Aiming at the problems of nitration reaction such as intense exotherm,large volume online,and serious safety haz-ards during the synthesis of N-nitromethylamine(NMA),the precursor of linear nitramine energetic plasticizers(DNDAs),mi-cro reaction technology was adopted to carry out the nitration of 1,3-dimethylurea using nitrate-sulfur mixed acid.Critical in-termediate NMA was further synthesized through the hydrolysis reaction.The structure of synthesized NMA was characterized,and the reaction conditions of nitration were also optimized.The results show that micro-reaction technology can solve the problems of uncontrollability and high safety risk caused by large amounts of heat release and volume online of nitration reaction in the process of synthesizing NMA.The optimal nitration reaction temperature is 15 ℃,the optimal material mol ratio of nitric acid,sulfuric acid and 1,3-dimethylurea is 1:0.78:0.67,and the average residence time was 22.5s.The yields of NMA reached 90.7％,and the purity was 99.2％.This micro-reaction process has the advantages of high reaction temperature,high safety,fast reaction rate,and high product yield.
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维普
