Photocatalytic degradation is a combination of photochemical and catalytic processes in which light and a catalyst are needed to carry out chemical transformations. In this research, a photocatalytic degradation method has been developed using the TiO2−Fe(VI) system with UV light activation. This method is one of the appropriate alternative methods for the treatment of azo dye waste because it is safe, economical, and environmentally friendly. The purpose of this study was to determine the effect of pH and contact time on the TiO2−Fe(VI)-UV system on the photocatalytic degradation of methylene blue. The results showed that in the TiO2−Fe(VI)-UV system, the percentage of methylene blue degradation reached 99.97% at pH 2.