Asmaa S. Morshedy, Elbadawy A. Kamoun, Mostafa Y. Nassar, Amany S. El‐Khouly, Tahany Mahmoud, Mahmoud F. Mubarak
Developing cost‐effective and reusable adsorbents is critical for sustainable wastewater remediation. This study addresses this need by presenting a sonochemically synthesized CuO‐sulfonated charcoal nanocomposite (CuO@charcoal‐SO 3 H) for the efficient removal of Congo red dye (CR). Different analytical tools are used to confirm the structure of as‐ prepared materials. The composite achieved a high specific surface area (465.2 m 2 /g) and an enhanced adsorption capacity of 355.8 mg/g, surpassing both pristine charcoal (300.1 mg/g) and sulfonated charcoal (325.6 mg/g). Under optimal conditions (pH 6, 30°C, 0.5 g/L adsorbent dose, 180 min), adsorption followed pseudo‐second‐order kinetics ( R 2 = 0.998, k 2 = 0.0062 g/mg min), indicating chemisorption as the dominant mechanism. Thermodynamic analysis confirmed a spontaneous and endothermic process, with Δ G = −10.50 kJ/mol, Δ H = 31.75 kJ/mol, and Δ S = 98.55 J/mol K. The nanocomposite maintained 85% efficiency over five regeneration cycles and demonstrated economic viability with a production cost of 0.32–0.65 USD/g. These results establish CuO@Charcoal‐SO 3 H as a high‐performance, reusable, and cost‐effective adsorbent for industrial dye removal.