A new class of structured mesoporous materials consisting of gallium oxide nanoparticles embedded and stabilised in a silica matrix was designed, synthesised and tested as catalysts for the epoxidation of various alkenes with aqueous hydrogen peroxide. The structure and texture of the mesoporous gallia-silica composites were elucidated by powder X-ray diffraction, isothermal N-2 sorption and TEM. The most active epoxidation catalysts are the materials containing 80 and 90% of Ga2O3 nanoparticles. These materials give much higher epoxide yields compared to the parent nanoparticles, thus demonstrating the positive effect of structuring on the catalytic performance. The synthesis of the mesoporous gallia-silica composite catalysts was optimised by investigating the effect of the calcination conditions. Finally, different methods for recycling the catalysts were studied. Mild calcination at 250 degrees C for 3 h under controlled N-2 flow was identified as the most suitable treatment to retain the catalytic activity upon reuse. (C) 2012 Elsevier B. V. All rights reserved.