多孔氧化铝以及氧化铝—沸石复合物的制备和表征
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摘要
多孔材料具有大量纳米孔道,结构多样,比表面积较大,在光、电、磁、催化、生物医药、纳米工程和传感领域都具有巨大潜在的应用价值,已发展为一个新兴的跨学科研究领域。经过多年的研究探讨,一大批孔径可调、组成丰富、形貌多样、孔道形状各异且孔道排列方式多样的多孔材料已经被不断地合成出来。然而,尽管人们已经取得了很多优异的成绩,但是多孔材料的研究过程中仍然有许多未知和不足,需要我们探索和寻求解决之道。其中,开发简单、经济、快速、大批量生产高质量多孔材料的新方法,并不断推进多孔材料在催化领域的实用化,仍有大量的工作需要我们去做。这个过程充满了机遇和挑战。
具有比表面大、结构严整、孔径大、表面具有酸性中心等诸多突出特点的新型多孔氧化铝材料,有望在重油大分子的催化裂化、多相催化、石化过程中的吸附分离以及固载酶转化等方面取得较好的进展。但是由于铝的电负性比硅低,更易进行亲核反应,导致铝盐水解、缩聚速率过快,容易形成具有蠕虫状孔道以及无定形的骨架,进而表现出较差的热稳定性和水热稳定性,制约了多孔氧化铝材料的实际应用。另外,有序介孔氧化铝的孔径大小和形貌非常重要,它与催化剂的反应活性和选择性密切相关,因此研究方法去控制介孔氧化铝的孔径和形貌,进一步实现对催化剂性能的调变也是值得关注的。所以本文将致力于采用经济、便捷的方法,合成具有高比表面、相对大孔径的有序介孔氧化铝,以及具有晶化墙壁的多级孔氧化铝材料,并在此基础上初步探寻氧化铝在催化以及沸石粘结剂方面的应用。
在本论文的第二章中,以P123作为表面活性剂,异丙醇铝为无机前驱体,盐酸、柠檬酸作为酸度调节剂,均三甲苯为有机添加剂,采用溶剂挥发诱导组装的方法合成具有大孔径的高度有序以及多级孔径的氧化铝材料。另外,我们还研究了添加剂均三甲苯对于介孔氧化铝孔径以及结构的影响。发现当加入的均三甲苯的量较少时,则可生成具有大孔径的二维六方结构的有序介孔氧化铝,并且随着均三甲苯量的增加,得到的介孔氧化铝的孔径也逐渐变大；当加入的均三甲苯与P123的质量比为5时,则得到具有多级孔分布的氧化铝材料。
在第三章中,利用聚甲基丙烯酸甲酯胶态晶体作为形成有序大孔结构的硬模板,三嵌段高分子聚合物P123作为形成有序介孔结构的软模板。通过软硬双模板的共同作用并结合挥发诱导自组装合成法,制备出了多级有序大孔-介孔Υ-A12O3。此种孔材料具有反蛋白石结构。随后,我们研究了得到的多级孔氧化铝材料作为载体在丙烷氧化脱氢反应上的催化性能。不仅如此,在体系中添加有机溶剂均三甲苯作为膨胀剂和可塑剂,合成了具有球形形貌的介孔氧化铝。
在第四章中,巧妙地以海绵为基底材料,成功合成出具有大孔的沸石单片材料,再结合溶剂挥发诱导组装的方法得到同时具有微孔、介孔和大孔三级孔分布的沸石-氧化铝以及沸石-掺杂金属的氧化铝复合材料。利用XRD, TEM, SEM,BET等手段对其进行了结构和组分分析。此种方法可以将沸石微晶“装配”成具有特定宏观形貌和多级孔道体系的沸石材料,利用其大孔-介孔分子作为客体分子的运输渠道及微孔作为反应的场所,在减少扩散阻力的同时则可充分发挥沸石微孔的作用。
Porous materials with numerous nanoscale pore channels and high surface areas are attracting much attention owing to their unique applications in catalysis, electrics, magnetism, optics, biochemistry, nanotechnology, and sensors et al. After years of efforts and discussions, the porous composite materials with tunable pores, various components, different morphologies and pore channels have been synthesized. However, many challenges and difficulties need to be overcome in the large-scale production and application of ordered mesoporous materials and hierachical porous materials. The synthetic methods with simple, fast, economical and environmental-friendly properties must be developed to obtain the porous materials with high quality, i.e high thermal, hydrothermal stability and crystalline framework. Moreover, the special functionalization of porous materials should be dug for their widely application in catalyst field. This procedure is full of opportunities and challenges.
