Abstract: Desulfurization adsorbents of Cu(Ⅱ)-Ce(Ⅳ) bimetal ion-exchanged 13X zeolites，and Cu(Ⅱ)/13X ion-exchanged and Ce(Ⅳ)/13X ion-exchanged were prepared, respectively. The prepared adsorbents were characterized by XRD and N2 adsorption-desorption. Desulfurization performance of the desulfurization adsorbents for dimethyl disulfide, dimethyl sulfide, and tert-butyl mercaptan was investigated. The results indicate that compared with results of the adsorbents before modification the specific surface area and total pore volume of the prepared desulfurization adsorbents decrease, while the average pore diameter and the number of mesopore increase. The Cu(Ⅱ)-Ce(Ⅳ) bimetal ion-exchanged 13X zeolites exhibit good desulfurization performance, better than the results of single metal-exchanged adsorbents Cu(Ⅱ)/13X and Ce(Ⅳ)/13X, due to the synergistic effect between the two cations. Regeneration performance of spent desulfurization adsorbents was investigated and the results demonstrate that the regenerated adsorbents have a perfect desulfurization performance, and the desulfurization rate of the adsorbents after first regeneration is 98% of the fresh adsorbents.