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Incorporation of cubane-type Mo3S4 molybdenum cluster sulfides in the framework of mesoporous silica

机译:在介孔二氧化硅的骨架中加入立方烷型mo3s4钼簇硫化物

摘要

A new molybdenum siloxo cluster of formula [Mo3S4(dmpe)3(MPTES)3]PF6 (dmpe = 1,2-(bis)dimethylphosphinoethane; MPTES = (3-mercaptopropyl)triethoxysilane) has been synthesized with the ultimate goal of incorporating it into ordered mesoporous silica via covalent attachment. For this purpose, two different approaches, in situ and grafting, are employed. The first one is based in the co-condensation of the Mo3S4 siloxo cluster and tetraethylorthosilicate (TEOS) as mixed silicon sources in the presence of a surfactant (CTAB). The use of this approach allows for the incorporation of the Mo3S4 siloxo cluster into the structure of the mesoporous silica. For comparison purposes, the same Mo3S4 siloxo cluster has been immobilized on the surface of conventional mesoporous silica MCM-41, using more traditional grafting techniques. The physical and structural properties of both series of materials, containing different Mo3S4 cluster loadings, have been thoroughly investigated by means of powder X-ray diffraction (XRD), N2 adsorption/desorption isotherms, transmission electron microscopy (TEM), magic-angle spinning (MAS) 31P and CP/MAS 29Si NMR, Fourier transform infrared (FT-IR) and UV–Vis diffuse reflectance (DRUV–Vis) spectroscopies. The chemical and structural integrity of the diphosphino Mo3S4 siloxo cluster is preserved in both the in situ and grafted mesoporous silica based materials. Depending on the incorporation approach, immobilization of the trinuclear sulfido cluster occurs into the silica matrix structure for the in situ materials or on the surface for the grafted ones. With these results, we show that it is possible to extend the incorporation of chemical functionalities into the structure of mesoporous materials to Mo3S4 siloxo clusters.
机译:合成了一个新的式[Mo3S4(dmpe)3(MPTES)3] PF6的钼硅氧烷基团(dmpe = 1,2-(双)二甲基膦基乙烷; MPTES =(3-巯基丙基)三乙氧基硅烷)通过共价连接成有序介孔二氧化硅。为此,采用了两种不同的方法,即原位和接枝。第一个是在表面活性剂(CTAB)存在下,Mo3S4硅氧烷簇和原硅酸四乙酯(TEOS)作为混合硅源的共缩合。该方法的使用允许将Mo 3 S 4硅氧烷簇结合到中孔二氧化硅的结构中。为了进行比较,使用更传统的接枝技术,将相同的Mo3S4 Siloxo团簇固定在常规中孔二氧化硅MCM-41的表面上。通过粉末X射线衍射(XRD),N2吸附/解吸等温线,透射电子显微镜(TEM),魔角旋转等手段,对包含不同Mo3S4团簇负载的两种材料的物理和结构性质进行了彻底研究。 (MAS)31P和CP / MAS 29Si NMR,傅里叶变换红外(FT-IR)和UV-Vis漫反射(DRUV-Vis)光谱。在原位和接枝介孔二氧化硅基材料中都保留了二膦基Mo3S4硅氧烷簇的化学和结构完整性。根据掺入方法的不同,三核硫基团簇的固定发生在原位材料的二氧化硅基质结构中或接枝材料的表面上。通过这些结果,我们表明可以将化学官能团的结合扩展到Mo3S4 siloxo团簇的介孔材料结构中。

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