Fe2O3/TiO2/AC composites were successfully synthesized via a sol-gel method, and their efficacy in decomposing methyl orange via adsorption-photocatalytic processes was reported for the first time in this study. Systematic exploration of the physicochemical properties impacting photocatalytic activity was conducted through X-ray diffraction (XRD), scanning electron microscopy - Energy-dispersive X-ray spectroscopy (SEM-EDS), and Fourier transform infrared spectroscopy (FTIR) characterizations. The study revealed that the degradation of methyl orange resulted from a synergistic interplay between adsorption and photocatalysis. The incorporation of Fe2O3 nanoparticles significantly elevated photocatalytic activity by 70%, with additional enhancement observed upon the introduction of activated carbon (AC) particles. The synergistic effects of AC adsorption and TiO2/Fe2O3 photocatalysis exhibited remarkable efficiency in degrading methyl orange under visible light irradiation. The trial functioning of Fe2O3 and AC in the TiO2/Fe2O3/AC composite, which serves as an adsorbent, an electron trap, and a co-catalyst providing active sites, significantly improved photocatalytic activity. These findings not only contribute to understanding the crucial role of composite TiO2 in conjunction with metal and carbon-based co-catalysts but also hold valuable implications for advancing research in the development of adsorption-photocatalytic systems for wastewater treatment.