<p>This study presents the synthesis of hybrid mesoporous sulphur-doped CoMn oxide @ cobalt alginate-derived carbon spongy-like beads (M-CoACBs) to remove methylene blue (MB) dye from aqueous solutions. The M-CoACBs were synthesized through a two-step process, followed by extensive characterization using SEM, EDX-mapping, XPS, XRD, and N₂ adsorption-desorption isotherms. The characterization revealed that the sulphur-doped CoMn oxide significantly enhanced the cobalt alginate-derived carbon beads’ structural integrity and surface properties, leading to increased adsorption capacity. The decolorization performance of the M-CoACBs was systematically evaluated and compared to untreated CoACBs. Results showed a remarkable 35% increase in MB removal efficiency with the M-CoACBs, demonstrating the effectiveness of sulphur-doping in improving adsorption capacity. Batch adsorption experiments were conducted to optimize key parameters such as pH, sorbent dose, and initial dye concentration. The optimal conditions were found at pH 7, where the maximum dye removal efficiency was achieved. The adsorption data best fit the Langmuir isotherm (R² = 0.98) and pseudo-second-order kinetic model (R² = 0.99), indicating high capacity and chemisorption. Machine learning (ML) techniques, specifically the Extra Trees algorithm, were employed to predict the adsorption capacity, achieving an R² of 0.999, with error metrics of MSE = 0.263, RMSE = 0.513, and MAE = 0.334. The ML model highlighted the importance of key variables such as initial MB concentration and stirring time. The M-CoACBs exhibited high adsorption capacity and rapid adsorption kinetics, making them a promising material for removing MB dye in wastewater treatment applications. The study highlights the potential of sulphur-doped CoMn oxide as a powerful modification for enhancing the adsorptive properties of carbon-based materials, providing an efficient and sustainable solution to the growing issue of dye pollution in water systems.</p>