2-甲基-2-硝基-1,3-二叠氮基丙烷的合成

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%。

Synthesis of 2-Methyl-2-nitro-1,3-diazido-propane

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),T_g(DSC) -51.5 ℃,T_p(DSC) 234 ℃,impact sensitivity 34 cm,friction sensitivity 32%.