六硝基六氮杂异伍兹烷中杂质的结构表征及热分解研究  

A Study of Structure Characterization and Thermal Decomposition of the Impurities of HNIW

作　　者：刘进全[1] 欧育湘[1] 王艳飞[1] 孟征[1] 吴相国[1] 

机构地区：[1]北京理工大学材料科学与工程学院,北京100081

出　　处：《兵工学报》2007年第1期122-124,共3页Acta Armamentarii

摘　　要：分别以四乙酰基二苄基六氮杂异伍兹烷(TADBIW)为硝解基质通过亚硝解/硝解一锅法和四乙酰基二甲酰基六氮杂异伍兹烷(TADFIW)为硝解基质通过硝硫混酸法制备六硝基六氮杂异伍兹烷(HNIW).用柱色谱对HNIW的主要杂质进行分离,以FTIR1、H NMR、MS、元素分析确定主要杂质为五硝基一乙酰基六氮杂异伍兹烷(PNMAIW)和五硝基一甲酰基六氮杂异伍兹烷(PNMFIW).PNMFIW与PNMAIW的DSC分析和动力学参数计算表明,前者的初始分解温度和分解峰温均比后者的高,且前者的分解表观活化能约为后者的2倍,这可能是因为,对于一取代基的五硝基六氮杂异伍兹烷六元环上的甲酰基比五元环上的乙酰基有助于笼型结构的稳定。HNIW was respectively synthesized with TADBIW by use of a sub-nitrolysis/nitrolysis onepot method and with TADFIW by use of a mixed acid method. The main impurities of HNIW were separated using a column chromatography and confirmed as PNMAIW and PNMFIW via FTIR, ^1H NMR, MS and element analysis. The DSC and kinetics calculations show that the initial and peak decomposition temperatures of PNMFIW are higher than those of PNMAIW and the apparent decomposition active energy of the former is twice as much as that of the latter. The reason maybe is that the formyl on the hexabasic ring is more stable than the acetyl on the pentabasic ring to the cage structure for PNIW with one substituting group.

关 键 词：有机化学 HNIW PNMAIW PNMFIW 热分解 

分 类 号：O657.3[理学—分析化学]