2,4,6-三氨基-5-硝基嘧啶-1,3-二氧化物的合成工艺研究  

Research on The Synthesis Process of 2,4,6-Triamino-5-nitropyrimidine-1,3-dioxide

作　　者：唐思宇 董秦 罗郑航 黄明[2] 杨海君[1] TANG Siyu;DONG Qin;LUO Zhenghang;HUANG Ming;YANG Haijun(Department of Materials and Chemistry,Southwest University of Science and Technology,Mianyang 621010,China;Institute of Chemical Materials,China Academy of Engineering Physics,Mianyang 621999,China)

机构地区：[1]西南科技大学材料与化学学院,四川绵阳621010 [2]中国工程物理研究院化工材料研究所,四川绵阳621999

出　　处：《合成化学》2024年第1期67-72,共6页Chinese Journal of Synthetic Chemistry

基　　金：国家自然科学基金资助项目(22075260);四川省自然科学基金面上项目(2022NSFSC0288);装备部基础科研项目(192ZW22002)。

摘　　要：2,4,6-三氨基-5-硝基嘧啶-1,3-二氧化物(ICM-102)是一种新型高能低感含能分子,开展其合成研究有利于工程化应用。以2,4,6-三氨基嘧啶(1)为原料,经2,4,6-三氨基-5-硝基嘧啶(2)对2,4,6-三氨基-5-硝基嘧啶-1,3-二氧化物一水合物(3,ICM-102·H_(2)O)进行了合成研究。用FT-IR,^(1)H NMR,^(1)C NMR和HPLC等对化合物2及化合物3进行分析表征。研究了硝化体系、硝酸用量和反应温度等对化合物2产率的影响,以及氧化体系、三氟乙酸(TFA)和H_(2)O_(2)用量等对化合物3产率的影响,获得了最佳工艺条件。当n(1)∶n(68%HNO_(3))=1.00∶3.80,反应温度20~50℃,反应时间25 min时,化合物2的产率达98.8%;当n(2)∶n(30%H_(2)O_(2))=1.00∶4.19,室温,反应时间8 h时,化合物3的产率为71.1%。通过工艺条件研究,用68%HNO_(3)替代了发烟硝酸,且硝酸和TFA用量降低,总产率提升至70.2%。HPLC测试化合物3的纯度为98.1%。2,4,6-Triamino-5-nitropyrimidine-1,3-dioxide(ICM-102)is a new type of high-energy energetic molecule with low sensitivity.The research on the synthesis of ICM-102 is beneficial for its engineering applications.The synthesis of 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide monohydrate(3,ICM-102·H_(2)O)via compound 2,4,6-triamino-5-nitropyrimidine(2)was studied starting from 2,4,6-triaminopyrimidine(1).Compounds 2 and 3 were characterized by FT-IR,^(1)H NMR,^(13)C NMR and HPLC.The effects of nitration systems,dosages of nitric acid and temperatures on the yields of compound 2,as well as the effects of oxidation systems,dosages of TFA and H_(2)O_(2)on the yields of product 3 were studied.The optimum process conditions were obtained.When n(1)∶n(68%HNO_(3))=1.00∶3.80,temperature range is 20~50℃,and reaction time is 25 min,the yield of compound 2 is up to 98.8%.When n(2)∶n(30%H_(2)O_(2))=1.00∶4.19,and reaction time is 8 h,the yield of 3 at room temperature is up to 71.1%.Through process study,fuming nitric acid was replaced by 68%HNO_(3),and the consumption of 68%HNO_(3)and TFA was significantly reduced.HPLC determined the purity of compound 3 as 98.1%.

关 键 词：含能材料 2 4 6-三氨基-5-硝基嘧啶-1 3-二氧化物 合成 硝化 氧化 工艺 

分 类 号：O626.41[理学—有机化学]