In this study, mixed phase of CaFe 2 O 4 and ZrO 2 magnetic nanocomposite (CaF-ZO-MNC) was fabricated through facile co-precipitation method and was explored for abatement of methyl orange (MO) dye from aqua matrix. X-ray diffraction (XRD) pattern of the synthesized CaF-ZO-MNC depicted significant diffraction peaks of ZrO 2 and CaFe 2 O 4 nanoparticles ensured the crystalline nature of the material. The coexistence of ZrO 2 and CaFe 2 O 4 nanoparticles in the composite increased the BET surface area (95.32m 2 /g) and improves its physicochemical properties as an adsorbent. Enhanced adsorption capacity towards MO dye was found to be 370.37 mg/g from Langmuir model, which is higher than standalone nanoscale Fe, Ca, and Zr metal oxide nanoparticles. The equilibrium adsorption data were found to follow Langmuir isotherm and the adsorption process followed second order kinetic model strictly. Response surface methodology (RSM) was utilized for optimizing the experimental conditions for maximizing the MO dye removal (%) with desirability function approach. Four factors five levels central composite design was implemented for RSM study and the simultaneous interaction of process variables on dye removal efficiency was studied by 3D response surface plots. Maximum MO dye removal of 98.92% was determined with MO dye concentration of 22 mg/L, adsorbent dose of 0.54 g/L, contact time of 25 min at recation temperature of 30°C.KEYWORDS adsorption capacity, kinetic and isotherm study, metal oxide nanocomposite, optimization, toxic dye