In this study, we compared two low-temperature synthesis procedures for the large-scale production of titania nanoparticles (NPs). The first takes place in an aqueous medium with an acidic environment, by using a triblock polymer surfactant (Pluronic 123). The second involves a polycondensation reaction of alkoxide precursors at 70 °C in a water-in-oil (W/O) microemulsion with a volume ratio of 1:1, using cetylpyridinium bromide (CPB) as a cationic surfactant. The morphological and structural characterization of the samples was carried out through Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD). The photoactivity of the nanostructured titania was evaluated by measuring the photodegradation of Methylene Blue (MB). The solvent-free synthetic approach provided spherical titania nanoparticles mainly constituted by rutile crystallites with a very good synthetic yield. However, the photodegradation rate of MB for such titania nanoparticles ranges from 30 % to 40 %, after 1h under solar irradiation. Conversely, titania nanoparticles obtained through microemulsion synthesis show a photodegradation rate of more than 90 % comparable to titania P25. This high-yield synthesis leads to the formation of TiO2 nanoparticles characterized by small crystallite aggregates (rutile and anatase).