Nitrate ester explosives were synthesized in chip based micro reactor. When alcohol and nitric-sulfuric mixed acid are mixed in the micro reactor, the yield of triethylene glycoldinitrate (TEGN) is 86.39%,and the yield of diethylene glycol dinitrate is 90.60%. The effects of the ratio between nitration agent and raw material, and the effect of liquid hourly space velocity (LHSV) on the reaction were studied. The results show that when the ratio of acid/alcohol is low, the yield of nitrate explosives decreases with the increase of LHSV, however, when the mole ratio of acid/alcohol increased for a certain, the yield of the product did not change significantly with the decrease of LHSV. And the optimal mole ratio of nitric acid/alcohol for diethyleneglycol is 5, and for triethylene glycol is 4.