DIANP合成工艺优化及杂质对其性能的影响

Optimization of synthesis process of DIANP and influence of impurities on its performance

为获取叠氮硝胺(1,5-二叠氮基-3-硝基-3-氮杂戊烷,DIANP)合成的最佳工艺条件,以吉纳(硝化二乙醇胺,DINA)和NaN;为原料,采用正交试验法,对工艺条件进行了优化,得到的最佳工艺条件为:在相转移催化剂四丁基溴化铵(TBAB)存在下,反应介质为二甲基亚砜(DMSO),反应温度为90~95℃,反应时间为8h,DINA与NaN;投料摩尔比为1:2.2。DIANP平均收率可达93.4%,质量分数可达98%以上。采用液相色谱质谱联用仪对杂质进行了定性研究,结果表明,经处理之后的产物中杂质主要为DINA和单叠氮硝胺(PNAN)。研究了杂质对DIANP稳定性及性能的影响,结果表明,在一定杂质含量范围内,杂质对DIANP储存稳定性无影响,但对撞击感度有明显影响,杂质越多,撞击感度越高。

In order to obtain the optimal process conditions for synthesis of the azido nitramine (1,5-diazido-3-nitro-3-azapentane,DIANP),using DINA (nitrodiethanolamine) and NaN;as raw materials,the process conditions were optimized by using the orthogonal experiment method.The obtained optimal process conditions are as follows:in the presence of the phase transfer catalyst tetrabutylammonium bromide (TBAB),the reaction medium is dimethyl sulfoxide (DMSO),the reaction temperature is 90~95℃,the reaction time is 8h,and the molar ratio of feeding DINA and NaN;is 1:2.2.The average yield of DIANP can reach 93.4%,and the mass fraction can reach above 98%.The impurities were qualitatively investigated by using the liquid chromatography-mass spectrometer.The results show that the impurities in the treated product are mainly DINA and monoazido nitramine (PNAN).The influence of impurities on the stability and performance of DIANP was investigated.The results show that within a certain impurity content range,the impurities have no effect on the storage stability of DIANP,but have significant effect on the impact sensitivity.The more the impurities,the higher the impact sensitivity.