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Issue 14, 2002
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In situ XANES study on TiO2–SiO2 aerogels and flame made materials

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Abstract

The structures of TiO2–SiO2 based aerogels and flame made particles, used as epoxidation catalysts, are compared by X-ray absorption near edge structure (XANES) spectroscopy and in situ XANES during dehydration of the calcined catalyst samples. The results are interpreted in terms of the titanium species present in the catalyst and the catalytic performance in the test reaction, the epoxidation of 2-cyclohexene-1-ol by tert-butylhydroperoxide (THBP) at 90 °C. XANES shows that tetrahedral titanium sites are the favoured sites at low TiO2 concentrations (1–3.2 wt.% in this study). The catalytic performance (turnover frequency, selectivity) of such aerogels or flame made materials with low TiO2 content is much better than that of corresponding samples with high TiO2 content. In aerogels, regardless of the TiO2 content, the amount of titanium with tetrahedral coordination increases significantly after dehydration at elevated temperature. In contrast, the pre-edge height and its position in the XANES spectra of the flame made catalyst samples is comparable, even without dehydration, to that of TS-1, which contains titanium in tetrahedral coordination. Thus the extent of tetrahedral Ti is intrinsically high in flame made catalysts and increases only slightly during the drying process. This behaviour can be attributed to the hydrophobic character of the flame made materials and ameliorates the catalytic performance, i.e. the selectivity.

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Publication details

The article was received on 18 Feb 2002, accepted on 18 Apr 2002 and first published on 05 Jun 2002


Article type: Paper
DOI: 10.1039/B201760A
Citation: Phys. Chem. Chem. Phys., 2002,4, 3514-3521
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    In situ XANES study on TiO2–SiO2 aerogels and flame made materials

    J. Grunwaldt, C. Beck, W. Stark, A. Hagen and A. Baiker, Phys. Chem. Chem. Phys., 2002, 4, 3514
    DOI: 10.1039/B201760A

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