物理化学学报 >> 2009, Vol. 25 >> Issue (01): 137-144.doi: 10.3866/PKU.WHXB20090125

研究论文 上一篇    下一篇

离子胶束诱导微波合成SAPO-11分子筛微球

罗小林; 陈亚芍; 常鹏梅; 杨德锁; 姜娈   

  1. 宝鸡文理学院化学化工系, 陕西 宝鸡 721013; 应用表面与胶体化学教育部重点实验室, 陕西师范大学化学与材料科学学院, 西安 710062
  • 收稿日期:2008-07-03 修回日期:2008-10-06 发布日期:2008-12-31
  • 通讯作者: 罗小林 E-mail:luoxl225@163.com

Synthesis of SAPO-11 Molecular Sieve Microspheres Using a Microwave Technique and Mediated by Ionic Micelles

LUO Xiao-Lin; CHEN Ya-Shao; CHANG Peng-Mei; YANG De-Suo; JIANG Luan   

  1. Department of Chemistry and Chemistry Engineering, Baoji University of Arts and Sciences, Baoji 721013, Shaanxi Province, P. R. China; Key Laboratory of Applied Surface and Colloid Chemistry, Ministry of Education, School of Chemistry and Materials Science, Shaanxi Normal University, Xi’an 710062, P. R. China
  • Received:2008-07-03 Revised:2008-10-06 Published:2008-12-31
  • Contact: LUO Xiao-Lin E-mail:luoxl225@163.com

摘要: 以十六烷基三甲基氯化铵(CTAC)与正丁醇(n-butanol)形成的胶束为外模板, 采用微波法制备了SAPO-11分子筛微球.考察了CTAC浓度、晶化时间以及HF用量对SAPO-11分子筛形成的影响, 并利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、热分析(TG-DTA)、电子衍射能谱(EDS)和N2物理吸附等技术对所得产物进行了系统表征. 结果表明: 当c(CTAC)+c(n-butanol)=0.180 mol·L-1时可得到结晶度较高的SAPO-11分子筛微球; 延长反应时间, 所得产物结晶度逐渐提高; 适量的HF, 有助于分子筛中Si物种的取代以及分子筛微球的形成. 通过对比实验, 提出了离子胶束诱导微波合成SAPO-11分子筛微球的反应机理.

关键词: 胶束, SAPO-11 分子筛, 微球, 微波合成

Abstract: Micelles formed by cetyltrimethylammoniumchlorine (CTAC) and n-butanol were used as shape-directing templates to synthesize SAPO-11 molecular sieve microspheres by a microwave technique. Effects of CTAC concentration, time of crystallization, and dosage of HF were investigated. Properties of the products were characterized systematically by X-ray powder diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), thermal analysis (TG-DTA), electron diffraction spectroscopy (EDS) and N2 physisorption. When c(CTAC)+c(n-butanol)=0.180 mol·L-1, SAPO-11 molecular sieve microspheres with the preferred crystallinity were obtained. The crystallinity of the synthesized SAPO-11 molecular sieve microspheres was improved by prolonging the reaction time. The substitution of Si species and the crystallization of SAPO-11 molecular sieve microspheres were also improved by appropriate usage of HF. Using control experiments, the reaction mechanism for the crystallization of SAPO-11 molecular sieve microspheres as mediated by ionic micelles and using the microwave technique is proposed.

Key words: Micelle, SAPO-11 molecular sieve, Microsphere, Microwave synthesis

MSC2000: 

  • O647