1,3-二叠氮基-2-叠氮乙酸丙酯的合成与性能

Synthesis and Properties of 1,3-Diazido-2-azido-propylacetate

以氯代乙酸乙酯为原料,经叠氮化、水解、酯化等反应合成了新型含能增塑剂1,3-二叠氮基-2-叠氮乙酸丙酯(PCPAA)。采用红外光谱、核磁共振及元素分析对其结构进行了鉴定。优化了酯化反应条件。研究了影响酯化反应收率的因素,包括1,3-二叠氮丙醇/叠氮乙酸(DAG/AAE)摩尔比、催化剂和反应时间。采用DSC和感度测试仪测定了PCPAA的热性能,冲击感度和摩擦感度。结果表明,在确定的最佳酯化反应条件(酯化反应∶DAG/AAE摩尔比为1.4,催化剂为硫酸,反应时间为9 h下,收率为71.4%,纯度为99.1%。对PCPAA,ρ=1.32 g·cm^(-3),玻璃化温度T_g(DSC)<-80℃、分解峰温T_p(DSC)=240.7℃,摩擦感度为0%,撞击感度为37.2cm。

A new energetic plasticizer 1,3-diazido-2-azido-propyl acetate（ PCPAA） was synthesized via. azide substitution,hydrolysis,esterification etc reaction using ethylchloroacetate as primary substance. Its structure was identified by IR spectrometry,nuclear magnetic resonance spectrometry and elemental analysis. The esterification reaction conditions were optimized. The factors affecting the esterification reaction yield,including 1,3-diazido-propan-2-ol（ DAG）/2-azido-acetic acid（ AAE） molar ratio,catalyst,and reaction time were investigated.The thermal properties,friction sensitivity and impact sensitivity of PCPAA were measured by DSC and sensitivity tester. Results show that under the determined optimal reaction conditions of esterification reaction： molar ratio of DAG/AAE is 1.4,catalyst is H2SO4,reaction time is 9h,the yield is 71.4% and the purity is 99.1%. For PCPAA,ρ = 1.32 g·cm-3,glass transition temperature as Tg（ DSC） 〈-80 ℃,decomposition peak temperature Tp（ DSC） = 240.7 ℃,friction sensitivity as 0%,impact sensitivity as 37.2 cm.