摘要
以硝基乙烷、甲醛为原料,自行设计合成路线,经缩合、磺酰化、叠氮化等反应合成了2-甲基-2-硝基-1,3-二叠氮基丙烷(NMPA)。采用红外光谱、核磁共振及元素分析对其结构进行了表征;研究了叠氮化温度、时间及反应介质对产物得率的影响,确定最佳反应条件为:反应温度93～95℃,反应介质二甲基亚砜,反应时间30h,总收率(以硝基乙烷计)为71.5%,纯度达99%以上。测得NMPA的一些性能如下:ρ=1.28g.cm-3,Tg(DSC)=-51.5℃,Tp(DSC)=234℃,撞击感度为34cm,摩擦感度32%。
2-Methyl-2-nitro-1,3-diazidopropane （NMPA） can be used as a low-molecular plasticizer of propellants and as an ingredient of gas generators. NMPA was mentioned in literatures,but its detailed synthesis procedures were not reported. The authors synthesized NMPA via a self-designing process that consists of three steps, i. e. condensation ,sulfonation and azido-substitution, using nitroethane and formaldehyde as starting materials. The factors affecting the NMPA＇s yield,including reaction temperature,time and media for azido-substitution, were investigated. Based on this investigation, the optimal reaction conditions were determined： T=93 -95 ℃,t=30 h,medium DMSO,which made NMPA＇s yield （based on nitroethane） up to 71.5% and purity of 99%. The structure of the resulting product was identified by IR, NMR and element analysis. Some properties of NMPA were measured as follows,ρ 1.28 g . cm^ -3, Tg （DSC） -51.5 ℃, Tp （DSC） 234 ℃, impact sensitivity 34 cm,friction sensitivity 32%.
出处
《含能材料》
EI
CAS
CSCD
北大核心
2010年第1期11-14,共4页
Chinese Journal of Energetic Materials
基金
武器装备部预研基金项目(51328050505)
