Resin and asphaltene were separated from Liaohe heavy oil. Catalytic aquathermolysis of asphaltene and resin was investigated by using water soluble catalysts (NiSO4 and FeSO4) and oil soluble catalysts (nickel naphthenate and iron naphthenate). Before and after aquathermolysis, the properties of the resin and asphaltene was compared by means of ultimate analysis, vapor pressure osmometer (VPO) average molecular weight, X-ray diffraction (XRD), 13C and 1H nuclear magnetic resonance (NMR). The conversion sequence was as follows: No-catalyst<NiSO4<FeSO4<nickel naphthenate<iron naphthenate. In the presence of catalysts, the amount of H2 and CO increased significantly, while H2S in the gas product decreased. The molecular weight of asphaltene and resin increased after reaction without catalyst. But the catalysts restrained this trend. The H/C ratio of asphaltene and resin decreased after reaction. From the results of average structural parameters and molecular weight, it was found that asphaltene and resin were partly aggregated after aquathermolysis.