Novel porous alumina materials with large surface areas, ordered structures, large pore sizes and prominent acidic center can be applied in heavy oil macromolecular FCC, heterogeneous catalysis, adsorption and separation in the petrochemical process, and carried enzyme transformation aspects. However, the fast polycondensation rate of alumina gel makes it easier to form disorder pore and amorphous skeleton owing to the lower electronegativity of aluminum comparing with silicon. In addition, the pore size and morphology of mesoporous alumina as the load have a direct effect on the activity of catalyst. It is possible to tune the composition of catalytic reaction products by proper choice of organized mesoporous alumina with different pore sizes as supports. Based on the above considerations, in this thesis, we focus on the synthesis of ordered mesoporous alumina with large pore sizes and hierarchical structure with crystalline framework. Then, we also investigate their applications in catalysis and binder.
In chapter two, alumina materials with ordered mesoporosity and hierarchical porosity have been synthesized via a one-step process using aluminum iso-propoxide as an inorganic precursor, pluronic P123 as a template, hydrochloric acid and citric acid as the pH adjustors, and 1,3,5-trimethylbenzene (TMB) as a swelling agent. In addition, the weight ratios of TMB/P123 play important roles in controlling the mesostructures and pore sizes of the final alumina materials. Mesoporous alumina with highly ordered 2-D hexagonal symmetry (space group p6mm) can be synthesized with weight ratios of TMB/P123 ranging from 0 to 3. Simultaneously, the pore sizes of ordered mesoporous aluminas can be gradually enlarged with the increase of the TMB content. However, phase transformation of the mesoporous alumina from the 2-D hexagonal to hierarchical could be realized when the TMB/P123 weight ratio was increased to 5.
In chapter three, highly organized macroporous-mesoporous aluminas have been synthesized using poly (methyl methacrylate) colloidal crystal as a hard template and polymer P123 as a soft template. By a combination of hard-soft double template method and evaporation induced self-assemble mathod, we have prepared highly organized hierachical gama-almina. The final materials have anti-opals structure. Then, we studied the catalytic performance of propane dehydrogenation oxidation using the macroporous-mesoporous alumina materials as a support. Furthermore, spherial mesoporous alumina nanoparticles can be produced on the presence of TMB as expansive agent and plastic agent.
In chapter four, large monolith ZSM-5 with macroporous architecture by using a polyether polyol-based polyurethane (PU) foam as a sacrificial scaffold has been prepared. Then, we injected the precursors of mesoporous alumina and alumina-supported metal oxides into the ZSM-5 monolith to obtain hierachical composite materials. We analyzed the structures and compotants of these materials by kinds of characterization methods, such as XRD, TEM, SEM and so on. The above method can assemble the zeolite nanocrystals into hierarchical porous zeolite materials with controllable macroscopic maorphologies, mesoporous alumina or alumina-supported metal oxides matrials. Due to the ramified pore structure in several levels, the efficency of catalysis and separation performed on the hierarchical porous zeolite materials can be well improved.
具有比表面大、结构严整、孔径大、表面具有酸性中心等诸多突出特点的新型多孔氧化铝材料,有望在重油大分子的催化裂化、多相催化、石化过程中的吸附分离以及固载酶转化等方面取得较好的进展。但是由于铝的电负性比硅低,更易进行亲核反应,导致铝盐水解、缩聚速率过快,容易形成具有蠕虫状孔道以及无定形的骨架,进而表现出较差的热稳定性和水热稳定性,制约了多孔氧化铝材料的实际应用。另外,有序介孔氧化铝的孔径大小和形貌非常重要,它与催化剂的反应活性和选择性密切相关,因此研究方法去控制介孔氧化铝的孔径和形貌,进一步实现对催化剂性能的调变也是值得关注的。所以本文将致力于采用经济、便捷的方法,合成具有高比表面、相对大孔径的有序介孔氧化铝,以及具有晶化墙壁的多级孔氧化铝材料,并在此基础上初步探寻氧化铝在催化以及沸石粘结剂方面的应用。
在本论文的第二章中,以P123作为表面活性剂,异丙醇铝为无机前驱体,盐酸、柠檬酸作为酸度调节剂,均三甲苯为有机添加剂,采用溶剂挥发诱导组装的方法合成具有大孔径的高度有序以及多级孔径的氧化铝材料。另外,我们还研究了添加剂均三甲苯对于介孔氧化铝孔径以及结构的影响。发现当加入的均三甲苯的量较少时,则可生成具有大孔径的二维六方结构的有序介孔氧化铝,并且随着均三甲苯量的增加,得到的介孔氧化铝的孔径也逐渐变大；当加入的均三甲苯与P123的质量比为5时,则得到具有多级孔分布的氧化铝材料。
在第三章中,利用聚甲基丙烯酸甲酯胶态晶体作为形成有序大孔结构的硬模板,三嵌段高分子聚合物P123作为形成有序介孔结构的软模板。通过软硬双模板的共同作用并结合挥发诱导自组装合成法,制备出了多级有序大孔-介孔Υ-A12O3。此种孔材料具有反蛋白石结构。随后,我们研究了得到的多级孔氧化铝材料作为载体在丙烷氧化脱氢反应上的催化性能。不仅如此,在体系中添加有机溶剂均三甲苯作为膨胀剂和可塑剂,合成了具有球形形貌的介孔氧化铝。
在第四章中,巧妙地以海绵为基底材料,成功合成出具有大孔的沸石单片材料,再结合溶剂挥发诱导组装的方法得到同时具有微孔、介孔和大孔三级孔分布的沸石-氧化铝以及沸石-掺杂金属的氧化铝复合材料。利用XRD, TEM, SEM,BET等手段对其进行了结构和组分分析。此种方法可以将沸石微晶“装配”成具有特定宏观形貌和多级孔道体系的沸石材料,利用其大孔-介孔分子作为客体分子的运输渠道及微孔作为反应的场所,在减少扩散阻力的同时则可充分发挥沸石微孔的作用。
