AbstractIn this study, waste tires (WTs) were carbonized under an N2 atmosphere. Subsequently, KOH/WTs‐char with KOH‐assisted CO2 activation was used to prepare activated carbon (AC) as a highly porous carbon material for the removal of Cr(VI) and Cd(II) from water. Various techniques such as elemental analysis, Fourier‐transform infrared spectroscopy, scanning electron microscopy, and N2 adsorption/desorption were employed to investigate the physical and chemical characteristics of the prepared carbons. The WTs‐char activated with KOH under CO2 exhibited a microstructure with a high BET surface area and pore volume of 1841 m2/g and 0.869 cm3/g, respectively, demonstrating excellent adsorbent performance. The maximum removal efficiencies of 99.91 % for Cd(II) and 99.81 % for Cr(VI) were achieved using AC2 carbon under the following conditions: pH 2 for Cr(VI) and pH 5 for Cd(II), contact time of 120 min, adsorbent dose of 0.4 g/100 mL, and temperature of 298 K. The adsorption kinetics followed the pseudo‐second‐order equation, and the equilibrium data fit well with the Redlich–Peterson isotherm equation. The positive values of ▵G indicated that the uptake process for both ions was nonspontaneous and nonfeasible over the temperature studied. Both ions showed negative values of ΔH and ΔS on carbon, suggesting exothermic adsorption and a decrease in disorder. Regeneration studies showed that NaOH was a better desorbing agent than HCl. Cr(VI) desorption resulted in over 90 % removal recovery by AC2 using 1.0 M NaOH even after the fifth cycle. However, the low activation energy indicated that the adsorption was favorable kinetically. Overall, this study demonstrated the effective preparation of highly porous carbon and its successful performance in removing Cr(VI) and Cd(II) ions.