WO3/ZrO2 systems were prepared by sol–gel technique using different procedures for the solvent extraction: evaporation in vacuum at room temperature (xerogel) and extraction in supercritical conditions (aerogel). Two reactions of industrial interest were investigated under mild conditions: (i) acylation of veratrole with acetic anhydride; (ii) acylation of anisole with benzoic anhydride. Several techniques were employed in order to study the influence of the synthetic parameters on texture and catalytic activity: N2 physisorption, Fourier transformed-infrared spectroscopy, X-ray photoelectron spectroscopy, temperature programmed reduction and temperature programmed oxidation analyses. The solvent extraction strongly influences metal reducibility, surface area, pores organisation, W/Zr surface density and metallic interactions. The aerogel sample shows the best catalytic results for both conversion and yield. The supercritical extraction plays a central role especially in the recycling: by proper air activation, the aerogel sample attains the complete restoration of the catalytic activity even after three runs.
Aerogel and xerogel WO3/ZrO2 samples for fine chemicals production / M. Signoretto, E. Ghedini, F. Menegazzo, G. Cerrato, V. Crocellà, C.L. Bianchi. - In: MICROPOROUS AND MESOPOROUS MATERIALS. - ISSN 1387-1811. - 165(2013), pp. 134-141. [10.1016/j.micromeso.2012.08.003]
Aerogel and xerogel WO3/ZrO2 samples for fine chemicals production
C.L. BianchiUltimo
2013
Abstract
WO3/ZrO2 systems were prepared by sol–gel technique using different procedures for the solvent extraction: evaporation in vacuum at room temperature (xerogel) and extraction in supercritical conditions (aerogel). Two reactions of industrial interest were investigated under mild conditions: (i) acylation of veratrole with acetic anhydride; (ii) acylation of anisole with benzoic anhydride. Several techniques were employed in order to study the influence of the synthetic parameters on texture and catalytic activity: N2 physisorption, Fourier transformed-infrared spectroscopy, X-ray photoelectron spectroscopy, temperature programmed reduction and temperature programmed oxidation analyses. The solvent extraction strongly influences metal reducibility, surface area, pores organisation, W/Zr surface density and metallic interactions. The aerogel sample shows the best catalytic results for both conversion and yield. The supercritical extraction plays a central role especially in the recycling: by proper air activation, the aerogel sample attains the complete restoration of the catalytic activity even after three runs.File | Dimensione | Formato | |
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