Abstract: The Ag-Y/MIL-101 adsorbents were successfully prepared via loading Ag and Y onto MIL-101. The adsorbents were characterized by XRD, SEM-EDS, BET and TG-DTG methods. The effects of the loading order and concentrations of metals, the amount of AgNO₃ solution and Y(NO₃)₃ solution, and the loading residence time on adsorptive removal performance of thiophene were studied. The conditions of adsorptive desufurization were also optimized. The results show that the lattice structure of MIL-101 remains after the introduction of metals. Compared with MIL-101, the specific surface area and pore volume of Ag-Y/MIL-101 decrease. The optimal preparation conditions of Ag-Y/MIL-101 adsorbent are to load Ag first and then Y with 30 mmol/L of both the loading concentrations of Ag and Y ion, 1 mL of both the dosages of AgNO₃ solution and Y(NO₃)₃ solution, and 8 h of the loading residence time. The optimal desulfurization conditions are 10 mL of model oil, 0.05 g of Ag-Y/MIL-101 dosage, the adsorption temperature of 60℃, and the adsorption time of 8 h. At these conditions, the thiophene desulfurization capacity over Ag-Y/MIL-101 reaches 21.7 mg/g. The Ag can significantly improve the adsorption sulfur capacity of MIL-101, and Y can significantly improve the adsorption selectivity of MIL-101. Therefore, the synergistic effect of Ag and Y in Ag-Y/MIL-101 adsorbent makes it have higher sulfur capacity and thiophene desulfurization selectivity than MIL-101.