采用甲醇法制备三维有序大孔结构(3DOM)Ti O2,再经过有机胺(Et O)3Si(CH2)3NH2(APS)功能化修饰后,通过自组装技术将取代型杂多酸盐K5[Ni(H2O)PW11O39](PW11Ni)固载上去,从而制备了三维有序大孔取代型多金属氧酸盐-有机胺-Ti O2杂化催化剂3DOM PW11Ni-APS-Ti O2。通过FT IR,ICP-AES,XRD,UV-Vis/DRS,XPS和SEM等测试手段对其组成、结构和形貌等进行了表征。结果表明,通过自组装技术将APS功能化修饰的3DOM Ti O2与杂多酸盐PW11Ni负载后,该杂多酸盐PW11Ni通过Ni-N配位键与3DOM Ti O2键合。同时,所制备的3DOM PW11Ni-APS-Ti O2具有Ti O2锐钛矿结构,且该合成产物由于模板剂聚苯乙烯(PS)胶球的作用呈现着规则、有序和开放性的三维有序大孔结构,其通透性的孔结构十分有利于反应过程中反应物和产物分子的扩散。紫外光催化降解若丹明B实验结果表明,3DOM PW11Ni-APS-Ti O2的紫外光催化降解活性明显高于直接光解和其他对比体系。
The 3D ordered macroporous (3DOM) TiOz was prepared in methanol bath with soaking polystyrene (PS) spheres, and it was further funetionalized using 3-aminopropyhriethoxysilane (APS). Amine-functionalized 3DOM TiO2 material impregnated with K5 [ Ni( H2O) PW11O39 ] (PW11Ni) was prepared by coordination of nickel of POM, with the amine groups on the surface of 3DOM TiO2. The obtained material was well characterized by FT IR, XRD, UV-Vis/DRS, XPS, and SEM. The results showed that the primary Keggin structure was remained intact in as-prepared composite, at the same time, PW11 Ni was successfully bonded on 3DOM TiO2by Ni-N bond with APS as the coupling agent. 3DOM PW11 Ni-APS-TiO2 had anatase crystalline structure; moreover, the 3DOM structure was the opening and permeability macroporous which could significantly improve the accessibility of diffusing species. Compared to PW11Ni, 3DOM TiO2 and PW11Ni-APS-TiO2, the activity of 3DOM PW11Ni-APS-TiO2 was better under UV photocatalytic degradation of Rhodamine B.