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化学学报
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化学学报 ›› 2006, Vol. 64 ›› Issue (4): 313-319. 上一篇    下一篇

研究论文

具有碱催化活性的有序氮氧化硅MCM-41介孔分子筛的制备与性能研究

张存满*,1，刘茜2，徐政1   

  1. (1同济大学材料科学与工程学院 上海 200092)
    (2中国科学院上海硅酸盐研究所 高性能陶瓷和超微结构国家重点实验室 上海 200050)
  • 投稿日期:2005-04-21 修回日期:2005-10-14 发布日期:2006-02-28
  • 通讯作者: 张存满

Preparation and Performance Study of Ordered Silicon Oxynitride MCM-41 Molecular Sieves with Basic Catalytic Activity

ZHANG Cun-Man*,1, LIU Qian2, XU Zheng1   

  1. (1 School of Material Science and Engineering, Tongji University, Shanghai 200092)
    (2 State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics,
    Chinese Academy of Sciences, Shanghai 200050)
  • Received:2005-04-21 Revised:2005-10-14 Published:2006-02-28
  • Contact: ZHANG Cun-Man

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被引次数

30 | 2

以介孔氧化硅MCM-41为氮化前驱体, 以纯的氨气为氮源, 通过调节氮化工艺参数, 制备出了氮含量高达23.01 wt%、比表面积高达665.4 m2•g－1、平均孔径为2.5 nm的氮氧化硅有序介孔分子筛材料. 采用CNH元素分析、N2吸附- 脱附分析、小角XRD、高分辨透射电镜(HRTEM)、红外光谱以及29Si 固体核磁共振谱(MAS NMR)等技术对材料的结构进行系统的研究. 并且通过苯甲醛和丙二腈的缩合反应研究了该类材料的碱催化活性. 研究表明, 在30 ℃反应3 h后苯甲醛的转化率达到99.9%.

关键词: 氮氧化硅, 有序介孔材料, MCM-41, 碱性催化

The ordered silicon oxynitride mesoporous materials with nitrogen content 23.01 wt%, BET surface area 665.4 m2•g－1 and mean pore size 2.5 nm were successfully prepared by controlling nitridation process parameters. The changes in composition and structure of the silicon oxynitride MCM-41 were investigated by means of elemental analysis, nitrogen sorption measurements, low-angle XRD, Si MAS NMR, IR spectra and high-resolution TEM. The resulting materials showed high activity toward the Knoevenagel condensation of benzaldehyde with malononitrile and the yield reached 99.9% after reacting for 3 h at 30 ℃, which often acts as a probing reaction for base catalysis.

Key words: silicon oxynitride, ordered mesoporous material, MCM-41, base catalysis