Adsorption followed by ozone oxidation process is successfully applied in the PSA process. The dynamic adsorption capacity of 13X molecular sieves for o-xylene is 2.7 mmol/g at a pressure of 3.5 kg/cm2. The 13X molecular sieves is efficiently regenerated in 70 min by ozone oxidation process at 25 °C. The PSA system is ran continuously for 50 h and there is no o-xylene breakthrough observed in the fresh air.