物理化学学报 >> 1998, Vol. 14 >> Issue (04): 320-326.doi: 10.3866/PKU.WHXB19980407

研究论文 上一篇    下一篇

高硅ZSM-5分子筛和二次合成Ti-ZSM-5分子筛的结构

赵琦, 韩秀文, 刘秀梅, 刘宪春, 翟润生, 包信和, 林励吾, 郭新闻, 张法智, 王祥生   

  1. 中国科学院大连化学物理研究所，催化基础国家重点实验室，大连 116023|大连理工大学，碳资源综合利用开放实验室，大连 116012
  • 收稿日期:1997-07-02 修回日期:1997-10-31 发布日期:1998-04-15
  • 通讯作者: 包信和

Structure of Highly Siliceous ZSM-5 Zeolites and Ti-ZSM-5 Zeolites Obtained by Indirect Synthesis

Zhao Qi, Han Xiu-Wen, Liu Xiu-Mei, Liu Xian-Chun, Zhai Run-Sheng, Bao Xin-He, Lin Li-Wu, Guo Xin-Wen, Zhang Fa-Zhi, Wang Xiang-Sheng   

  1. State Key Laboratory of Catalysis,Dalian Institute of Chemical Physics,Chinese Academy of Sciences,Dalian 116023|Open Laboratory of Comprehensive Utilization for Carbon Resource,Dalian University of Technology,Dalian 116012
  • Received:1997-07-02 Revised:1997-10-31 Published:1998-04-15
  • Contact: Bao Xin-He

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摘要：

运用度角旋转（MAS）和交叉极化（CP）等核磁共振波谱和红外光谱技术，分别对采用不同模板剂制备的高硅ZSM－5分子筛和以此为母体，经气固同晶取代法得到Ti－ZSM－5分子筛的结构特性进行了研究．结果表明：在水热法合成高硅ZSM-5分子筛过程中，模板剂明显制约着所制得的分子筛的结构特性．通过选用合适的模板剂，可直接获得具有正交晶系结构的高硅ZSM－5分子筛．在随后的气固相同晶取代过程中，钛原子通过占据分子筛骨架中的缺陷位进入骨架，形成具有一定Ti／Si比例的钛硅分子筛（Ti－ZSM－5）. 骨架结构中缺陷位的含量直接影响分子筛的载钛量.

关键词: MAS NMR, IR, ZSM-5分子筛, Ti-ZSM-5分子筛, 二次合成

Abstract:

 Solid state NMR with magic angle spinning (MAS) and cross polarization(CP) techniques, and IR spectroscopy have been used to investigate the structural Characterizations of the highly siliceous ZSM-5(S-1) zeolites synthesized using various organic ammoniums or amines as templates and the Ti-ZSM-5 zeolites prepared by the solid reaction of ZSM-5 zeolites with titaniumtetrachloride vapor at 873K . It has been shown that the structure of the ZSM-5 zeolite is strongly governed by the variety of the templates used in the synthesis, and the zeolites templated by TEABr and HDA present the orthorhombic symmetry, while those prepared using TPABr and TPAOH as templates exhibit only monoclinic symmetry . Furthermore, the distribution of the structural defects in the obtained zeolites was found to be also dependent on the templates used. These T-atom defect sites in the framework, defined as Si(OSi)3O-,are available for the insertion of Ti atoms in the subsequent reaction with titaniuintetrachloride vapor at elevated temperatures and the concentration of defects was proved to be correlative to the amounts of Ti atoms being derived into the framework of zeolite.

Key words: MAS NMR, IR, ZSM-5 zeolites, Ti-ZSM-5 zeolites, Indirect synthesis