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An effective heterojunction with robust charge separation and enormous degradation efficiency is the major task for photocatalyst preparation. In this study, we have prepared the FeCo 2 O 4 -loaded g-C 3 N 4 nanosheet by the sol-gel-assisted calcination method for photo-Fenton-like degradation under visible-light irradiation by activating persulfate. The nanocomposite exhibits a higher charge separation efficiency than pure g-C 3 N 4 and FeCo 2 O 4 for the degradation reaction against naproxen drugs. An effective interaction between the nanoparticles increases the degradation efficiency up to 91% with a synergistic index of 73.62%. Moreover, the nanocomposite exhibits a 78% mineralization efficiency against the naproxen pollutant under visible-light irradiation. For practical implementation, the degradation reaction was tested with various pH values, different water sources (DI, lake, and tap water), and light sources (LED (visible)/direct sunlight (UV-visible)). Moreover, the possible degradation mechanism predicted by the elemental trapping experiment and the recycling experiment clearly revealed that the heterojunction composite has a high enough degradation stability., Competing Interests: The authors declare no competing financial interest., (© 2021 The Authors. Published by American Chemical Society.)