高等学校化学学报 ›› 1997, Vol. 18 ›› Issue (9): 1407.

• 论文 •    下一篇

在(TPA)2O-Na2O-SiO2-H2O体系中MFI型硅沸石的结晶行为(Ⅱ)──硅沸石微细晶粒的低温合成及其结构和性质表征

吴爱梅, 龙英才   

  1. 复旦大学化学系, 上海 200433
  • 收稿日期:1996-09-16 出版日期:1997-09-24 发布日期:1997-09-24
  • 通讯作者: 龙英才
  • 作者简介:吴爱梅, 女, 26岁, 硕士研究生.
  • 基金资助:

    国家自然科学基金

Studies on the Crystallization Behavior of Zeolite Silicalite-1 in(TPA)2O-Na2O-SiO2-H2O System(Ⅱ)──Low Temperature Preparation and Characterization of Fine Crystals

WU Ai-Mei, LONG Ying-Cai   

  1. Department Of Chemistry, Nankai University, Tianjin 300071
  • Received:1996-09-16 Online:1997-09-24 Published:1997-09-24

摘要: 以白炭黑和硅溶胶为桂源, 在(TPA)2O-Na2O-SiO2-H2O体系60℃下合成了高结晶度纯相硅佛石.由SEM测得其晶粒尺寸为0.2μm和0.45μm, 用XRD线宽法测得的为0.02μm.与180℃时合成的硅沸石样品相比, 低温合成的细晶粒硅沸石已具备纳米级材料的若干特性.其正乙烷吸附量反常增大;XRD、FTIR、29SiMASNMR和TG/DTG/DTA的研究证明, 其结构破坏温度和单斜/正交对称性相转变温度明显下降, 桂羟基缺陷明显增加.

关键词: 硅沸石, 纳米材料, 低温合成, 吸附, 结构表征

Abstract: Zeolite slllcallte-1 with a high crystallinity was synthesized in the system of(TPA)2O-Na2O-SiO2-H2Oat 60℃ by using fumed silica-silica aerogel(Ⅰ) or silica sol(Ⅱ)as the silicon source. The crystal size of products obtained is 0.2 μm in(Ⅰ) and 0.45μm in(Ⅱ) measured by SEM, and 0.02μm determined by the method of XRDpeak broadness.Incomparison with the properties of sample Aprepared at 180℃,the fine crystals Bsynthe-sized at 60℃ possess some characters which the nanometer particles have.The adsorption ofn-hexane on sample Bis abnormaly high.Investigated by XRD, FT-IR, 29Si MAS NMRandTG/DTG/DTA, the temperatures for structural damage and for monoclinic/orthorhombicspmmetrt transformation ofsample Bare obviously lower than that of sample A. The de-fects of Si-OHin sample Bare much more than those in sample A.

Key words: Zeolite silicalite-1, Nanometer material, Low temperature synthesis, Adsorption, Structural characterization

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