Abstract: Chemical vapor deposition (CVD) from methane on activated carbon prepared by zinc chloride activation of residue extracted from sunflower seeds, has been optimized to produce carbon molecular sieves using the Taguchi method, targeted at achieving maximum CO₂ adsorption capacity and an increased product yield. The carbon molecular sieves were characterized by N₂ adsorption, CO₂ adsorption, elemental analysis, SEM and FTIR. The CO₂ adsorption capacities were measured at 1 bar/273 K. The optimized carbon molecular sieve with the highest product yield of 91 wt.% had a maximum CO₂ adsorption of 2.622 8 mmol g^-1. Both nitrogen and oxygen surface functional groups and the narrow micropores are crucial for CO₂ adsorption. The Taguchi method is a powerful tool to simultaneously optimize the carbon dioxide adsorption capacity and the yield of carbon molecular sieves.