ABSTRACT In the present study, SiO2 NPs (nanoparticles) were designed and synthesised from brown rice husk ash with the assistance of ultrasonic waves. The synthesised SiO2 NPs with high purity were modified using Fe-Mn oxides. The adsorption ability of SiO2 NPs and Fe-Mn oxides@SiO2 hybrid nanomaterials has been investigated for cobalt removal from wastewater. The characteristics of prepared adsorbents were determined using different techniques of identification. The pseudo-second-order model could describe well the effect of contact time. The Langmuir model described the equilibrium manner of the process well, and one gram of Fe-Mn oxides@SiO2 could attract 284.24 mg of cobalt at saturation state. The thermodynamic parameters show the exothermic and spontaneity of the adsorption process. The electrostatic interaction, physical adsorption in meso-macropores, and complexation reaction are the involved mechanisms. The regeneration of prepared adsorbent was investigated at 4 adsorption/desorption cycles in the continuous process. Synthesised hybrid nanomaterial can remove 70.5% cobalt and reduce 61% COD of the actual effluent from the Petrochemical wastewater.