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出 处:《含能材料》2013年第6期730-733,共4页Chinese Journal of Energetic Materials
基 金:国家自然科学基金-中国工程物理研究院联合基金(11076017);国防预研重大专项(J-KY-2012-1317)
摘 要:以硝基胍(NQ)为原料、100%硝酸/20%发烟硫酸/硝酸铵为硝化体系,经硝化反应合成了1,2-二硝基胍(DNG)。用IR、1H NM R、13C NM R、M S表征了DNG的结构。研究了影响DNG产率和正交实验的因素。用T G和DSC研究了DNG的热分解行为。结果表明,硝化反应的优化条件为n(HNO3)n(NQ)n(NH4NO3)=1521,V(H2SO4)V(HNO3)=1.251,反应时间为8 h,反应温度为10℃。优化条件下DNG产率达61.76%。DNG的DSC曲线峰温为182.83℃,显示DNG有良好的热稳定性。1 ,2-Dinitroguanidine(DNG) was synthesized via the nitration reaction using nitroguanidine(NQ) as raw material and 100% nitric acid/20% oleum/ammonium nitrate as nitrating system. The structure of DNG were identified by IR, 1H NMR,13C NMR and MS. The factors affecting the yield of DNG and orthogonal experiment were investigated. The thermal decomposition behavior of DNG was studied using TG and DSC. The results show that the optimized conditions of the nitration reaction are: n(HNO3)n(NQ)n(NH4NO3)=1521,V(H2SO4)V(HNO3)=1.251, the reaction time 8 h and reaction temperature 10 ℃. The yield of DNG can reach up to 61.76% under the optimized conditions. The peak temperature of DSC curve for DNG is 182.83 ℃, indicating that DNG has a better thermal stability.
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