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H3PW12O40 supported on mesoporous MCM-41 and Al–MCM-41 materials: preparation and characterisation

机译:H3 PW12 O40 介孔MCM-41和Al–MCM-41材料的负载:制备和表征

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摘要

MCM-41 and Al–MCM-41 has been synthesized using cetyl-trimethylammonium bromide (CTAB) surfactant as template and adding the silica precursor to aqueous solutions containing CTAB. The obtained solids were calcined at 600 °C for 4 h. HPW heteropolyacid supported on the mesoporous were prepared using the incipient wetness method. The characterization of materials was performed by X-ray diffraction, Transmission Electron Microscopy, N2 adsorption, 29Si Cross Polarization–Magic Angle Spinning and 27Al MAS NMR. Results showed that the hexagonal structure is obtained in both cases. The Aluminium species are located inside an extra-framework. The impregnation reduces the surface area of the mesoporous materials especially of the Al–MCM-41 suggesting a participation of aluminium during the impregnation. HPW is well dispersed in the mesoporous materials and is located inside the pores interacting with the silanol group of the pores wall. 27Al MAS NMR measurements have showed that the impregnation causes the removal of the non-framework aluminium.
机译:MCM-41和Al-MCM-41已使用十六烷基三甲基溴化铵(CTAB)表面活性剂作为模板,并将二氧化硅前体添加到含有CTAB的水溶液中合成。将获得的固体在600℃下煅烧4小时。使用初期润湿法制备了负载在中孔上的HPW杂多酸。通过X射线衍射,透射电子显微镜,N2 吸附,29 交叉极化-魔角旋转和27 MAS NMR对材料进行表征。结果表明,在两种情况下均获得了六边形结构。铝材位于额外的框架内。浸渍减少了介孔材料的表面积,特别是Al–MCM-41的表面积,这表明铝在浸渍过程中会参与其中。 HPW很好地分散在中孔材料中,并且位于孔内,与孔壁的硅烷醇基相互作用。 27 Al MAS NMR测量表明,浸渍会除去非骨架铝。

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  • 来源
    《Journal of Materials Science》 |2011年第22期|p.7114-7120|共7页
  • 作者单位

    Institute of Biodiversity and Ecosystems Research, Bulgarian Academy of Sciences, Sofia, Bulgaria;

    Dipartimento di Chimica “S. Cannizzaro”, Università di Palermo and INSTM-Udr Palermo, Parco d’Orleans II Viale delle Scienze pad 17, 90128, Palermo, Italy;

    Centro Grandi Apparecchiature—UniNetLab, Università di Palermo, Via F. Marini 14, 90128, Palermo, Italy;

    Centro Grandi Apparecchiature—UniNetLab, Università di Palermo, Via F. Marini 14, 90128, Palermo, Italy;

    Dipartimento di Chimica “S. Cannizzaro”, Università di Palermo and INSTM-Udr Palermo, Parco d’Orleans II Viale delle Scienze pad 17, 90128, Palermo, Italy;

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