117,420 research outputs found

    Surface acidity modifications induced by thermal treatments and acid leaching on microcrystalline H-BEA zeolite. A FT-IR, XRD and MAS-NMR study

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    Samples of beta-zeolite thermally treated at di†erent temperatures and acid leached with diluted hydrochloric acid solution have been investigated by XRD, 27Al MAS-NMR spectroscopy and FTIR spectroscopy. The results have been used to interpret the behaviour of the samples as catalysts for the acylation of 2-methoxynaphthalene. It has been shown that the as prepared sample presents two types of extraframework species. These are identiÐed as Al hydroxo-ions highly dispersed in the internal zeolite channels and Al oxide nanoparticles. Calcination causes dealumination of the framework and progressive conversion of the Al hydroxo-ions into Al oxide nanoparticles that reduce the zeolite channels practicability, modifying the shape selectivity e†ect. The acid sites present in the sinusoidal channels cm BrÔnsted (l ~1) can be OH \ 3608 distinguished from those located in the larger ones cm (l ~1), due to the inability of the bulky OH \ 3620È3612 probe molecule pivalonitrile to enter the former. However, internal terminal silanols cm (l ~1) also OH \ 3735 apparently display a signiÐcant acidity, deÐnitely higher than the acidity of those absorbing at 3747 BrÔnsted cm~1, thought to be located at the external crystal surface. The strongest Lewis acidity is displayed by the aluminum hydroxo-ions, while that of alumina nanoparticles is a little weaker. Acid-leached beta-zeolite also displays a medium strength Lewis acidity, likely due to framework Al cations. Thus a partial reinterpretation of the real structure of beta-zeolite and a partial reassignment of the bands due to the surface hydroxy groups are proposed

    VAPOR-PHASE PROPENE HYDROFORMYLATION CATALYZED BY THE RH/AL SYSTEM ON SILICA

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    A Rh/Al system with rhodium nanocrystals was prepared by reducing rhodium trichloride supported on silica with lithium aluminum hydride at low temperature in THF. After pretreatment in Ar and in CO/H2 the system was found to be an active catalyst of vapour phase propene hydroformylation at atmospheric pressure. The nature and composition of the active surface was studied by X-ray diffraction, X-ray photoemission spectroscopy (XPS) and Fourier transform-IR spectroscopy. Regioselectivity and chemoselectivity data are correlated to the proposed nature and morphology of the active sites of the catalyst derived from spectroscopic data. The Rh/Al system is compared with the Rh/B system we described in preceding papers. © 1993

    STRUCTURAL STUDIES OF AL-BASED POWDERS PREPARED BY CHEMICAL METHODS

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    Finely dispersed metal powders have been obtained after chemical reduction of Ni and Co acetylacetonate by lithium aluminum hydride in tetrahydrofuran at low temperature. The Al/Ni and Al/Co stoichiometry of the as-reduced powders was 1.1 and 1.2, respectively. The structure and thermal stability of the as-reduced powders were affected by the temperature of reduction. For the NiAl powders it was found that the thermal treatment initially induces a separation of highly unstable Ni(Al) and Al(Ni) solid solutions, which subsequently react to give a single NiAl phase of cubic structure not reported in the equilibrium phase diagram. Conversely, the reduction of cobalt acetylacetonate directly gives a cubic metastable phase, from which precipitates some hexagonal form of Co after treatment at 450-degrees-C
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