的结构特点、结构与性能之间的关系以及形成机理。中微双孔分子筛的成功制备对于处理复杂气体组分吸附与分离、大分子传递与输送以及大分子多级反应等方面具有重要的意义,也为新材料(如膜材料、纳米功能材料、纳米复合催化剂材料等)的加工与制备开辟了广阔的前景;原子级模型的成功建立为中微双孔分子筛的结构研究提供了更多的微观信息,也为定量构-效关系的建立及材料性能的预测奠定了坚实的基础;采用分子模拟技术探索中微双孔分子筛的形成机理,弥补了现阶段实验表征技术的缺陷,为指导实验定向合成具有特定微/中孔搭配的中微双孔分子筛提供了重要的理论依据。
The micropore structures and high intrinsic activities frequently make zeolites subject to diffusion limitations that, for example, restrict reactant accessibility to the active sites on the interior surfaces of zeolites and inhibit the full utilization of zeolite catalysts, while the ordered mesoporous molecular sieves suffer from the poor hydrothermal stability due to their amorphous frameworks, which restricts their applications in refineries and petrochemical processes. Due to that, the nanofabrication of hierarchical zeolites with micro- and mesoporosity is a proven strategy for integrating shape selectivity (provided by the intrinsic micropore structures) and efficient mass transfer (facilitated by the mesopore structures).
In this paper, three different approaches have been employed to synthesis a series of micro-mesoporous zeolites, including confined synthesis in hard templates, assembly of zeolite nanocrystals, and soft template methods. Moreover, molecular simulation technology has been used for structure exploration and structure-property relationship study of micro-mesoporous zeolites.
Three-dimensionally ordered mesoporous-imprinted (3DOm-i) zeolites with LTA, MFI, BEA, FAU, and LTL topologies have been synthesized within the confined space of 3DOm carbon by conventional hydrothermal treatment. The mesoporosity can be easily tuned by varying the mesopore size of 3DOm carbon and mesoporous structure of the carbon template, and a wide range of crystal morphologies can be achieved by varying the nucleation and crystal growth rate. Moreover, zeolite suspensions of monodisperse nanocrystals with size range and uniformity have been obtained by disassembly of 3DOm-i zeolites, and further used in the fabrication of zeolite/Au and zeolite/zeolite nanocomposite catalysts.
Steam-assisted crystallization treatment has been used for the confined synthesis of lamellar MFI zeolite spheres with hollow structures, and the treatment process demonstrated here has also provided a feasible approach for the morphology control of lamellar MFI zeolites.
Micro-mesoporous zeolite ZSM-5-MCM-41 has been synthesized via assembly of zeolite nanocrystals on ordered mesoporous molecular sieve by microwave treatment. A structure model of ZSM-5-MCM-41 in atomicscale has been established for the first time and further used to investigate the adsorption properties of ZSM-5-MCM-41.
Micro-mesoporous zeolite SBA-15 has been synthesized by soft template methods with P123 as the structure directing agent. An optimized structure model by Anneal Dynamics method has been built and used to demonstrate the effects of micropores located in the intrawall positions of SBA-15 on the adsorption properties of SBA-15
Mesoscopic Dynamics (MesoDyn) method has been employed to simulate the aggregation behavior of triblock copolymer P123, and further explore the structure formation mechanism and analyze the feasibility of accurately adjusting the pore size of SBA-15. Moreover, the effects of charge matching interactions between surfactants and silicate species on mesophase morphologies of SBA-15 have been further discussed.
Overall, the nanofabrication of hierarchical zeolites with micro- and mesoporosity will provide a possibility for quantitatively studying the mass-transfer limitation of porous materials on the adsorptive and catalytic process and may provide building blocks for the synthesis of zeolite thin-films and other nanomaterials, and the structure modeling of micro-mesoporous zeolite will demonstrate a proven strategy for the structure exploration and structure-property relationship investigation, while the formation mechanism study by molecular simulation will provided a theoretical basis for accurately adjusting the pore structure of micro-mesoporous zeolite.
