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作 者:许宜铭[1]
机构地区:[1]浙江大学化学系
出 处:《高等学校化学学报》1999年第5期670-674,共5页Chemical Journal of Chinese Universities
摘 要:用不同pH值的混合物制备了不同孔径的全硅MCM-41和不同金属离子取代的M-MCM-41(M=Al,Mn,Fe和V)分子筛.这些试样均呈现MCM-41的X射线粉末衍射特征峰和Ⅳ型氮气吸附等温线,但混有不同含量的无定形氧化硅.样品中MCM-41晶体的含量与溶胶的pH值和所用表面活性剂的碳链链长有关.骨架硅的金属离子取代降低了MCM-41的有序度。Siliceous MCM 41 samples with two different pore size and metal substituted MCM 41 samples with different metals have been synthesized at different pH of the mixture, and characterized by X ray powder diffraction and nitrogen adsorption analysis. The results show that all the samples exhibit a typical XRD diffraction of MCM 41 and an adsorption isotherm of type Ⅳ, but there exists a considerable amount of amorphous silica in the samples. The sample prepared at pH=11(MCM 3) shows the best in quality among the others, and has less content of amorphous silica phase. When the MCM 3 is regarded as a standard, the sample prepared without pH adjustment contains only 36% of pure MCM 41 crystallites, while the sample prepared at pH=10.5 has 84% of pure MCM 41 phase. It has also been observed that the quality of the resulted samples is decreased when a shorter chain surfactant is used. When the metal substituted M MCM 41 (M=Al, Mn, Fe, V) is prepared at pH=11, their quality can be improved. However, the diffraction intensity of d 100 phase is still lower than that of the corresponding siliceous MCM 41, and decreases accordingly from Al to V.
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