Ti-Fe-β沸石的合成与结构表征  

Synthesis and Structural Characterization of Ti-Fe-β Zeolites

作　　者：何红运[1] 于为[1] 何震[1] 

机构地区：[1]湖南师范大学化学生物学及中药分析教育部重点实验室,中国长沙410081

出　　处：《湖南师范大学自然科学学报》2009年第3期63-67,共5页Journal of Natural Science of Hunan Normal University

基　　金：国家大学生创新实验计划项目(071054226);湖南省自然科学基金资助项目(08JJ3026)

摘　　要：分别以白炭黑为硅源,四乙基氢氧化铵为模板剂,硫酸钛为钛源,硫酸铁为铁源和氟化钠为矿化剂,采用水热法合成了Ti-Fe-β沸石,探讨了合成条件对Ti-Fe-β沸石形成的影响,运用XRD、IR、UV-Vis固体紫外/可见漫反射光谱、TG/DTA、SEM和ICP等多种测试技术对样品的结构进行了表征,测定了样品中Ti和Fe的含量.结果表明,按下列化学组成配制初始反应混合物:60SiO2∶xTiO2∶xFe2O3∶y(TEA)2O∶zH2O∶wNaF,0.5≤x≤1,y≥12,480≤z≤720,24≤w≤0.6,将所得胶状物质转入带聚四氟乙烯衬里的20mL不锈钢反应釜中,在413K晶化12d,可制备出Ti-Fe-β沸石,所合成的样品具有BEA拓扑结构,结晶良好,Ti和Fe原子进入了沸石骨架.Ti-Fe-β zeolite were synthesized under hydrothermal conditions with fumed silica （ SiO2 ） as the silica source, tetraethyl ammonium hydroxide （TEAOH） as the template, titanium sulfate as the titanium source, ferric sulfate as the iron source and sodium fluoride（NaF） as mineral agent respectively. The influence of synthesis condition on the crystallization of Ti-Fe-β zeolite was investigated.. The iron and titanium content and structural characterization of products were determined by ICP, XRD, IR, TG/DTA, SEM and UV-Visible diffuse reflectance spectra. The results indicate that Ti-Fe-β zeolite can be synthesized as following synthesis procedure：the starting reaction mixture with following chemical composition was prepared：60SiO2：2 x TiO2： x Fe2O3：y （TEA）2O： z H20： w NaF, 0.5 ≤ x ≤ 1, y 1≥ 12,480 ≤ z ≤ 720,24 ≤ w ≤ 0.6, the gels obtained was then transferred to a tetrafluoroethylene-lined 20 mL stainless-steel autoclave and kept in an oven at 413 K for 12 d. The samples synthesized contain a BEA phase of good species, and suggest the presence of Ti and Fe atoms in framework position.

关 键 词：水热合成 Ti—Fe-β沸石 分子筛 

分 类 号：O611.4[理学—无机化学]