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作 者:周诚[1] 李祥志[1] 王伯周[1] 周彦水[1] 霍欢[1]
出 处:《化学推进剂与高分子材料》2015年第5期56-58,共3页Chemical Propellants & Polymeric Materials
基 金:总装重大专项(00401010202)资助
摘 要:研究了一种高安全性合成1,1–二氨基–2,2–二硝基乙烯(FOX–7)的方法,以盐酸乙脒与乙二酸二乙酯为原料,经环化反应合成了2–甲氧基–2–甲基–4,5–咪唑烷二酮,再用硝硫混酸硝化得到2–(二硝基亚甲基)–4,5–咪唑烷二酮,水解反应得到了FOX–7,总收率为56.7%。考察了硝化剂、反应温度、反应时间等因素对硝化反应收率的影响,确定了最佳硝化反应条件:以硝硫混酸(体积比1:2)为硝化剂,反应温度为15~20℃,反应时间为1 h,硝化收率可达62.8%。A high safety synthesis method of 1,1-diamino-2, 2-dinitroethylene(FOX-7) was investigated. The 2-methoxy-2-methyl-4,5-imidazolidinedione was synthesized by cyclization reaction using acetamidine hydrochloride and diethyl oxalate as raw materials. The FOX-7 was obtained by the first step product nitrating with nitric-sulfuric mixed acid to 2-(dinitromethylene)-4,5-imidazolidinedione and then hydrolyzing. The overall yield is 56.7%. The influence of the factors including nitrating agent, reaction temperature, reaction time etc. on the yield of nitration reaction was investigated. The confirmed optimal nitration reaction conditions are as follows: nitric-sulfuric mixed acid(volume ratio 1:2) as nitrating agent, the reaction temperature 15~20 ℃, the reaction time 1 h. The nitration yield is 62.8%.
关 键 词:1 1–二氨基–2 2–二硝基乙烯 FOX–7 2–甲氧基–2–甲基–4 5–咪唑烷二酮
分 类 号:TQ560.6[化学工程—炸药化工] V51[航空宇航科学与技术—航空宇航推进理论与工程]
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