以苯基桥联硅氧烷[1,4-bis(trimethoxysilyl)benzene,BTSB]和三嵌段共聚物聚氧乙烯-聚氧丙烯-聚氧乙烯(EO20PO70EO20,P123)分别作为硅源和模板剂,在无酸体系中利用ZrOCl2-K2SO4的协同作用方便制得二维六方苯环桥联型杂化介孔材料(periodic mesoporous organosilicas,PMOs)。通过高分辨透射电镜、小角X射线散射、N2吸附-脱附等温线、固体13C交叉极化和29Si核磁共振技术等分析手段系统表征PMOs的结构性能。分析结果表明:保持摩尔比n(K2SO4):n(Si)=2,可在n(Zr):n(Si)=0.01~0.10时制备高度规整的苯环桥联型杂化材料。基于ZrOCl2自身水解生成的弱酸性环境和K2SO4对P123胶束的作用特点,探讨无机盐组合在研究体系中的协同促进机制。
Ordered benzene-bridged periodic mesoporous organosilicas(PMOs) with hexagonal frameworks were prepared with as-sistance of ZrOCl2-K2SO4 salt pairs using nonionic P123(EO20PO70EO20) and 1,4-bis(trimethoxysilyl)benzene(BTSB) as a structure-directing agent and silica precursor,respectively.The product was thoroughly characterized by the small-angle X-ray scattering,high-resolution transmission electron microscopy and N2-adsorption/desorption isotherms,as well as solid state 13C cross polariza-tion/29Si magic angle spinning nuclear magnetic resonance spectroscopy techniques.Analysis results show that,with mole ratio n(K2SO4):n(Si)=2,high-quality benzene-bridged PMOs are easily prepared within a wide range of n(Zr):n(Si)=0.01-0.10,thus clearly illustrating the cooperative effect of both salts in assembly of the hybrid mesostructure in the proposed synthesis system.