Fe-HMS的合成、表征及催化苯酚羟基化  

Synthesis,Characterization and Catalytic Phenol Hydroxylation Performance of Iron-modified Hexagonal Mesoporous Silica

作　　者：陈君华[1] 丁志杰[1] 郭雨[1] 王飞[2] 伏再辉[3] 

机构地区：[1]安徽科技学院化学系,安徽蚌埠233100 [2]南京林业大学化工学院,江苏南京210037 [3]湖南师范大学化学化工学院,湖南长沙410081

出　　处：《精细化工》2010年第4期346-352,共7页Fine Chemicals

基　　金：安徽省高校自然科学基金(2001Kj059);安徽科技学院重点学科基金(YZD2004-21)~~

摘　　要：以正硅酸乙酯(TEOS)、三氯化铁为原料,十二胺(DDA)为模板剂,采用溶胶-凝胶法合成了铁改性六方介孔硅分子筛(Fe-HMS),利用XRD、FTIR、UV-vis、ESR、TG-DTA、ESEM、TEM及N2吸附-脱附技术对材料结构进行了表征,同时以苯酚羟基化反应为探针考察了Fe-HMS的催化性能。结果表明,Fe-HMS材料由细小的球状纳米粒子组成,材料具有稳定的六方介孔结构,铁已进入六方介孔硅(HMS)载体的骨架;在苯酚羟基化反应中材料显示出较高的催化活性,苯酚的转化率最高可达46.9%,催化剂经450℃焙烧2 h即可再生,重复使用7次苯酚转化率仍可达36.4%。An iron-modified hexagonal mesoporous silica（Fe-HMS） was prepared by the sol-gel method with tetraethyl orthosilicate（TEOS）,iron trichloride and template reagent of dodecyl amine（DDA） as the raw materials.The physicochemical properties of the synthesized Fe-HMS were characterized by XRD,FTIR,UV-vis,ESR,TG-DTA,ESEM,TEM and the nitrogen adsorption-desorption testing technology.In addition the catalytic performance of the Fe-HMS on the reaction of phenol hydroxylation was also investigated.The results showed that the prepared Fe-HMS was spherical small particles with stable hexagonal mesoporous structure,and the irons were embedded into the frameworks of the HMS.Furthermore,the Fe-HMS exhibited a higher catalytic activity in the hydroxylation reactions of phenol,and the highest conversion ratio of phenol reached 46.9%.The catalyst could be regenerated after being calcined at 450 ℃ for 2 h.The conversion of phenol still could reach 36.4% even after seventh cycle.

关 键 词：六方介孔硅(HMS) 表征 催化 苯酚 羟基化 

分 类 号：O643.3[理学—物理化学] TQ138[理学—化学]