Porous materials with numerous nanoscale pore channels and high surface areas are attracting much attention owing to their unique applications in catalysis, electrics, magnetism, optics, biochemistry, nanotechnology, and sensors et al. After years of efforts and discussions, the porous composite materials with tunable pores, various components, different morphologies and pore channels have been synthesized. However, many challenges and difficulties need to be overcome in the large-scale production and application of ordered mesoporous materials and hierachical porous materials. The synthetic methods with simple, fast, economical and environmental-friendly properties must be developed to obtain the porous materials with high quality, i.e high thermal, hydrothermal stability and crystalline framework. Moreover, the special functionalization of porous materials should be dug for their widely application in catalyst field. This procedure is full of opportunities and challenges.
Novel porous alumina materials with large surface areas, ordered structures, large pore sizes and prominent acidic center can be applied in heavy oil macromolecular FCC, heterogeneous catalysis, adsorption and separation in the petrochemical process, and carried enzyme transformation aspects. However, the fast polycondensation rate of alumina gel makes it easier to form disorder pore and amorphous skeleton owing to the lower electronegativity of aluminum comparing with silicon. In addition, the pore size and morphology of mesoporous alumina as the load have a direct effect on the activity of catalyst. It is possible to tune the composition of catalytic reaction products by proper choice of organized mesoporous alumina with different pore sizes as supports. Based on the above considerations, in this thesis, we focus on the synthesis of ordered mesoporous alumina with large pore sizes and hierarchical structure with crystalline framework. Then, we also investigate their applications in catalysis and binder.
In chapter two, alumina materials with ordered mesoporosity and hierarchical porosity have been synthesized via a one-step process using aluminum iso-propoxide as an inorganic precursor, pluronic P123 as a template, hydrochloric acid and citric acid as the pH adjustors, and 1,3,5-trimethylbenzene (TMB) as a swelling agent. In addition, the weight ratios of TMB/P123 play important roles in controlling the mesostructures and pore sizes of the final alumina materials. Mesoporous alumina with highly ordered 2-D hexagonal symmetry (space group p6mm) can be synthesized with weight ratios of TMB/P123 ranging from 0 to 3. Simultaneously, the pore sizes of ordered mesoporous aluminas can be gradually enlarged with the increase of the TMB content. However, phase transformation of the mesoporous alumina from the 2-D hexagonal to hierarchical could be realized when the TMB/P123 weight ratio was increased to 5.
In chapter three, highly organized macroporous-mesoporous aluminas have been synthesized using poly (methyl methacrylate) colloidal crystal as a hard template and polymer P123 as a soft template. By a combination of hard-soft double template method and evaporation induced self-assemble mathod, we have prepared highly organized hierachical gama-almina. The final materials have anti-opals structure. Then, we studied the catalytic performance of propane dehydrogenation oxidation using the macroporous-mesoporous alumina materials as a support. Furthermore, spherial mesoporous alumina nanoparticles can be produced on the presence of TMB as expansive agent and plastic agent.
In chapter four, large monolith ZSM-5 with macroporous architecture by using a polyether polyol-based polyurethane (PU) foam as a sacrificial scaffold has been prepared. Then, we injected the precursors of mesoporous alumina and alumina-supported metal oxides into the ZSM-5 monolith to obtain hierachical composite materials. We analyzed the structures and compotants of these materials by kinds of characterization methods, such as XRD, TEM, SEM and so on. The above method can assemble the zeolite nanocrystals into hierarchical porous zeolite materials with controllable macroscopic maorphologies, mesoporous alumina or alumina-supported metal oxides matrials. Due to the ramified pore structure in several levels, the efficency of catalysis and separation performed on the hierarchical porous zeolite materials can be well improved.
引文
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