2,2-dinitro-1,3-propangdiol was synthesized using nitromethane and 38.5% formalin as raw matieral via two-step reaction, retraction and oxidative nitration, replacing the traditional oxidant of silver nitrate by sodium persulfate and potassium ferricyanide. The overall yield was more than 24.1% and purity was more than 97%. The effects of molar ratio of oxidated system, reaction temperature and reaction time on yields were investigated during oxidative nitration by orthogonal experiment.The optimum reaction conditions are as follows: K3Fe(CN)6, 0.1 mol, Na2S2O8, 0.25 mol, reaction temperature, -5~0 ℃, reaction time, 4 hours.
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刘亚静,陈斌,刘卫孝,等.绿色方法合成2,2-二硝基-1,3-丙二醇[J].含能材料,2010,18(6):623-626. LIU Ya-jing, CHEN Bin, LIU Wei-xiao, et al. Green Synthesis of 2,2-Dinitro-1,3-propangdiol[J]. Chinese Journal of Energetic Materials,2010,18(6):623-626.