本文创新地将水热合成法用于限制域生长,以三维有序介孔碳为硬模板,成功制备了一系列具有不同晶相结构和相同三维高度有序中孔结构的3DOm-i分子筛(3DOm-i LTA, 3DOm-i MFI, 3DOm-i BEA, 3DOm-i FAU, 3DOm-i LTL),并通过控制反应条件实现3DOm-i分子筛的硅铝比及孔结构在一定范围内内自由调变。
本文采用超声溶解的方法对水热合成出的3DOm-i分子筛进行了拆卸,制备了单分散的沸石纳米晶体,并创新地将密度梯度离心方法用于沸石纳米晶体的分离与提纯;本文还通过BEA纳米晶体与Silicalite-1纳米晶体、Au纳米晶体相互复合,制备出新型的沸石/沸石、沸石/纳米金复合材料,有望将双重酸活性位、酸活性位/金属活性位之间的协同作用应用于特定的催化反应,实现双重/多重活性位的协同催化。
本文采用限制域生长的方法,研究新类型的分子筛材料——片层状MFI分子筛,在有限空间内的生长,成功制备了具有中空结构、外壳为层状MFI的分子筛微球,这是目前对片层状MFI分子筛形貌控制的首次报道。
本文采用沸石纳米微晶自组装的方法成功制备了中微双孔分子筛ZSM-5-MCM-41,并采用分子建模技术首次建立起具有稳定结构的原子级模型,并运用该结构模型研究了ZSM-5-MCM-41对气体的吸附性能。
本文以双亲性表面活性剂P123为模板制备出高质量的中微双孔分子筛SBA-15,并通过建立其原子级结构模型从微观层面研究SBA-15微/中孔结构对气体吸附的影响。
本文创新地采用介观动力学模拟方法研究了双亲性表面活性剂P123在中微双孔分子筛SBA-15形成过程中的致孔机理,深入研究了有机模板剂、硅酸物种的电荷效应以及它们之间的电荷匹配作用对SBA-15介观相结构的影响;此外,通过模拟温度对模板剂P123聚集结构的影响,找寻出了一种温控的方法调节SBA-15微/中孔结构,可望指导实验定向合成具有特定微/中孔搭配的中微双孔分子筛SBA-15。
本文从分子工程学的角度出发,开发和制备了多种兼具沸石分子筛的酸催化活性和可降低传质阻力的中孔结构的中微双孔分子筛,并将分子模拟技术与实验技术相结合,从微观层面上研究了中微双孔分子筛的结构特点、结构与性能之间的关系以及形成机理。中微双孔分子筛的成功制备对于处理复杂气体组分吸附与分离、大分子传递与输送以及大分子多级反应等方面具有重要的意义,也为新材料(如膜材料、纳米功能材料、纳米复合催化剂材料等)的加工与制备开辟了广阔的前景;原子级模型的成功建立为中微双孔分子筛的结构研究提供了更多的微观信息,也为定量构-效关系的建立及材料性能的预测奠定了坚实的基础;采用分子模拟技术探索中微双孔分子筛的形成机理,弥补了现阶段实验表征技术的缺陷,为指导实验定向合成具有特定微/中孔搭配的中微双孔分子筛提供了重要的理论依据。
The micropore structures and high intrinsic activities frequently make zeolites subject to diffusion limitations that, for example, restrict reactant accessibility to the active sites on the interior surfaces of zeolites and inhibit the full utilization of zeolite catalysts, while the ordered mesoporous molecular sieves suffer from the poor hydrothermal stability due to their amorphous frameworks, which restricts their applications in refineries and petrochemical processes. Due to that, the nanofabrication of hierarchical zeolites with micro- and mesoporosity is a proven strategy for integrating shape selectivity (provided by the intrinsic micropore structures) and efficient mass transfer (facilitated by the mesopore structures).
In this paper, three different approaches have been employed to synthesis a series of micro-mesoporous zeolites, including confined synthesis in hard templates, assembly of zeolite nanocrystals, and soft template methods. Moreover, molecular simulation technology has been used for structure exploration and structure-property relationship study of micro-mesoporous zeolites.
Three-dimensionally ordered mesoporous-imprinted (3DOm-i) zeolites with LTA, MFI, BEA, FAU, and LTL topologies have been synthesized within the confined space of 3DOm carbon by conventional hydrothermal treatment. The mesoporosity can be easily tuned by varying the mesopore size of 3DOm carbon and mesoporous structure of the carbon template, and a wide range of crystal morphologies can be achieved by varying the nucleation and crystal growth rate. Moreover, zeolite suspensions of monodisperse nanocrystals with size range and uniformity have been obtained by disassembly of 3DOm-i zeolites, and further used in the fabrication of zeolite/Au and zeolite/zeolite nanocomposite catalysts.
Steam-assisted crystallization treatment has been used for the confined synthesis of lamellar MFI zeolite spheres with hollow structures, and the treatment process demonstrated here has also provided a feasible approach for the morphology control of lamellar MFI zeolites.
Micro-mesoporous zeolite ZSM-5-MCM-41 has been synthesized via assembly of zeolite nanocrystals on ordered mesoporous molecular sieve by microwave treatment. A structure model of ZSM-5-MCM-41 in atomicscale has been established for the first time and further used to investigate the adsorption properties of ZSM-5-MCM-41.
Micro-mesoporous zeolite SBA-15 has been synthesized by soft template methods with P123 as the structure directing agent. An optimized structure model by Anneal Dynamics method has been built and used to demonstrate the effects of micropores located in the intrawall positions of SBA-15 on the adsorption properties of SBA-15
Mesoscopic Dynamics (MesoDyn) method has been employed to simulate the aggregation behavior of triblock copolymer P123, and further explore the structure formation mechanism and analyze the feasibility of accurately adjusting the pore size of SBA-15. Moreover, the effects of charge matching interactions between surfactants and silicate species on mesophase morphologies of SBA-15 have been further discussed.
Overall, the nanofabrication of hierarchical zeolites with micro- and mesoporosity will provide a possibility for quantitatively studying the mass-transfer limitation of porous materials on the adsorptive and catalytic process and may provide building blocks for the synthesis of zeolite thin-films and other nanomaterials, and the structure modeling of micro-mesoporous zeolite will demonstrate a proven strategy for the structure exploration and structure-property relationship investigation, while the formation mechanism study by molecular simulation will provided a theoretical basis for accurately adjusting the pore structure of micro-mesoporous zeolite.
引文
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