The pulp and paper industry have historically been one of the world’s largest consumers of freshwater resources and producers of wastewater discharges. More than 250 chemicals have been identified in effluents including chlorine-based organic and other toxic compounds. Some of these are resistant to biological degradation such as color-related compounds. The goal of this study was to analyze the real wastewater from the paper mill and to suggest a photocatalytic treatment method in order to reduce the organic pollutants load. The efficiency of the commonly used treatment photocatalytic processes (photo-TiO2 and photo-Fenton reagent) on the treatment of real paper mill effluent was investigated. Additionally, the performance of TiO2 photocatalytic reactions with and without the addition of hydrogen peroxide was also examined. For the experiment, a 500 mL pyrex UV reactor and a 125-W high-pressure mercury lamp, surrounded by pyrex filter blocking wavelengths below 290 nm were used. The approach has been applied for the treatment of effluents produced from a papermaking industry.