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过程工程学报 ›› 2018, Vol. 18 ›› Issue (5): 1082-1087.DOI: 10.12034/j.issn.1009-606X.217433

• 材料工程 • 上一篇    下一篇

混合表面活性剂体系合成锆掺杂介孔分子筛

刘 悦1， 曹 磊2， 李 达2， 曹 坤2， 隋富生3， 赵 伟2*， 吕 伟1*， 齐 涛2   

  1. 1．山东大学化学与化工学院，山东 济南 250061 2．中国科学院过程工程研究所，北京 100190 3．中国科学院声学研究所，北京 100190
  • 收稿日期:2017-12-15 修回日期:2018-02-05 出版日期:2018-10-22 发布日期:2018-10-12
  • 通讯作者: 吕伟 lwei@sdu.edu.cn
  • 基金资助:
    科技部科技支撑项目;中国科学院科技服务网络计划（STS计划）;中国科学院云南省科技合作项目;铜仁市专项研发项目

Synthesis of zirconium substituted mesoporous molecular sieve using mixed surfactants as templates

Yue LIU1, Lei CAO2, Da LI2, Kun CAO2, Fusheng SUI3, Wei ZHAO2*, Wei LÜ1*, Tao QI2   

  1. 1. School of Chemistry and Chemical Engineering, Shandong University, Jinan, Shandong 250061, China 
    2. Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China 
    3. Institute of Acoustics, Chinese Academy Sciences, Beijing 100190, China
  • Received:2017-12-15 Revised:2018-02-05 Online:2018-10-22 Published:2018-10-12
  • Contact: Lv 1Wei lwei@sdu.edu.cn

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摘要： 在水热体系中研究了以阳离子表面活性剂为主，阴离子表面活性剂、非离子表面活性剂、中性伯胺等为辅的混合表面活性剂对合成锆掺杂介孔分子筛的影响，考察了水/SiO2摩尔比、晶化温度、晶化时间及混合表面活性剂/SiO2摩尔比对所制分子筛结构的影响，对优化条件下合成的样品进行了表征. 结果表明，锆掺杂介孔分子筛的最佳合成体系为阴阳离子表面活性剂混合体系，最佳合成配方为水/SiO2摩尔比58，混合表面活性剂/SiO2摩尔比0.15, 100℃下晶化48 h. 最佳条件下合成的样品在小角区域有一个明显的衍射峰，表明其具有一定的长程有序性，晶面间距d=9.71 nm，平均孔径为5.55 nm，壁厚4.16 nm，具有三维蠕虫状孔道结构，吸附亚甲基蓝、罗丹明B与甲基橙的混合溶液时，对亚甲基蓝的吸附选择性较好，吸附率达90.24%.

关键词: 锆掺杂介孔分子筛, 混合表面活性剂, 水热合成

Abstract: The rapid economic development has also brought many environmental problems while providing people with a high quality of life. In particular, a large number of industrial solid wastes have become increasingly prominent. This facilitates the synthesis of highly active and doped mesoporous molecular sieves inexpensively because some industrial solid wastes contain both silicon species and transition metal elements. In this paper we used mixed surfactants system as template and the industrial silicon slag with zirconium as raw material for the synthesis process of zirconium substituted mesoporous molecular sieve. In the synthesis process, cationic surfactants (cetyltrimethylammonium bromide CTAB was used in this paper) were mainly used, and other surfactants (such as nonionic surfactant polyphenol vinyl ether-10, OP-10; neutral primary amine dodecylamine, DDA, and anionic surfactant sodium dodecyl benzene sulfonate, SDBS and sodium dodecyl sulfate SDS) supplemented, the effect of different mixed surfactants systems on the synthesis of zirconium substituted mesoporous molecular sieves in hydrothermal system were studied. In order to improve the synthesis repeatability, the effects of various factors on the proprietary of zirconium substituted mesoporous molecular sieves, such as the molar ratios of water to silicon and mixed surfactants to SiO2, crystallization temperature and crystallization time were also studied. The sample obtained under optimum conditions were characterized with different methods. The results showed that the optimized synthesis system was the mixed anionic and cationic surfactants (CTAB and SDBS), the suitable mole ratios of surfactant/SiO2 and H2O/SiO2 were 0.15 and 58, respectively. The optimized crystallization temperature and time were 100℃ and 48 h. The zirconium substituted mesoporous molecular sieves had a clear diffraction peak in the low angle region, indicating that the sample had a certain long-range order. The interplanar spacing d was 9.71 nm, the average pore diameter was 5.55 nm and the wall thickness was 4.16 nm. The zirconium substituted sample had a three-dimensional worm-like pore structure. For the mixed dyes solution of methylene blue, rhodamine B and methyl orange, the sample showed a good selective adsorption ability to methylene blue, the adsorption rate was 90.31%.

Key words: Zirconium substituted mesoporous molecular sieve, mixed surfactants, hydrothermal synthesis