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Mixed metal oxide composites have been widely used as adsorbents for the removal of heavy metal ions from wastewater. In this work, Fe2O3/TiO2 composite was sustainably prepared via the treatment of titanium slag with a low-concentration sulfuric acid solution (20%) and used for the removal of As(V) from aqueous solutions. The resulting products were characterized by X-ray diffraction (XRD), N2 adsorption−desorption, Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The batch adsorption was employed to investigate the removal efficiency of the Fe2O3/TiO2 adsorbent toward As(V). The Langmuir and Freundlich isotherms were plotted in order to study the adsorption process. The adsorption of As(V) on FeO3/TiO2 fitted well with the Freundlich isotherm model, suggesting a multilayer adsorption process with an adsorption capacity of 68.26 mg·g−1. The adsorption kinetics study demonstrated that the adsorption behavior of the Fe2O3/TiO2 composite for the As(V) was pseudo-second-order. With low-cost preparation and high adsorption capacity, the prepared Fe2O3/TiO2 adsorbent could be used as an effective adsorbent for As(V) removal from contaminated water sources. The approach utilized in this research is viewed as a sustainable route for creating a proficient adsorbent for the purification of water.