以桥联硅氧烷1,1'-双[(2-三乙氧基硅基)乙基]二茂铁(BTEF)和正硅酸乙酯为前驱体,以十六烷基三甲基溴化铵为结构导向剂,采用共聚法制备了二茂铁功能化的周期介孔有机硅烷材料(PMO-Fc).同时以BTEF为修饰剂,以甲苯为分散剂,采用嫁接法制备了Fc-MCM-41杂化介孔材料.采用N2物理吸附、X射线衍射、透射电镜和红外光谱等手段对材料进行了表征,评价了其催化苯羟化反应活性.结果表明,PMO-Fc具有有序的二维六方形孔道结构,较大的比表面积和孔体积,在苯羟化反应中表现出比Fc-MCM-41更高的催化活性,苯酚的选择性和收率分别为65.3%和20.2%.
A new Ferrocene(Fc)-containing periodic mesoporous organosilica(PMO-Fc) was synthesized directly through co-condensation of 1,1'-bis[2-(triethoxylsilyl)ethyl]ferrocene and tetraethyl orthosilicate using supramolecular templates of cetyltrimethylammonium bromide as structure directing agents.A hybrid material,Fc-MCM-41,was also prepared by covalently anchoring ferrocene onto the mesoporous silica material MCM-41 using toluene as the dispersant.The prepared materials were characterized by nitrogen adsorption,X-ray diffraction,transmission electron microscopy,and Fourier transform infrared spectroscopy.The results showed that PMO-Fc had an ordered two-dimensional hexagonal mesostructure,higher BET surface area and pore volume.In the hydroxylation of benzene to phenol,PMO-Fc was highly active with 65.3% of phenol selectivity and 20.2% of phenol yield.