The development of nanomaterials for dye degradation has garnered significant interest due to their efficiency, environmental benefits, and cost‐effectiveness. In this study, a nanocomposite adsorbent composed of α‐Fe2O3 coupled with carbon derived from eco‐friendly corn husk has been developed. This material effectively captured cationic dyes, Methylene Blue (MB) and Malachite Green (MG), from aqueous solutions, including industrial dye effluent from local industry. The synthesized nanocomposite demonstrated rapid removal of MB and MG from the solution without the need for additional oxidizing or reducing agents. The adsorption conditions by varying parameters such as adsorbent dose, contact time, solution pH, initial dye concentration, and temperature have been optimized. Adsorption isothermal studies indicated that the Langmuir isotherm model best explained the adsorption process. Kinetic studies revealed that the adsorption process follows a pseudo‐first‐order model for MB, while the intraparticle diffusion model is more appropriate for MG. Moreover, the nanocomposite exhibited excellent reusability and regenerability for dye adsorption. Our study showcases the effectiveness of the synthesized nanocomposite adsorbent, comprising α‐Fe2O3 integrated with carbon derived from eco‐friendly corn husk using a simple and sustainable methodology, in efficiently removing cationic dyes from textile wastewater. This approach offers a promising solution for environmental remediation.