The persistence of azo dyes in industrial effluents poses significant environmental risks; therefore, there is a need to develop effective adsorbents. This study investigates the efficiency of a Cu₂O/CuO nanocomposite as an adsorbent for the removal of a model dye, methyl orange (MO), from aqueous solutions. The material was characterized by XRD, SEM and BET analyses, revealing a dominant Cu₂O phase (96 wt%) with CuO fractions, and an average particle size of ~18 nm paired with a specific surface area of 19.54 m² g⁻¹. FTIR and TOC assays revealed the adsorption and degradation of MO by action of the nanocomposite. Operational parameters such as adsorbent dosage, initial dye concentration, pH, and the point of zero charge (PZC) were investigated. Under the optimized conditions, the nanocomposite achieved a dye removal efficiency of 97.0%. The kinetic results showed a strong correlation with the pseudo-second-order model. Furthermore, isotherm analysis revealed that the adsorption process is best described by the Langmuir–Freundlich model, demonstrating an outstanding maximum theoretical adsorption capacity (q_max) of 254.76 mg g⁻¹, which closely aligns with the experimental value (249.48 mg g⁻¹). The findings demonstrated that the synthesized Cu₂O/CuO nanocomposite acts as an efficient and promising adsorbent for the remediation of dye-contaminated waters.