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Red Amaranth (RA) Azo dye is a persistent pollutant in wastewater and stands as a toxicological risk, which has led to the development of effective methods for its removal and photocatalytic degradation. Therefore, CeO2 nanoparticles were synthesized by a controlled precipitation method, and Ultraviolet-Visible (UV–Vis) analysis and Tauc plots yielded a band gap of ~3.24 eV. The CeO2 nanoparticles showed the fluorite cubic phase, and nearly spherical particles with an average size of ~10 nm. Nitrogen physisorption revealed a type IV isotherm with a Brunauer–Emmett–Teller (BET) surface area of 85.27 m2·g−1 and a total pore volume of 0.27 cm3·g−1, indicating a mesoporous structure and high surface accessibility. The chemical behavior showed Ce and O, consistent with phase purity. Photocatalytic performance was evaluated in 20 ppm aqueous solution of RA under 365 nm UV irradiation (LED 100 W), with a temperature of ~20 °C and a 15 min dark adsorption step. Concentration decay was followed at λmax = 520 nm by Lambert–Beer. The degradation efficiency η and pseudo-first-order kinetic were obtained from ln(C0/Ct) vs. time. In addition, chemical oxygen demand (COD) tests were performed on RA solution before and after photodegradation, showing a COD reduction of ~85% (from 19.8 to 3 mg O2·L−1), which corroborates mineralization beyond chromophore bleaching. Under [C0 = 20 mg·L−1] and [mcat = 1.0 g·L−1], CeO2 achieved [RA = 90% at 180 min, k = 0.0125 min−1]. These results demonstrate that CeO2 is an effective photocatalyst for RA degradation under UV-A irradiation, integrating adsorption, kinetic behavior, and mineralization performance into a coherent structure–property relationship.