物理化学学报
物理化學學報
물이화학학보
ACTA PHYSICO-CHIMICA SINICA
2009年
5期
981-986
,共6页
六硝基六氮杂异伍兹烷%热分解%残余物%TG-DSC-MS%TG-FTIR%FTIR
六硝基六氮雜異伍玆烷%熱分解%殘餘物%TG-DSC-MS%TG-FTIR%FTIR
륙초기륙담잡이오자완%열분해%잔여물%TG-DSC-MS%TG-FTIR%FTIR
Hexanitrohexaazaisowurtzitane%Thermal decomposition%Residue%TG-DSC-MS%TG-FTIR%FTIR
在(2.0±0.1)MPa氩气氛围下六硝基六氮杂异伍兹烷(HNIW)在(204.0±0.5)、(208.0±0.5)、(212.0±0.5)和(216.0±0.5)℃下分别加热10、20、30、40、50和60 min.采用元素分析、扫描电子显微镜(SEM)、傅立叶变换红外(FTIR)光谱仪、差示扫描量热(DSC)仪、热重-差示扫描量热仪-质谱(TG-DSC-MS)仪和热重-红外(TG-FTIR)仪对(208.0±0.5)℃下得到的残余物进行研究.结果表明,HNIW离子在210.0℃左右恒温热解60 min后,残余物的组成为C2H2N2O.残余物中未分解的HNIW比初始HNIW稳定性差.在等温条件下,HNIW是逐步分解的.HNIW残余物的热分解分为三个阶段,第一个分解阶段主要为未分解的HNIW的热分解,第二阶段主要为五员环硝铵和碳氮杂环化合物的分解反应,第三阶段主要为五员环硝铵的分解反应和NO2的二次反应,并获得了每一个阶段的热分解产物.
在(2.0±0.1)MPa氬氣氛圍下六硝基六氮雜異伍玆烷(HNIW)在(204.0±0.5)、(208.0±0.5)、(212.0±0.5)和(216.0±0.5)℃下分彆加熱10、20、30、40、50和60 min.採用元素分析、掃描電子顯微鏡(SEM)、傅立葉變換紅外(FTIR)光譜儀、差示掃描量熱(DSC)儀、熱重-差示掃描量熱儀-質譜(TG-DSC-MS)儀和熱重-紅外(TG-FTIR)儀對(208.0±0.5)℃下得到的殘餘物進行研究.結果錶明,HNIW離子在210.0℃左右恆溫熱解60 min後,殘餘物的組成為C2H2N2O.殘餘物中未分解的HNIW比初始HNIW穩定性差.在等溫條件下,HNIW是逐步分解的.HNIW殘餘物的熱分解分為三箇階段,第一箇分解階段主要為未分解的HNIW的熱分解,第二階段主要為五員環硝銨和碳氮雜環化閤物的分解反應,第三階段主要為五員環硝銨的分解反應和NO2的二次反應,併穫得瞭每一箇階段的熱分解產物.
재(2.0±0.1)MPa아기분위하륙초기륙담잡이오자완(HNIW)재(204.0±0.5)、(208.0±0.5)、(212.0±0.5)화(216.0±0.5)℃하분별가열10、20、30、40、50화60 min.채용원소분석、소묘전자현미경(SEM)、부립협변환홍외(FTIR)광보의、차시소묘량열(DSC)의、열중-차시소묘량열의-질보(TG-DSC-MS)의화열중-홍외(TG-FTIR)의대(208.0±0.5)℃하득도적잔여물진행연구.결과표명,HNIW리자재210.0℃좌우항온열해60 min후,잔여물적조성위C2H2N2O.잔여물중미분해적HNIW비초시HNIW은정성차.재등온조건하,HNIW시축보분해적.HNIW잔여물적열분해분위삼개계단,제일개분해계단주요위미분해적HNIW적열분해,제이계단주요위오원배초안화탄담잡배화합물적분해반응,제삼계단주요위오원배초안적분해반응화NO2적이차반응,병획득료매일개계단적열분해산물.
Hexanitrohexaazaisowurtzitane(HNIW)particles were heated isothermally at(204.0±0.5),(208.0±0.5),(212.0±0.5),and(216.0±0.5)℃for 10,20,30,40,50,and 60 min under(2.0±0.1)MPa pressure in an argon atmosphere.Residues obtained at(208.0±0.5)℃ were studied by elemental analysis,scanning electron microscopy(SEM),Fourier transform infrared (FTIR)spectroscopy,differential scanning calorimetry(DSC),thermogravimetry-differential scanning calorimetry-mass spectrometry (TG-DSC-MS)and thermogravimetry-Fourier transform infrared (TG-FTIR)spectroscopy.Results showed that after isothermal decomposition of HNIW crystals at about 210.0 ℃ for 60 min residues were formed with an average molecular formula of C2H2N2O.Unreacted HNIW is present in the residue and is more thermally unstable than the original HNIW.We confirmed that HNIW crystals decomposed stepwise under isothermal conditions.Three stages were found to exist during the thermal decomposition of HNIW residues.The first decomposition stage consists of an initial decomposition of unreacted HNIW,the second stage comprises an elimination reaction of five-membered ring amides and nitrogen hemrocyclic compounds and in the third stage five-membered ring amides are degraded and secondary reactions involving NO2 occur.The main gaseous products in every stage are discussed.
