The nitration of toluene was performed through replacing nitro/sulfuricmixed acid with the mixture of nitric acid and N₂O₅ as a nitrating agent. The effects of reaction temperature, reaction time, and concentration of N₂O₅ on the nitration reaction were investigated. The nitration product of toluene was analyzed by gas chromatography, IR spectrormetry and mass spectrometry. Results show that the nitration product is mainly dinitrotoluene (DNT). The optimum nitration reaction conditions obtained are reaction temperature 10 ℃, N₂O₅ concentration 3 mol·L^-1 and reaction time 1 h. The yield of DNT is 100%. The molar ratio of isomerides 2, 4-DNT and 2, 6-DNT is 4.44:1.