This paper reports on the preparation, characterization, and catalytic properties of the Pd@UIO-66 for toluene oxidation. The samples are prepared by the double-solvent method to form catalysts with large specific surface area, highly dispersed Pd⁰ (Elemental palladium) and abundant adsorbed oxygen, which are characterized by X-ray Photoelectron Spectroscopy (XPS), Brunauer-Emmett-Teller (BET) and Transmission Electron Microscopy (TEM). The results show that as the Pd content increases, the adsorbed oxygen content further increases, but at the same time Pd⁰ will agglomerate and lose some active sites, which will affect its catalytic performance. While 0.2%Pd@UIO-66 has the highest concentration of Pd⁰, the result shows it has the best catalytic activity and the T₉₀ temperature is 210 °C.