波谱学杂志 ›› 2001, Vol. 18 ›› Issue (3): 243-247.

• 研究论文 • 上一篇    下一篇

丝光沸石催化剂的固体高分辨核磁共振研究

杨一青,孔祥铭,杨德琴   

  1. 上海石油化工研究院,上海 201208
  • 收稿日期:2001-05-28 修回日期:2001-06-19 出版日期:2001-09-05 发布日期:2001-09-05
  • 作者简介:杨一青(1963-),女,硕士,高工.

STUDY OF MORDENITE CATALYSTS USING HIGH RESOLUTION SOLID STATE NMR

YANG Yi-qing,  KONG Xiang-ming, YANG De-qin   

  1. Shanghai Research Institute of Petrochemical Technology, Shanghai 201208
  • Received:2001-05-28 Revised:2001-06-19 Online:2001-09-05 Published:2001-09-05

摘要:

利用29Si MAS NMR及27Al MAS NMR技术研究了丝光沸石催化剂制备过程中的结构变化,并利用Al的四极作用大小来区分重叠在一起的不同的Al物种.

关键词: 29Si MAS NMR, 27Al MAS NMR, 丝光沸石催化剂

Abstract:

Mordenite catalysts were studied by solid-state 29Si and 27 Al NMR. The relative d istribution of the Si and Al atoms in the framework and the framework Si/Al rati o were obtained by 29Si MAS NMR, and the aluminum species were charact erized by 27Al MAS NMR. 34.3% of the aluminum is lost from the structure fol lowi ng a calcination at 500℃, but only 10.1% of the aluminum became non-framew ork octahedral a luminum that is NMR visible, and 24.2% of the aluminum became non-framework alu minum that is NMR invisible. Possible mechanism of dealumination was suggeste d. After binding with Al2O3, the 29Si MAS NMR spectrum is similar  to that of pur e NH4-MOR, but the 27Al MAS NMR spectrum is different from the simp le addition  of the 27Al MAS NMR spectrum of NH4-MOR and Al2O3. Short pulse length was used to quantify the 27Al MAS NMR experiment, and 27Al MAS NMR wi th various pulse widths (0.5μs, 2μs, 3.5μs and 3.9μs) were used to character ize aluminum sites. With the increase in pulse width, a sharp peak appears on a broad resonance at 0ppm, indicating that there are two different nonframework sites at 0ppm, the broad on e is d u e to octahedrally coordinated aluminum of Al2O3, and the narrow one may be some Al3+ cations, possibly arising from Al2O3 in the process of binding.

Key words: 29Si MAS NMR,  27Al MAS NMR, Mor denite catalysts

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