The invention discloses a method for preparing nitro compounds using nitrogen subvalent oxides. Nitrogen monoxide, nitrogen dioxide, dinitrogen monoxide, dinitrogen trioxide, dinitrogen tetroxide and other low-valent oxides of nitrogen are used, under the promotion of molecular oxygen, through aluminosilicate, silicon aluminum phosphate, phosphorus molybdenum Sodium acid and other heteropoly acid salts, transition metal oxides, triphenylphosphine metal-organic complexes, transition metal ion clay catalysts, and react with alicyclic compounds, aromatic compounds, and heterocyclic compounds to prepare nitro compounds. The method is used to replace the traditional industrial preparation method of nitrogen (V) compounds such as dinitrogen pentoxide, nitric acid, nitrate, and nitrate to prepare nitro compounds, and improves the atomic utilization rate of industrial nitration to prepare nitro compounds. Atom economic properties of nitro compounds.