化学学报 ›› 2010, Vol. 68 ›› Issue (20): 2035-2040. 上一篇    下一篇

研究论文

微波辅助晶化法合成MCM-22分子筛的研究

凌云,郑玉婷,刘月明*,王振东,吴海虹,吴鹏   

  1. (华东师范大学化学系 上海市绿色化学与化工过程绿色化重点实验室 上海 200062)
  • 投稿日期:2010-03-07 修回日期:2010-05-11 发布日期:2010-06-12
  • 通讯作者: 郑玉婷 E-mail:zhengyuting1986@yahoo.com.cn

A Study on Microwave-Assisted Synthesis of MCM-22 Zeolite

LING Yun, ZHENG Yu-Ting, LIU Yue-Ming, WANG Zhen-Dong, WU Hai-Hong, WU Peng   

  1. (Shanghai Key Laboratory of Green Chemistry and Chemical Processes, Department of Chemistry, East China Normal University, Shanghai 200062)
  • Received:2010-03-07 Revised:2010-05-11 Published:2010-06-12

开展了微波辅助法合成MCM-22分子筛的研究, 经过29 h微波晶化得到了与传统水热法合成5 d相同的100%晶化的样品, 有效地缩短了合成时间. 通过XRD, SEM, FT-IR, ICP和27Al MAS NMR技术表征, 微波辅助合成样品具有高纯度、均一形貌, Al原子有效进入骨架等特征. 对合成中的关键性条件, 如结构导向剂的含量进行了深入研究, 并给出了可能的合成机理. 此外, 通过在合成液中添加少量高介电损失物质, 进一步缩短了合成时间.

关键词: MCM-22, 沸石, 微波合成, 水热合成

MCM-22 zeolite has been synthesized successfully from hydrogels with microwave (MW) heating method, the process of which was compared with that of conventional hydrothermal synthesis (HTS). The MW-assisted heating showed a significant advantage that it reduced greatly the crystallization time. For instance, it led to a fully crystallized MCM-22 within 29 h in contrast to 5 d required by HTS synthesis. Microwave-assisted MCM-22 had good quality in phase purity, crystallinity, textual properties and incorporated tetrahedral Al ions as evidence by the characterizations with XRD, SEM, FT-IR, ICP and 27Al MAS NMR techniques. The paramount role of structure-directing agent in the MW-assisted process has been investigated to give a possible mechanism of crystallization. Moreover, by adding a small amount of alcohols in the initial gels, the crystallization time was further shortened to 24 h.

Key words: MCM-22, zeolite, microwave-assisted synthesis, hydrothermal synthesis