An experimental study of the pressure swing adsorption (PSA) process, which separates CO2 from the flue gas of the power plant, was investigated. Three adsorption columns packed with activated carbon were used and pressurization, adsorption, pressure equalization, rinse, and evacuation steps were applied in a cyclic process. Two cases of the rinse method were used with various feed and product flow rates, and also two kinds of recycle methods were introduced for enhancing the recovery. As a result, the PSA process that separates CO2 at a purity of 99% and recovery of 55% from the gas mixture similar to the flue gas of a power plant, was obtained.