In this study, a novel biomass adsorbent based on activated carbon incorporated with sulfur-based binary metal oxides layered nanoparticles (SML-AC), including sulfur (S₂), manganese (Mn), and tin (Sn) oxide synthesized via the solvothermal method. The newly synthesized SML-AC was studied using FTIR, FESEM, EDX, and BET to determine its functional groups, surface morphology, and elemental composition. Hence, the BET was performed with an appropriate specific surface area for raw AC (356 m²·g⁻¹) and modified AC-SML (195 m²·g⁻¹). To prepare water samples for ICP-OES analysis, the suggested nanocomposite was used as an efficient adsorbent to remove lead (Pb²⁺), cadmium (Cd²⁺), chromium (Cr³⁺), and vanadium (V⁵⁺) from oil-rich regions. As the chemical structure of metal ions is influenced by solution pH, this parameter was considered experimentally, and pH 4, dosage 50 mg, and time 120 min were found to be the best with high capacity for all adsorbates. At different experimental conditions, the AC-SML provided a satisfactory adsorption capacity of 37.03–90.09 mg·g⁻¹ for Cd²⁺, Pb²⁺, Cr^3+, and V⁵⁺ ions. The adsorption experiment was explored, and the method was fitted with the Langmuir model (R² = 0.99) as compared to the Freundlich model (R² = 0.91). The kinetic models and free energy (<0.45 KJ·mol⁻¹) parameters demonstrated that the adsorption rate is limited with pseudo-second order (R² = 0.99) under the physical adsorption mechanism, respectively. Finally, the study demonstrated that the AC-SML nanocomposite is recyclable at least five times in the continuous adsorption–desorption of metal ions.