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用沉淀二氧化硅合成钛硅分子筛TS-2的研究

郭建维1; 王乐夫2; 刘卅2; 张焜1; 易国斌1; 李大光1; 余林1   

  1. 1. 广东工业大学轻工化工学院, 广州 510090; 2. 华南理工大学, 广州 510640
  • 收稿日期:2004-03-01 修回日期:2004-04-28 出版日期:2005-03-20 网络出版日期:2005-03-20

Synthesis of Titanium Silicalite Molecular Sieve TS-2 by Precipitate Silica

GUO Jian-Wei1; WANG Le-Fu2; LIU Sa2; ZHANG Kun1; YI Guo-Bin1; LI Da-Guang1; YU Lin1   

  1. 1. Faculty of Chemical Engineering & Light Industry; Guangdong University of Technology; Guangzhou 510090; China; 2.Southchina University of Technology; Guangzhou 510641; China
  • Received:2004-03-01 Revised:2004-04-28 Published:2005-03-20 Online:2005-03-20

摘要: 以沉淀二氧化硅为硅源,钛酸四丁酯为钛源,四丁基氢氧化铵为模板剂,采用水热晶 化法合成了TS-2分子筛.在优化合成步骤的基础上,采用XRD、FT-IR、UV-Vis、SEM 等测试方法系统研究了晶化温度、凝胶Si/Ti对晶化动力学行为及TS-2分子筛晶相结构的影 响.结果表明:高纯TS-2分子筛的最佳晶化温度为175℃,过高的晶化温度易导致MEL结构 向MFI晶相结构的转变及晶粒的逐渐长大.高纯TS-2样品的极限Ti/Si值为0.04,高于此值 则生成非骨架钛氧化物,并造成相对结晶度和催化氧化性能显著降低.

关键词: 钛硅分子筛, TS-2, 合成, 沉淀二氧化硅

Abstract: Titanium silicalite molecular sieve TS-2 was synthesized by hydrothermal crystallization using precipitate
silica as Si source, tetrabutylorthotitanate(TBOT) as Ti source, tetrabutyl ammonium hydroxide(TBAOH) as template. The influences of crystallization
temperature and Si/Ti of the pre-gel on the crystallization kinetics and the crystal structure of TS-2 were investigated systematically by using XRD, FT-IR,
SEM, UV-Vis on the base of the optimized synthetic procedure. It could be concluded from the experimental results that the optimal crystallization
temperature should be 175℃. The higher crystallization temperature readily results in the increase of crystal particle size and the conversion
of crystal structure from MEL to MFI. The highest value of Ti/Si(mol/mol) of TS-2 product should be 0.04.The higher value of Ti/Si(>0.04) of TS-2 could
result in the formation of extra-framework titanium, as well as the decrease of relative crystallinity and catalytic performance.

Key words: titanium silicalite molecular sieve, TS-2, synthesis, precipitate silica

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