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以双环[3.3.1]壬烷-2,6-二酮为原料,经腙化、消除、环氧化、环合、乙酰化、硝化等步骤,合成了一种新型硝基笼形化合物2-硝基-2-氮杂金刚烷-4,8-二醇二硝酸酯,总收率为27%。以硝硫混酸为硝化剂,考察了硫酸与硝酸摩尔比、反应温度、反应时间对硝化反应的影响。确定的最佳反应条件为:摩尔比n(H_2SO_4)∶n(HNO_3)=1∶2,反应温度60℃,反应时间4 h,此时,硝化反应收率达81%。利用热重分析(TG)和差示扫描量热法(DSC)研究了目标化合物的热性能,发现其从170.0℃开始分解,热分解峰温为193.7℃。通过Kamlet-Jacobs公式预估了目标化合物的物化与爆轰性能,其密度为1.71 g·cm~(-3),爆速为5780 m·s~(-1),爆压为11.0GPa。
A novel nitro-cage compound 2 was synthesized from bicyclo [3.3.1] nonane-2,6-dione via hydrazoneation, elimination, epoxidation, cyclization, acetylation and nitration Nitro-2-azaadamantane-4,8-diol dinitrate in a total yield of 27%. The effects of the molar ratio of sulfuric acid to nitric acid, reaction temperature and reaction time on the nitrification reaction were investigated by using nitric-sulfur mixed acid as nitrating agent. The optimal reaction conditions were determined as follows: molar ratio of n (H 2 SO 4): n (HNO 3) = 1: 2, reaction temperature 60 ℃ and reaction time 4 h. The thermal properties of the target compounds were investigated by TG and DSC. The results showed that the target compounds decomposed from 170.0 ℃ and the peak temperature of thermal decomposition was 193.7 ℃. The physico-chemical properties and detonation properties of the target compounds were estimated by the Kamlet-Jacobs formula with a density of 1.71 g · cm -3, a detonation velocity of 5780 m · s -1 and a burst pressure of 11.0 GPa.