A new high energetic density material,N-acetyl-3,3-dinitroazetidine(ADNAZ),was synthesized with advantages as low melting point,high density,insensitive to detonation on impact and forming a eutectic with TNAZ which c...A new high energetic density material,N-acetyl-3,3-dinitroazetidine(ADNAZ),was synthesized with advantages as low melting point,high density,insensitive to detonation on impact and forming a eutectic with TNAZ which can be shaped charge antitank weapons or be used energetic carrier for higher melting meaterial such as HMX and the like.ADNAZ was synthesized by a five-steps reaction,using nitromethane,paraformaldehyde and tert-butylamine etc.as starting materials,with overall yield of 42.8%.Some factors affecting yield of ADNAZ was also discussed.The structures of intermediates and ADNAZ were confirmed by IR,HNMR,CNMR and MS.展开更多
直接法硝解乌洛托品制备黑索今的过程中合成了一种新型的环形副产物,采用硅胶柱层析法分离得到3,5-二硝基-1-氧-3,5-二氮杂环己烷,洗脱剂为:丙酮/二氯甲烷,梯度洗脱.以丙酮为溶剂培养得到了3,5-二硝基-1-氧-3,5-二氮杂环己烷单晶,用元...直接法硝解乌洛托品制备黑索今的过程中合成了一种新型的环形副产物,采用硅胶柱层析法分离得到3,5-二硝基-1-氧-3,5-二氮杂环己烷,洗脱剂为:丙酮/二氯甲烷,梯度洗脱.以丙酮为溶剂培养得到了3,5-二硝基-1-氧-3,5-二氮杂环己烷单晶,用元素分析、傅里叶变换红外(FTIR)光谱、核磁共振氢谱(NMR)以及质谱(MS)对其结构进行了表征,用X射线单晶衍射仪测定了其晶体结构.结果表明,晶体C3H6N4O5分子量为178.12,属于单斜晶系,空间群P121/n1,晶胞参数:a=0.58128(13)nm,b=1.72389(14)nm,c=0.71072(6)nm,β=112.056°,V=0.66006(16)nm3,Z=4,DC=1.792 g cm–3,μ=0.17 mm–1,F(000)=368.0,最终偏差因子R=0.0397.用同步热分析仪技术研究了3,5-二硝基-1-氧-3,5-二氮杂环己烷的热行为,DSC曲线上在383.15和519.05 K分别有一个尖锐的熔化吸热峰和分解放热峰.另外,根据Kissinger方程及Flynn-Wall-Ozawa方程和不同升温速率下的TG曲线计算得到了该化合物的热分解动力学参数(活化能和指前因子),利用Coats-Redfern法研究了该物质的热分解机理.结果表明:3,5-二硝基-1-氧-3,5-二氮杂环己烷是一种低熔点、热稳定性好的化合物.Kissinger方程计算其活化能为212.32 k J mol–1,指前因子为6.20×1020 s–1,Flynn-Wall-Ozawa方程计算其活化能为210.39 k J mol–1,该物质的热分解动力学方程为G(α)=(1–α)–1–1,反应级数为2.展开更多
文摘A new high energetic density material,N-acetyl-3,3-dinitroazetidine(ADNAZ),was synthesized with advantages as low melting point,high density,insensitive to detonation on impact and forming a eutectic with TNAZ which can be shaped charge antitank weapons or be used energetic carrier for higher melting meaterial such as HMX and the like.ADNAZ was synthesized by a five-steps reaction,using nitromethane,paraformaldehyde and tert-butylamine etc.as starting materials,with overall yield of 42.8%.Some factors affecting yield of ADNAZ was also discussed.The structures of intermediates and ADNAZ were confirmed by IR,HNMR,CNMR and MS.
基金supported by the National Natural Science Foundation of China(20573098)Science and Technology Foundation of the National Defense Key Laboratory of Propellant and Explosive Combustion in China(9140C3501020901)~~
基金supported by the National Natural Science Foundation of China(11447219)Defense Product Innovation Project,China~~
文摘直接法硝解乌洛托品制备黑索今的过程中合成了一种新型的环形副产物,采用硅胶柱层析法分离得到3,5-二硝基-1-氧-3,5-二氮杂环己烷,洗脱剂为:丙酮/二氯甲烷,梯度洗脱.以丙酮为溶剂培养得到了3,5-二硝基-1-氧-3,5-二氮杂环己烷单晶,用元素分析、傅里叶变换红外(FTIR)光谱、核磁共振氢谱(NMR)以及质谱(MS)对其结构进行了表征,用X射线单晶衍射仪测定了其晶体结构.结果表明,晶体C3H6N4O5分子量为178.12,属于单斜晶系,空间群P121/n1,晶胞参数:a=0.58128(13)nm,b=1.72389(14)nm,c=0.71072(6)nm,β=112.056°,V=0.66006(16)nm3,Z=4,DC=1.792 g cm–3,μ=0.17 mm–1,F(000)=368.0,最终偏差因子R=0.0397.用同步热分析仪技术研究了3,5-二硝基-1-氧-3,5-二氮杂环己烷的热行为,DSC曲线上在383.15和519.05 K分别有一个尖锐的熔化吸热峰和分解放热峰.另外,根据Kissinger方程及Flynn-Wall-Ozawa方程和不同升温速率下的TG曲线计算得到了该化合物的热分解动力学参数(活化能和指前因子),利用Coats-Redfern法研究了该物质的热分解机理.结果表明:3,5-二硝基-1-氧-3,5-二氮杂环己烷是一种低熔点、热稳定性好的化合物.Kissinger方程计算其活化能为212.32 k J mol–1,指前因子为6.20×1020 s–1,Flynn-Wall-Ozawa方程计算其活化能为210.39 k J mol–1,该物质的热分解动力学方程为G(α)=(1–α)–1–1,反应级数为2.
