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One wt% Ru/TiO2 catalysts prepared by a one-pot microwave-assisted polyol method have been shown to be highly active for Levulinic acid hydrogenation to γ-Valerolactone. Preparation temperature, microwave irradiation time and choice of Ru precursor were found to have a significant effect on catalyst activity. In the case of Ru(acac)3-derived catalysts, increasing temperature and longer irradiation times increased catalyst activity to a maximum LA conversion of 69%. Conversely, for catalysts prepared using RuCl3, shorter preparation times and lower temperatures yielded more active catalysts, with a maximum LA conversion of 67%. Catalysts prepared using either precursor were found to contain highly dispersed nanoparticles <3 nm in diameter. XPS analysis of the most and least active catalysts shows that the catalyst surface is covered in a layer of insoluble carbon with surface concentrations exceeding 40% in some cases. This can be attributed to the formation of large condensation oligomers from the reaction between the solvent, ethylene glycol and its oxidation products, as evidenced by the presence of C-O and C = O functionality on the catalyst surface

Rapid Microwave-Assisted Polyol Synthesis of TiO2-Supported Ruthenium Catalysts for Levulinic Acid Hydrogenation