化学学报 ›› 2006, Vol. 64 ›› Issue (24): 2389-2395.    下一篇

研究通讯

四氢呋喃/水体系中以蒸气相传输法合成高硅FER沸石

程晓维, 汪靖, 龙英才*   

  1. (复旦大学化学系 上海市分子催化与新材料重点实验室 上海 200433)
  • 投稿日期:2006-06-12 修回日期:2006-08-03 发布日期:2006-12-28
  • 通讯作者: 龙英才

High-silica FER Zeolite Synthesized in Tetrahydrofuran/Water Sys-tems with VPT Method

CHENG Xiao-Wei; WANG Jing; LONG Ying-Cai*   

  1. (Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials, Department of Chemistry, Fu-dan University, Shanghai 200433)
  • Received:2006-06-12 Revised:2006-08-03 Published:2006-12-28
  • Contact: LONG Ying-Cai

以X射线衍射(XRD), 红外光谱(FT-IR), 扫描电镜(SEM), 低温氮吸附, 29Si固体核磁共振(MAS NMR)等研究了含FER晶种的Na2O-SiO2-Al2O3干胶(SDG)在四氢呋喃(THF)/水(H2O)混合蒸气相中的结晶行为, 同时研究了体系中THF分子和[SiO4], [AlO4]基团在结晶前后状态的变化. 结果表明, 在THF/H2O混合蒸气中以蒸气相传输法(VPT)可合成结晶度较高、结构完美且孔道开放的FER沸石. 13C交叉极化固体核磁共振(CPMASNMR)和差热分析(TG-DTG-DTA)等研究证明THF分子作为模板剂, 位于FER笼内. FER晶种和水能促进FER沸石的结晶.

关键词: 镁碱沸石, FER沸石, 蒸气相传输法, 四氢呋喃, 结晶

The transformation of FER-seeded Na2O-SiO2-Al2O3 dry gel (SDG) in the mixed vapor of tetrahydrofuran (THF) and water (H2O) was studied using the characterizations of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), N2 adsorption and 29Si magic-angle spinning (MAS) nuclear magnetic resonance (NMR), and the state changes of THF molecules and [SiO4] and [AlO4] groups in the systems before and after crystallization were compared with each other. The results show that the FER zeolite with high crystallinity, perfect structure and open channels has been synthesized with the method of vapor phase transport (VPT) in the mixed vapor of THF/H2O. The characterizations of 13C cross-polarization (CP) MAS NMR and TG-DTG-DTA indicate that THF molecules trapped in FER cages of the zeolite play a template role, and detailed studies show that FER zeolite seeds and H2O can promote the crystallization of FER zeolite.

Key words: ferrierite, FER zeolite, vapor phase transport, tetrahydrofuran, crystallization