N，N-二（三硝基乙基）硝胺（BTNNA）的合成工艺优化及热性能?

以硝仿(NF)和乌洛托品(HA)为主要原料,制备出了中间体N,N-二(三硝基乙基)胺(BTNA),并由硝硫混酸硝化得到了目标物N,N-二(三硝基乙基)硝胺(BTNNA),收率达93.6%。采用IR、NMR等方法,对产品结构进行了表征。在BTNA用量相同的条件下,考察了硝硫混酸摩尔比、反应温度及反应时间等关键因素对结果的影响,获得了适宜的反应条件:n(H2SO4)n(HNO3)=1.01.8,反应温度30℃,反应时间20 min。采用差示扫描量热法(DSC)和热重-微商热重(TG-DTG)研究了BTNNA的热性能,其分解温度为177.4℃,是一种性能较好的含能材料。

Synthesis Improvement and Thermal Properties of Bis(2,2,2-Trinitroethyl)-Nitramine (BTNNA)

After the synthesis of intermediate product bis(2,2,2-trinitroethyl)-amine(BTNA) with nitroform (NF) and hexamethylenetetramine(HA) as substrates, target compound bis(2,2,2-trinitroethyl)-nitramine(BTNNA) was obtained through a nitration process. With mixed nitric and sulfuric acid as nitrating agent, the yield of BTNNA reached 93. 6%. IR and NMR were utilized to characterize the structure of BTNNA. Besides, for the same amount of BTNA, key factors that affected the nitration process, including the mole ratio of mixed acid, reaction temperature, and reaction time, were investigated as well. Results show that the optimum reaction condition is when the mole ratio of concentrated sulfuric acid to fuming nitric acid of 1. 0︰1. 8 at 30 ℃ for 20 min. Thermal properties of BTNNA were also studied by differential scanning calorimetry ( DSC) and thermogravimetry-differential thermogravimetric ( TG-DTG) . The decomposition tempera-ture is determined to be 177. 4 ℃, indicating that BTNNA is an energetic explosive with good comprehensive performance.