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Rapid population growth and widespread industrialization are the main contributing factors to the increasing contamination of the world’s diminishing freshwater resources. This work investigates Fe/TiO₂ as an efficient and sustainable photocatalyst for treating organic micropollutants in water. The photocatalysts prepared by these mechanochemical methods used a high-energy ball milling technique to manipulate Fe/TiO₂’s structural, optical, and catalytic properties for the photo-oxidation of 2,4-Dichlorophenol (2,4-DCP). Doping with iron effectively reduced the band gap of rutile TiO₂ from 3 to 2.22 eV. By reducing the ball/powder ratio from 34 to 7, the removal efficiency of 2,4-DCP increased from 65.2 to 84.7%. Measuring the TOC indicated 63.5 and 49.4% mineralization by Fe/TiO₂-7 and rutile TiO₂, respectively, after 24 h. The energy yields for the Fe/TiO₂ and rutile TiO₂ were 0.13 and 0.06 g 2,4-DCP/kW h, respectively.