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

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.