This work focuses on the treatment of a dye solution, C.I. Basic Blue 41 (BB41), and industrial wastewater by UV/TiO2 photocatalytic process using aqueous catalyst suspensions of titanium dioxide (TiO2), Degussa P25. The procedures were carried out in a semi-pilot scale prototype solar photoreactor under solar radiation. Response surface methodology (RSM) based on Box-Wilson design was applied to assess individual effects of the five main independent parameters: initial dye concentration ([BB41]), TiO2 concentration ([TiO2]), flow rate (Q) initial pH and accumulated solar energy (Qvn) on the decolorization efficiency and to optimise the UV/TiO2 process. Photocatalytic mineralisation was carried out at the optimal conditions found by RSM and results were evaluated by total organic carbon (TOC) abatement for BB41 sloution and industrial wastewater. The optimal conditions found by RSM were: 0.4 g/L, 14.04 mg/L, 1,479.6 L/h, 5.52 and 80 KJ/L for TiO2 concentration, initial dye concentration, flow rate, initial pH and accumulated solar energy, respectively. Photocatalytic mineralisation results show that for accumulated visible solar energy equal to 377.714 kJ/L (after 6 hours of irradiation), under these conditions, the percentage of the initial TOC reduction is about 88% and 85.5% for industrial waste and BB41 solution, respectively.