笼形八(二硝基苯基)硅倍半氧烷的合成及性能研究

Study on Synthesis and Performances of Polyhedral Octa-(dinitrophenyl) Silsesquioxane

采用两种工艺路线制备了八(二硝基苯基)硅倍半氧烷(ODNPS),收率分别达到91%和86%。对获得的样品的结构进行了表征,表明八(2,4-二硝基苯基)硅倍半氧烷是一步法的唯一主要产物,但八(3,5-二硝基苯基)硅倍半氧烷和八(2,4-二硝基苯基)硅倍半氧烷同时出现在二步硝化法产物中。研究了ODNPS作为含能材料的安全性能,真空安定性试验发现它的放气量为0.13mL·g-1.48h(100℃),10kg落锤测试的特性落高H50为30.7cm;用线扫描摄像实时燃速测定系统测得燃烧速度为4.42mm·s-1(5MPa);快速分解爆炸温度为393℃。表明ODNPS是一种热稳定性较高的含能材料。

Octa-（dinitrophenyl） silsesquioxane （ODNPS） with the yields of 91% and 86% was synthesized by two nitration routes respectively. The composition and structure of the products were characterized by FTIR,^29Si NMR,XRD,etc. The results show that the one-step nitration produce octa （2,4-dinitrophcnyl） silscsquioxanc in major,and the two-step nitration give octa （3,5-dinitrophcnyl） silscsquioxanc and octa （2,4-dinitrophcnyl） silscsquioxanc. TGA test of the ODNPS shows that it detonates at 393 ℃. The volume of the released gas was 0.13 mL·g^-1 · 48 h（ 100 ℃ ） in the thermal stability test in vacuum. Impact sensitivity H50（ specific height） was 30.7 cm using 10 kg drop hammer. At 5 MPa,thc burning rate of the pressed ODNPS pellets was 4.42 mm·s^-1 with density of 1.85 g ·cm^-3 by a burning rate measurement system with real time llne scan camera. These indicate that ODNPS is a thermal stable energetic materials.