催化学报 ›› 2015, Vol. 36 ›› Issue (6): 838-844.DOI: 10.1016/S1872-2067(14)60255-2

• 论文 • 上一篇    下一篇

由纳米晶前驱体组装有序介孔silicalite-1分子筛

魏方方, 宋卫国, 魏芳, 曹昌燕   

  1. 中国科学院化学研究所分子纳米结构与纳米技术中国科学院重点实验室, 北京100190
  • 收稿日期:2014-09-30 修回日期:2014-11-20 出版日期:2015-05-21 发布日期:2015-05-21
  • 通讯作者: 宋卫国,电话/传真: (010)62557908; 电子信箱: wsong@iccas.ac.cn
  • 基金资助:

    国家自然科学基金(21273244, 21333009和21121063).

Ordered mesoporous silcalite-1 zeolite assembled from colloidal nanocrystalline precursors

Fangfang Wei, Weiguo Song, Fang Wei, Changyan Cao   

  1. Beijing National Laboratory for Molecular Sciences, Laboratory for Molecular Nanostructures and Nanotechnology, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190, China
  • Received:2014-09-30 Revised:2014-11-20 Online:2015-05-21 Published:2015-05-21
  • Supported by:

    This work was supported by the National Natural Science Foundation of China (21273244, 21333009 and 21121063).

摘要:

采用两步法将不同尺寸的silicalite-1分子筛纳米晶种通过自组装合成了一系列有序介孔silicalite-1分子筛. 首先将强碱性的silicalite-1前驱体分别加热不同时间得到纳米晶种, 然后在类似合成SBA-15的强酸性条件下组装成有序的介孔材料. 合成条件的剧烈变化阻止了分子筛晶种的继续长大, 并在三嵌段共聚物模板的诱导下组装成有序介孔材料. 这种"自下而上"的方法制备有序介孔分子筛同时包含微孔和介孔. 氮气吸脱附结果表明所制备的介孔分子筛材料均表现了很大的比表面积(730 m2/g以上).

关键词: 有序介孔, 分子筛, 自组装, 自下而上方法, 纳米晶种

Abstract:

A series of ordered mesoporous silicalite-1 zeolites has been synthesized by the self-assembly of nanosized zeolite silicalite-1 seeds with different sizes using a two-step procedure. The nanosized silicalite-1 seeds were prepared with an alkali precursor solution that was heated for different periods, and then assembled into ordered mesoporous materials under strongly acidic conditions, similar to that of mesoporous silica SBA-15 which has well ordered hexagonal mesopores and amorphous walls. A significant change in synthesis conditions prevents the continued growth of zeolite seeds and induces assemblage into ordered mesoporous materials templated by triblock copolymers. The samples assembled by zeolite nanoclusters were investigated by X-ray diffraction, electron microscopy, infrared spectroscopy, and N2 adsorption-desorption isotherms. This "bottom-up" approach yields porous materials that contain ordered micro- and mesopores. The mesoporous zeolite has a large surface area (> 730 m2/g).

Key words: Ordered mesoporous zeolite, Self-assembly, Bottom-up method, Nanosized seed