高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (11): 2035.

• 研究论文 • 上一篇    下一篇

三维有序大孔杂化材料SiW11O398--SiO2和γ-SiW10O368--SiO2的制备与表征

郭伊荇, 杨宇, 胡长文, 王恩波   

  1. 东北师范大学化学学院多酸化学研究所, 长春130024
  • 收稿日期:2001-12-04 出版日期:2002-11-24 发布日期:2002-11-24
  • 通讯作者: 胡长文(1955年出生),男,博士,教授,博士生导师,从事多酸化学研究.E-mail:huchw@nenu.edu.cn E-mail:huchw@nenu.edu.cn
  • 基金资助:

    国家自然科学基金(批准号:20071007);教育部骨干青年教师基金资助

Preparation and Characterization of Three-dimensional Ordered Macroporous Hybrid SiW11O398--SiO2 and γ-SiW10O368--SiO2 Composites

GUO Yi-Hang, YANG Yu, HU Chang-Wen, WANG En-Bo   

  1. Institute of Polyoxometalate Chemistry, Faculty of Chemistry, Northeast Normal University, Changchun 130024, China
  • Received:2001-12-04 Online:2002-11-24 Published:2002-11-24

摘要: 通过溶胶-凝胶和聚苯乙烯模板等方法制备了含缺位Keggin阴离子SiW11O398-和γ-SiW10O368-的三维有序大孔杂化氧化硅复合材料,并通过紫外漫反射光谱(UV/DRS)、傅里叶变换红外光谱(FTIR)、固体核磁共振波谱(MASNMR)等手段对其结构进行了表征.结果表明,杂化材料中的Keggin阴离子仍保留其基本骨架结构,但其与氧化硅基体之间存在化学作用.杂化材料的孔道结构用扫描和透射电子显微镜(SEM和TEM)进行表征,其平均孔径为(335±50)nm.对杂化材料孔壁的微孔性通过氮气吸附进行了测定.此类材料对水溶液中羟基丁二酸的降解反应具有活性,光催化过程中未发现Keggin阴离子自载体中脱落的现象.

关键词: 三维有序大孔杂化材料, 多金属氧酸盐, 溶胶-凝胶, 聚苯乙烯模板, 光催化

Abstract: Three-dimensional ordered macroporous hybrid silica materials based on lacunary Keggin anions such as SiW 11O398- and γ-SiW 10O368- were prepared via sol-gel method as well as polystyrene templating technique. The structures of as-synthesized composites were characterized by UV diffuse reflectance spectra, FTIR, and solid-state MAS NMR. The results indicate that the primary Keggin structures remain intact in the hybrid materials, and chemical interaction exists between POM molecules and silica matrix. The porous structures of the composites were characterized by SEM and TEM, and their average pore diameters were (335±50) nm. The microporosity of the wall structure was evaluated by the nitrogen adsorption determination. The composites exhibit a photocatalytic activity to degrade aqueous malic acid under irradiation in the near-UV areas, and the leakages of the POMs from the hybrid materials are hardly observed during the process of photocatalysis.

Key words: Three-dimensional ordered macroporous hybrid materials, Polyoxometalates, Sol-gel, Polystyrene templating, Photocatalysis

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