New photocatalysts based on TiO 2 were synthesized and characterized. The synthesis involved the controlled hydrolysis of titanium tetraisopropoxide using water containing different proportions of acetone. X-ray diffraction analyses combined with Raman spectroscopy revealed crystalline oxides characterized by the coexistence of the anatase and brookite phases. The Rietveld refinement of diffractograms showed that the presence of acetone in the synthesis process influenced the composition of these crystalline phases, with the proportion of brookite growing from 13 to 22% with the addition of this solvent in the synthesis process. The BET isotherms revealed that these materials are mesoporous with surface area approximately 12% higher than that of the oxide prepared from hydrolysis using pure water. The photocatalytic potential of these oxides was evaluated by means degradation tests using the dyes Ponceau 4R and Reactive Red 120 as oxidizable substrates. The values achieved using the most efficient photocatalyst among the synthesized oxides were, respectively, 83% and 79% for mineralization, and 100% for discoloration of these dyes. This same oxide loaded with 0.5% of platinum and suspended in a 5:1 v/v water/methanol mixture, produced 56 mmol of gaseous hydrogen in five hours of reaction, a specific hydrogen production rate of 138.5 mmol h-1 g-1 , a value 60% higher than that achieved using TiO 2 P25 under similar conditions.