摘要
以三羟甲基硝基甲烷为原料,经酯化、叠氮化两步反应合成出三(叠氮乙酰氧甲基)硝基甲烷,总收率为83.0%。利用红外光谱、核磁共振、元素分析表征了其结构。探讨了叠氮化反应的影响因素,确定其最佳反应条件为:Na N3摩尔加入量为理论值的1.10倍,混合溶剂中水占总体积的10%-25%,反应时间1 h。测试得到TMNTA的密度为1.45 g/cm^3,热分解温度为235.7℃,玻璃化转变温度为-26.23℃,撞击感度H50=44.7 cm(落锤2 kg),爆炸概率4%(摆角66°)。
TMNTA was synthesized using tris( hydroxymethyl) nitromethane as raw material,via the two-step reactions of esterif-ication, azidonation with a total yield of 83.0%.Its structures were confirmed by IR,NMR and elemental analysis.The affecting factors of azidonation were studied.The optimum conditions of the reactions were:nexp:ntheory=1.10 for NaN3(molar ratio),10%-25% of the total volume of acetone-H2O and reaction time 1 h. Some physicochemical properties of TMNTA were obtained by the tests.Results show that the density is 1.45 g/cm^3,decomposition temperature is 235.7℃,glass transition temperature is-26.23 ℃, H50=44.7cm(2 kg),friction sensitivity is 4%(66°).
出处
《固体火箭技术》
EI
CAS
CSCD
北大核心
2015年第3期392-395,共4页
Journal of Solid Rocket Technology
基金
装预研项目(40406030101)