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.