The invention relates to a preparation method of an ozone heterogeneous oxidation solid catalyst and belongs to the technical fields of environmental protection and chemical engineering catalysts. The preparation method comprises the following steps: by taking porous materials diatom pure, kyanite, brucite, serpentinite, amazon stones and lithium limestone as a carrier, after chambering and modifying the carrier through lithium hypochlorite and di(acetylacetone) beryllium, adding a surfactant dodecyl dimethyl hydroxyethyl ammonium chloride for surface activating treatment under the action of ultrasonic waves; then performing a hydrothermal reaction on the ultrasonic surface activated carrier in a hydrothermal reaction kettle with a compound mineralizer borax and potassium sulfate, catalytic active auxiliary agent precursors of tri(hexafluoroacetylacetone) yttrium (III) dehydrate, tricyclopentadiene promethium, tri[N,N-bis(trimethyl silane) amine] erbium and thulium trifluoromethanesulfonate (III) rare earth metal organic compounds, catalytic active central compound precursor common traditional metal organic compounds of vanadium isonicotinoyl hydrazone pyruvate and cobalt gluconate, and noble metal compounds dipotassium hexachloroosmate and iridium tetrachloride dihydrate under the action of an emulsifier didecyldimethylammonium chloride; and after drying a reaction product to remove water, firing the reaction product in a muffle furnace at a certain temperature to obtain the ozone heterogeneous oxidation solid catalyst.