波谱学杂志 ›› 2000, Vol. 17 ›› Issue (2): 109-113.

• 研究论文 • 上一篇    下一篇

含硼分子筛的11B VAS NMR和1H MAS NMR研究

陈铁红1, 孙平川1, 邓风2, 王敬中1, 丁大同1   

  1. 1 南开大学, 化学系, 高分子所, 物理系, 天津 300071;
    2 中国科学院武汉物理与数学研究所, 武汉 430071
  • 收稿日期:1999-12-13 修回日期:2000-01-04 出版日期:2000-04-05 发布日期:2018-01-11
  • 作者简介:陈铁红,男,1969年出生,博士,副教授
  • 基金资助:
    国家自然科学基金(29803004)及吸附分离功能高分子材料国家重点实验室开放课题资助项目

11B VAS NMR AND 1H MAS NMR STUDY ON THE BORON-CONTAINING ZEOLITES

CHEN Tiehong1, SUN Pingchuan1, DENG Feng2, WANG Jingzhong1, DING Datong1   

  1. 1 Nankai University, Tianjin 300071;
    2 Wuhan Institute of Physics and Mathematics, The Chinese Academy of Sciences, Wuhan 430071
  • Received:1999-12-13 Revised:2000-01-04 Online:2000-04-05 Published:2018-01-11

摘要: 以变角旋转(VAS) NMR方法考察了三配位硼的存在状态,得到其四极作用常数Cq为2.4MHz,电场梯度不对称系数η为0.0.硼引入骨架形成的酸性羟基质子的信号位于2.3ppm,1H{11B}双共振实验证实其与硼原子的关联很弱.与6.5ppm分子筛吸水峰同时出现的2.7ppm的信号也被认为是吸水的信号,与非骨架铝羟基质子的信号在同一位置,但可通过1H{27Al}双共振实验加以判别.

关键词: 变角旋转(VAS) NMR, 硼硅羟基, 双共振

Abstract: The VAS (Variable Angle Spinning) NMR method was applied in the study on the Boron containing ZSM-12 and ZSM-5 zeolites. By the 11B VAS NMR experiment and simulations of the powder patterns, the quadrupolar constant of the tri-coordinated boron was determined to be 2.4MHz, and the electrical field gradient coefficient 0.0. The resonance of the Boron-Silicon hydroxyl proton is at 2.3ppm, and by the 1H{11B} spin echo double resonance it is shown that the 2.3ppm protons are very weakly coupled with the boron atoms. Besides the 6.5ppm adsorbed water peak, a 2.7ppm water adsorption peak was also found, whose position is the same with the extra framework Al hydroxyls. This kind of water adsorption signal can be distinguished by the 1H{27Al} spin echo double resonance experiment.

Key words: VAS NMR, Boron-Silicon Hydroxyl, Double resonance