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Synthesis and characterization of zeolite-type materials: Germanates and zirconogermanates.

机译：沸石型材料的合成和表征：锗酸盐和锆锗酸盐。

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摘要

The great importance that zeolites have in the industry accounting for 40 billion US dollars a year to the petroleum cracking industry alone has attracted the interest of synthesizing and developing new crystalline microstructures.;This work presents the unique structural properties of germanates, zeolite-type materials, by first reviewing five unique structure building units (SBUs) that include: 4=1 units, D4R units and large clusters with 7-, 9-, and 10-germanium atoms. Then, the work of the syntheses and characterization of different germanate structures is presented.;The synthesis and characterization of four zirconogermanates constructed from the same cluster consisting of five tetrahedral germanium atoms and one zirconium atom in octahedral coordination is presented. The structures were prepared using different amines as structure directing agents (SDA); ASU-23 (using 1,4-bis(3-aminopropyl) consists of one layered structure, ASU-24 (using hexamethylenediamine) is a pillared layered structure with exceptionally low framework density (FD=8.48 metal atoms per nanometer cubed), ASU-25 and ASU-26 (using 1,3-diaminopropane and ethylenediamine respectively) have 3-dimensional (3D) frameworks.;The layer germanate (ASU-22) is built from 7-germanium clusters. X-ray structural analysis [P6(3)cm, a =28.794(2), c=20.603(4), V=14793(3) (unit cell parameters are in angstroms, volume in angstroms cubed)] revealed that the framework exhibits the kagome (kgm) topology. The extensive series of syntheses demonstrated the key role played by HF in the condensation of the 7-germanium clusters (these clusters have not been synthesized without HF).;The zirconogermanate, ASU-17, in the 1,4-diaminobutane-HF system, was synthesized as crystalline powder and identified in the cubic crystals system with space group Ia-3d and unit cell parameter a =51.3 (angstroms) and corresponds to the SU-M structure reported by a group in Sweden. Exploratory work leading to the discovery this 3D cubic framework built from 10-germanium clusters showing pore size reaching the mesoporous range is presented.;The synthesis and characterization of ASU-21, a crystalline germanate displaying large rigid cylinders, was also synthesized in the presence of hexamethylenediamine. The single crystal X-ray analysis [Ibam, a=49.257(10), b=28.439(6), c=14.866(3), V=20825(7) (unit cell parameters in angstroms and volume in angtrom cubed)] revealed the novel open-framework built form the same 10-germanium clusters found in ASU-17.
机译：仅在石油裂化行业中，沸石在行业中的重要性就达到每年400亿美元，这引起了合成和开发新的晶体微观结构的兴趣。这项工作展示了锗酸盐，沸石型材料的独特结构特性，首先查看五个独特的结构构建单元（SBU），这些单元包括：4 = 1单元，D4R单元以及具有7、9和10锗原子的大型簇。然后，介绍了不同锗酸盐结构的合成与表征工作。提出了由五面体锗原子和一个锆原子以八面体配位组成的同一簇构成的四种锆锗酸盐的合成与表征。使用不同的胺作为结构导向剂（SDA）制备结构； ASU-23（使用1,4-双（3-氨基丙基）由一层结构组成，ASU-24（使用六亚甲基二胺）是具有极低骨架密度（FD = 8.48金属原子/纳米立方）的柱状结构，ASU -25和ASU-26（分别使用1,3-二氨基丙烷和乙二胺）具有3维（3D）框架。锗酸盐层（ASU-22）由7个锗簇组成。X射线结构分析[P6 （3）cm，a = 28.794（2），c = 20.603（4），V = 14793（3）（单位晶胞参数以埃为单位，体积以埃为单位））显示框架呈现出kagome（kgm）拓扑。广泛的合成过程证明了HF在7-锗簇的缩合中起着关键作用（这些簇在没有HF的情况下无法合成）；锆锗锗酸盐ASU-17在1,4-二氨基丁烷-HF中合成为结晶粉末，并在空间群为Ia-3d且晶胞参数a = 51.3（埃）的立方晶体系统中进行鉴定并对应于瑞典一个小组报告的SU-M结构。进行了探索性工作，从而发现了由10个锗簇构成的3D立方框架，其孔径达到了介孔范围。；还存在下合成了具有大刚性圆柱体的结晶锗酸盐ASU-21的合成和表征。六亚甲基二胺。单晶X射线分析[Ibam，a = 49.257（10），b = 28.439（6），c = 14.866（3），V = 20825（7）（单位晶格参数以埃为单位，体积以angtrom立方表示）]揭示了与ASU-17中发现的10个锗簇相同的新型开放框架。

著录项

  • 作者

    Smith, Rebeca.;

  • 作者单位

    Arizona State University.;

  • 授予单位 Arizona State University.;
  • 学科 Chemistry Inorganic.;Engineering Materials Science.
  • 学位 Ph.D.
  • 年度 2009
  • 页码 238 p.
  • 总页数 238
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 无机化学;工程材料学;
  • 关键词

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