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化学学报
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化学学报 ›› 2005, Vol. 63 ›› Issue (8): 720-724. 上一篇    下一篇

研究论文

CXN天然沸石的研究 V. 结构超稳化

钟鹰1 2，程晓维1，郭娟1，黄强3，龙英才*1   

  1. (1复旦大学化学系 上海市分子催化与新材料重点实验室 上海 200433)
    (2昭通师范高等专科学校 昭通 657000)
    (3中非地质工程勘查研究院 北京 100010)
  • 投稿日期:2004-08-03 修回日期:2004-12-14 发布日期:2010-12-10
  • 通讯作者: 龙英才

Studies on CXN Natural Zeolite V. Ultra-stabilization of Structure

ZHONG Ying1,2, CHENG Xiao-Wei1, GUO Juan1, HUANG Qiang3, LONG Ying-Cai*1   

  1. (1 Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials, Department of Chemistry, Fudan University, Shanghai 200433)
    (2 Zhaotong Teacher's College, Zhaotong 657000)
    (3 Zhongfei Geological Prospecting Researching Academy, Beijing 100010)
  • Received:2004-08-03 Revised:2004-12-14 Published:2010-12-10
  • Contact: LONG Ying-Cai

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被引次数

19

以离子交换结合控制焙烧的方法分别制得结构超稳化高硅H-STI-I和H-STI-II沸石. EDX, 29Si MAS NMR, 27Al MAS NMR, FT-IR等表征证明, 其骨架硅铝原子比分别为4.43和10.62. 分段程序升温焙烧后的沸石样品经粉末XRD表征表明, 其结构热稳定性达到1000 ℃以上. 结构稳定化沸石呈现反映微孔特性的I型吸附等温线, 吸附孔道完美、开放. 经历过酸处理的H-STI-II沸石, 结构缺陷增多, 其热稳定性、比表面积及孔容积略低于H-STI-I.

关键词: STI沸石, 超稳化, 离子交换, 程序升温焙烧, 固体核磁共振, 氮吸附, 红外光谱

The samples of ultra-stable high-silica H-STI-I and H-STI-II zeolites were prepared using the method of ion-exchange combined with controlled calcinations. Characterizations with EDX, 29Si MAS NMR, 27Al MAS NMR and FT-IR indicate that the framework Si/Al ratios of H-STI-I and H-STI-II are 4.43 and 10.62, respectively. Investigations of the samples obtained in the processs of stage-temperature-programmed calcinations with XRD proved that the structure stability of both samples could be kept at temperature up to 1000 ℃. Type I isotherms of N2 adsorption at 77 K illuminated that the ultra-stable H-STI samples possessed perfect channel systems with opening micro-pore structures. The more structural defects in the framework of H-STI-II, which has been treated with acid in the process of preparation, led to worse thermal stability, lower surface area and pore volume than those of H-STI-I.

Key words: STI zeolite, ultra-stability, ion-exchange, temperature-programmed calcinations, solid NMR, N2 adsorption, FT-IR