Abstract
Layered double hydroxideswithMe-based oxyanions (Me_Mo, V) in the interlayer gallerywere prepared by ionexchange and used as efficient catalysts for the mild oxidation of organic sulfideswith H2O2. Raman spectroscopywas used as the main and very efficient technique for the advanced characterization of these materials duringtheir preparation and catalytic use. First, it served for monitoring the progression of the ion exchange duringthe preparation of the catalysts, and then the Raman spectroscopy provided precise information regarding thetype of the oxyanions located in the catalyst structure, before and after the oxidation reaction.