The invention provides a preparation of a transition metal hexacyanoferrate / titanium dioxide nanocomposite catalyst: using transition metal chloride or transition metal nitrate, potassium ferrocyanide, and titanium dioxide as raw materials, through an in-situ chemical solution method , in situ growth of transition metal hexacyanoferrate (MHCF) on the surface of titania nanoparticles yielded MHCF / TiO 2 nanocomposite catalysts. The present invention also provides a kind of MHCF / TiO 2 Nanocomposite catalyst light-Fenton synergistic reaction method for degrading organic pollutants: in the dark reaction without light, MHCF can degrade organic pollutants in the form of Fenton reaction, and under ultraviolet light irradiation, titanium dioxide (photocatalyst) can Electron-hole pairs are generated, and electrons can be accelerated by H in MHCF 2 o 2 The reduction of oxidized ferric iron, at the same time, MHCF can also inhibit the recombination of photogenerated electrons and holes by accepting the electrons of titanium dioxide, thereby accelerating the Fenton reaction and the efficiency of hydroxyl radicals generated by the photocatalytic process. have very good degradation efficiencies.