物理化学学报 >> 2012, Vol. 28 >> Issue (09): 2108-2114.doi: 10.3866/PKU.WHXB201206181

催化和表面科学 上一篇    下一篇

无有机模板剂水热合成Co同晶取代的丝光沸石分子筛

王琦1, 吴雅静2, 王军1, 林晓1   

  1. 1. 南京工业大学化学化工学院, 材料化学工程国家重点实验室, 南京 210009;
    2. 南京工业大学理学院, 南京 210009
  • 收稿日期:2012-04-26 修回日期:2012-06-18 发布日期:2012-08-02
  • 通讯作者: 王军 E-mail:junwang@njut.edu.cn
  • 基金资助:

    国家自然科学基金(21136005, 21101094, 20976084)资助项目

Organotemplate-Free Hydrothermal Synthesis of Isomorphously Co-Substituted Mordenite Molecular Sieve

WANG Qi1, WU Ya-Jing2, WANG Jun1, LIN Xiao1   

  1. 1. State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009, P. R. China;
    2. College of Sciences, Nanjing University of Technology, Nanjing 210009, P. R. China
  • Received:2012-04-26 Revised:2012-06-18 Published:2012-08-02
  • Contact: WANG Jun E-mail:junwang@njut.edu.cn
  • Supported by:

    The project was supported by the National Natural Science Foundation of China (21136005, 21101094, 20976084).

摘要:

在硅酸钠、硫酸铝、硝酸钴和氢氧化钠的全无机体系条件下, 采用无有机模板剂水热法合成了Co同晶取代的丝光沸石分子筛. 通过粉末X射线衍射(XRD)、扫描电子显微镜(SEM)、电感耦合等离子体(ICP)光谱、氮气吸附、紫外-可见(UV-Vis)光谱、热重(TG)分析等手段对所得固体产物的织构性质以及钴在分子筛中的存在状态进行了表征. 结果表明, 该方法成功地将Co离子引入到丝光沸石分子筛的骨架结构中, 未发现骨架外Co物种. 典型的合成条件为n(Co)/n(SiO2) =0.01-0.04, n(SiO2)/n(Al2O3) =20-50, n(H2O)/n(SiO2) =40, n(Na2O)/n(SiO2)=0.4, 晶化温度170 °C, 晶化时间3-7 d. 讨论了Na+离子在无有机模板剂合成中的结构导向作用. 全无机体系合成得到的产物无需进行传统的高温煅烧处理, 即可获得开放的微孔孔道, 实现了低成本、低能耗、环境友好的Co-丝光沸石的合成.

关键词: 微孔材料, 化学合成, 晶体生长, X射线衍射, 杂原子沸石

Abstract:

An organotemplate-free hydrothermal route was investigated for synthesizing isomorphously Co-substituted mordenite molecular sieve using only the inorganic raw materials such as sodium silicate, aluminum sulfate, cobalt nitrate, and sodium hydroxide. Textural properties and Co ion states for the obtained solid products were characterized by powder X-ray diffraction (XRD), scanning electron microscope (SEM), inductively coupled plasma (ICP), nitrogen adsorption, ultraviolet-visible (UV-Vis) spectra, and thermogravimetric (TG) analysis. The results showed that Co ions were incorporated into the framework structure of the mordenite without the presence of extra-framework Co species. Typical synthesis conditions were n(Co)/n(SiO2)=0.01-0.04, n(SiO2)/n(Al2O3)=20-50, n(H2O)/n(SiO2)=40, n(Na2O)/ n(SiO2) =0.4, crystallization temperature 170 ° C, and crystallization time 3-7 d. The structure-directing function of Na+ ions in the absence of an organic template was discussed. Products obtained by the present allinorganic systems possess open micropores and do not require traditional high-temperature calcination. Thus, we demonstrate a low cost, low energy consumption, and environmentally benign synthesis of Co-mordenite.

Key words: Microporous material, Chemical synthesis, Crystal growth, X-ray diffraction, Heteroatomic zeolite

MSC2000: 

  • O643.36