物理化学学报 >> 2013, Vol. 29 >> Issue (09): 2035-2040.doi: 10.3866/PKU.WHXB201306183

催化和表面科学 上一篇    下一篇

系列硅铝比纳米薄层ZSM-5分子筛的合成和表征

王务刚, 张少龙, 张兰兰, 王艳, 刘晓玲, 巩雁军, 窦涛   

  1. 中国石油大学(北京)化学工程学院, 重质油国家重点实验室, CNPC催化重点实验室, 北京 102249
  • 收稿日期:2013-04-25 修回日期:2013-06-14 发布日期:2013-08-28
  • 通讯作者: 巩雁军 E-mail:gongyj@cup.edu.cn
  • 基金资助:

    国家重点基础研究发展计划(973)项目(2012CB215002);国家自然科学基金(21276278, 21176255);中国石油天然气集团公司项目(2011A-2101)资助

Synthesis and Characterization of Nanosheet ZSM-5 Zeolites with Different SiO2/Al2O3 Molar Ratios

WANG Wu-Gang, ZHANG Shao-Long, ZHANG Lan-Lan, WANG Yan, LIU Xiao-Ling, GONG Yan-Jun, DOU Tao   

  1. State Key Laboratory of Heavy Oil Processing, Key Laboratory of Catalysis, China National Petroleum Corporation, College of Chemistry Engineering, University of Petroleum-Beijing, Beijing 102249, P. R. China
  • Received:2013-04-25 Revised:2013-06-14 Published:2013-08-28
  • Contact: GONG Yan-Jun E-mail:gongyj@cup.edu.cn
  • Supported by:

    The project was supported by the State Key Development Program for Basic Research of China (973) (2012CB215002), National Natural Science Foundation of China (21276278, 21176255), and China National PetroleumCorporation (CNPC) Program, China (2011A-2101).

摘要:

以自制不对称双子季铵盐表面活性剂为模板, 在水热合成体系中控制合成系列硅铝比纳米薄层ZSM-5分子筛.采用X射线衍射(XRD)、N2吸附-脱附、X射线荧光光谱(XRF)、扫描电镜(SEM)和27Al魔角旋转核磁共振(27Al MAS-NMR)对合成的样品进行了表征. 详细研究了晶化温度、晶化时间、结构导向剂(SDA)用量、碱度等对合成的影响和纳米薄层ZSM-5分子筛的形成过程. 结果表明: 分子筛硅铝比越高, 结构导向剂用量越大, 所需的晶化时间越短; 晶化温度越高, 晶化时间越短; 且不同硅铝比纳米薄层ZSM-5分子筛的形貌规整度、比表面积和介孔/微孔孔容比例随着硅铝比而变化.

关键词: 纳米薄层, ZSM-5分子筛, 合成化学, 硅铝比

Abstract:

Nanosheet ZSM-5 zeolites with different SiO2/Al2O3 molar ratios have been hydrothermally synthesized by an organic surfactant with a diquaternary ammoniumgroup. The samples were characterized by X-ray diffraction (XRD), N2 adsorption-desorption, X-ray fluorescence spectroscopy (XRF), scanning electron microscopy (SEM) and 27Al magic angle spinning nuclear magnetic resonance (27Al MAS-NMR) techniques. The synthesis conditions of the nanosheets ZSM-5 were studied, including the synthesis factors such as crystallization temperature and time, the amount of structure-directing agent (SDA) and alkalinity. The results showed that shorter crystallization times were required when synthesis was conducted at higher crystallization temperatures, higher SiO2/Al2O3 ratios, larger amounts of structure-directing agent were used, and higher SiO2/Al2O3 ratios. The morphology, BET and mesopore volume changed with increasing SiO2/Al2O3.

Key words: Nanosheet, ZSM-5 zeolite, Synthetic chemistry, SiO2/Al2O3 ratio

MSC2000: 

  • O641