高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (12): 1797.

• 论文 • 上一篇    下一篇

超临界条件下合成晶型骨架的介孔氧化锆

赵军平, 王树国, 巩雁军, 吴东, 孙予罕   

  1. 中国科学院山西煤炭化学研究所, 煤转化国家重点实验室, 太原 030001
  • 收稿日期:1999-11-23 出版日期:2000-12-24 发布日期:2000-12-24
  • 通讯作者: 孙予罕(1962年出生),男,博士,研究员,从事纳米材料合成与应用研究.
  • 基金资助:

    国家自然科学基金(批准号:29971057;29625307)资助

Synthesis of Mesoporous Zirconia with Crystalline Framework in Super-critical Ethanol

ZHAO Jun-Ping, WANG Shu-Guo, GONG Yan-Jun, WU Dong, SUN Yu-Han   

  1. State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China
  • Received:1999-11-23 Online:2000-12-24 Published:2000-12-24

摘要: 采用聚氧乙烯型非离子表面活性剂(PEO)为模板剂,超临界乙醇为介质,在不同条件下(各种PEO,不同pH值和络合剂)合成了类似于MSU的介孔氧化锆.XRD,N2物理脱吸附曲线,TEM及选区电子衍射证明该介孔氧化锆骨架为四方晶型;改变表面活性剂类型、络合剂及pH可调变介孔氧化锆的BET表面积与孔分布.

关键词: 聚氧乙烯型表面活性剂, 超临界乙醇, 介孔氧化锆, 晶型骨架

Abstract: By using nonionic polyethylene oxide surface(PEO) as a template, mesoporous zirconia was synthesized in super critical ethanol under different conditions(wide pH, various types of PEOand different chelates).XRD, N2adsorption desorption isotherm, TEMand selected area electron diffraction confirmed that the as synthesized powder was mesoporous zirconia with tetragonal walls.Similar to MSUsilica, mesoporous zirconia showed single XRDin small angle, spongy like pore arrangement and non monotonic relation between the pore size and the surfactant length.Thus, the analogous assembly mechanism most likely took place for PEOas the template by forming micelles in thermal ethanol.BETsurface area and pore size could be modified by varying PEO, pHand chelate.The as synthesized mesoporous zirconia had poor thermal stability.It might be because the calcination caused further crystallization and the deformation of crystalline framework, thus losing the meaoporous structure.It is well known that some oxides such as SiO2, Al2O3or TiO2can effectively stabilize totragonal zirconia.Therefore, incorporation with SiO2, Al2O3or TiO2, the meso structure of zirconia successfully retained on the calcination at673 K, or even up to723 Kin some cases.The related work will be published later

Key words: Polyethylene oxide surfactant, Super-critical ethanol, Mesoporous zirconia, Crystalline framework

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