Since the two most commonly used methods for TiO2 preparation are sol-gel (SG) and hydrothermal (HT) synthesis, this study attempts to compare both methods in order to determine which one is the most suitable to prepare photocatalysts for propene oxidation. In addition, this work studies how the concentration of the HCl used for hydrolysis of the TiO2 precursor affects the properties of the obtained materials. Also, the effect of avoiding the post-synthesis heat-treatment in a selection of samples is investigated. The photocatalysts are characterized by XRD, N2 adsorption-desorption isotherms and UV-vis spectroscopy, and the study tries to correlate the properties with the photocatalytic performance of the prepared TiO2 samples in propene oxidation. TiO2 materials with high crystallinity, between 67% and 81%, and surface area (up to 134 m2/g) have been obtained both by SG and HT methods. In general, the surface area and pore volume of the TiO2-HT samples are larger than those of TiO2-SG ones. The TiO2-HT catalysts are, in general, more active than TiO2-SG materials or P25 in the photo-oxidation of propene. The effect of HCl presence during the TiO2 synthesis and of the post synthesis heat treatment are much more marked in the case of the SG materials.