The degradation of high phenol concentrations (I g/L) in water solutions by TiO2 photocatalysis and the photo-Fenton reaction has been studied. From the obtained data it may be suggested that degradation of phenol by TiO2-UV takes place onto the catalyst surface by means of peroxo-compounds formation. At low phenol concentrations other mechanism, the insertion of OH• radicals, may be favored. On the other hand, highly concentrated phenol aqueous solutions treatment by the photo-Fenton reaction gives rise to the formation of polyphenolic polymers. These seem to reduce the process rate. Degradation intermediates have been identified by HPLC and FTIR. The FTIR study of the catalyst surface has shown infrared bands attributable to different chemisorbed peroxo-compounds, formates, ortho-formates and carboxylates that can inactivate the catalyst.

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