以吡唑为原料,经发烟硝酸和醋酐体系硝化后,将反应液在水热釜中高压反应,一锅法合成了3-硝基吡唑。产物经红外光谱、熔点、高效液相色谱表征。优化反应条件为:4.0 g吡唑、4.4 m L发烟硝酸、10.7 m L醋酐在冰水浴中反应1 h,然后将得到的...以吡唑为原料,经发烟硝酸和醋酐体系硝化后,将反应液在水热釜中高压反应,一锅法合成了3-硝基吡唑。产物经红外光谱、熔点、高效液相色谱表征。优化反应条件为:4.0 g吡唑、4.4 m L发烟硝酸、10.7 m L醋酐在冰水浴中反应1 h,然后将得到的反应液在170℃下、在水热釜中高压密封反应3 h,3-硝基吡唑的收率达46.2%。展开更多
Coordination to form polymer is emerging as a new technology for modifying or enhancing the properties of the existed energetic substances in energetic materials area. In this work, guanidine cation CN3 H6+ (Gu) and 3...Coordination to form polymer is emerging as a new technology for modifying or enhancing the properties of the existed energetic substances in energetic materials area. In this work, guanidine cation CN3 H6+ (Gu) and 3-amino-1,2,4-triazole C2H4N4(ATz) were crystallized into NaN5 and two novel energetic coordination polymers(CPs),(NaN5)5[(CH6-N3)N5](N5)3–(1) and(NaN5)2(C2H4N4)(2) were prepared respectively via a self-assembly process. The crystal structure reveals the co-existence of the chelating pentazole anion and organic component in the solid state. In polymer 1, Na+and N5– were coordinated to form a cage structure in which guanidine cation [C(NH2)3]+ was trapped;for polymer 2, a mixedligand system was observed;N5 – and ATz coordinate separately with Na+and form two independent but interweaved nets. In this way, coordination polymer has been successfully utilized to modify specific properties of energetic materials through crystallization. Benefiting from the coordination and weak interactions, the decomposition temperatures of both polymers increase from 111°C(1D structure [Na(H2 O)(N5)]?2 H2 O) to 118.4 and 126.5°C respectively. Moreover, no crystallized H2 O was generated in products to afford the anhydrous compounds of pentazole salts with high heats of formation( >800 kJ mol–1). Compared to traditional energetic materials, the advantage in heats of formation is still obvious for the cyclo-N5– based CPs, which highlights cyclo-N5– as a promising energetic precursor for high energy density materials(HEDMs).展开更多
文摘以吡唑为原料,经发烟硝酸和醋酐体系硝化后,将反应液在水热釜中高压反应,一锅法合成了3-硝基吡唑。产物经红外光谱、熔点、高效液相色谱表征。优化反应条件为:4.0 g吡唑、4.4 m L发烟硝酸、10.7 m L醋酐在冰水浴中反应1 h,然后将得到的反应液在170℃下、在水热釜中高压密封反应3 h,3-硝基吡唑的收率达46.2%。
基金financially supported by the National Natural Science Foundation of China (11702141, 21771108, and U1530101)
文摘Coordination to form polymer is emerging as a new technology for modifying or enhancing the properties of the existed energetic substances in energetic materials area. In this work, guanidine cation CN3 H6+ (Gu) and 3-amino-1,2,4-triazole C2H4N4(ATz) were crystallized into NaN5 and two novel energetic coordination polymers(CPs),(NaN5)5[(CH6-N3)N5](N5)3–(1) and(NaN5)2(C2H4N4)(2) were prepared respectively via a self-assembly process. The crystal structure reveals the co-existence of the chelating pentazole anion and organic component in the solid state. In polymer 1, Na+and N5– were coordinated to form a cage structure in which guanidine cation [C(NH2)3]+ was trapped;for polymer 2, a mixedligand system was observed;N5 – and ATz coordinate separately with Na+and form two independent but interweaved nets. In this way, coordination polymer has been successfully utilized to modify specific properties of energetic materials through crystallization. Benefiting from the coordination and weak interactions, the decomposition temperatures of both polymers increase from 111°C(1D structure [Na(H2 O)(N5)]?2 H2 O) to 118.4 and 126.5°C respectively. Moreover, no crystallized H2 O was generated in products to afford the anhydrous compounds of pentazole salts with high heats of formation( >800 kJ mol–1). Compared to traditional energetic materials, the advantage in heats of formation is still obvious for the cyclo-N5– based CPs, which highlights cyclo-N5– as a promising energetic precursor for high energy density materials(HEDMs).
基金financially supported by the joint fund of the National Natural Science Foundation of China and China Academy of Engineering Physics (NSAF, U1530101)
