含能材料
含能材料
함능재료
ENERGETIC MATERIALS
2010年
1期
29-33
,共5页
有机化学%3-氨基-5-硝基-1,2,4三唑(ANTA)%3,5-二硝基-1,2,4三唑%合成%表征
有機化學%3-氨基-5-硝基-1,2,4三唑(ANTA)%3,5-二硝基-1,2,4三唑%閤成%錶徵
유궤화학%3-안기-5-초기-1,2,4삼서(ANTA)%3,5-이초기-1,2,4삼서%합성%표정
organic chemistry%3-amino-5-nitro-1,2,4-triazole(ANTA)%3,5-dinitro-1,2,4-triazole%synthesis%characterization
以3-氨基-5-硝基-1,2,4三唑(ANTA)、3,5-二硝基-1,2,4三唑的铵盐(ADNT)及2,4,6-三硝基氯苯为原料,设计、合成了1-苦基-3-氨基-5-硝基-1,2,4三唑,4-苦基-3,5-二硝基-1,2,4三唑2种未见文献报道的硝基三唑衍生物,其熔点分别为251～252 ℃,156～157 ℃,同时改进了2,4,6-三(3-氨基-5-硝基-1,2,4三唑)-1,3,5-均三嗪合成方法,并采用红外光谱、核磁共振光谱、元素分析等对目标化合物进行了结构表征.探讨了3-氨基-5-硝基-1,2,4三唑与2,4,6-三硝基氯苯缩合反应机理,并研究了反应介质、催化剂等关键因素对缩合反应的影响.确定适宜的反应条件为： DMF作为介质,温度70 ℃,时间8 h.
以3-氨基-5-硝基-1,2,4三唑(ANTA)、3,5-二硝基-1,2,4三唑的銨鹽(ADNT)及2,4,6-三硝基氯苯為原料,設計、閤成瞭1-苦基-3-氨基-5-硝基-1,2,4三唑,4-苦基-3,5-二硝基-1,2,4三唑2種未見文獻報道的硝基三唑衍生物,其鎔點分彆為251～252 ℃,156～157 ℃,同時改進瞭2,4,6-三(3-氨基-5-硝基-1,2,4三唑)-1,3,5-均三嗪閤成方法,併採用紅外光譜、覈磁共振光譜、元素分析等對目標化閤物進行瞭結構錶徵.探討瞭3-氨基-5-硝基-1,2,4三唑與2,4,6-三硝基氯苯縮閤反應機理,併研究瞭反應介質、催化劑等關鍵因素對縮閤反應的影響.確定適宜的反應條件為： DMF作為介質,溫度70 ℃,時間8 h.
이3-안기-5-초기-1,2,4삼서(ANTA)、3,5-이초기-1,2,4삼서적안염(ADNT)급2,4,6-삼초기록분위원료,설계、합성료1-고기-3-안기-5-초기-1,2,4삼서,4-고기-3,5-이초기-1,2,4삼서2충미견문헌보도적초기삼서연생물,기용점분별위251～252 ℃,156～157 ℃,동시개진료2,4,6-삼(3-안기-5-초기-1,2,4삼서)-1,3,5-균삼진합성방법,병채용홍외광보、핵자공진광보、원소분석등대목표화합물진행료결구표정.탐토료3-안기-5-초기-1,2,4삼서여2,4,6-삼초기록분축합반응궤리,병연구료반응개질、최화제등관건인소대축합반응적영향.학정괄의적반응조건위： DMF작위개질,온도70 ℃,시간8 h.
Two new heat-resistant explosives of 1-picryl-3-amino-5-nitro-1,2,4-triazole(TNTA-TNB) and 4-picryl-3,5-dinitro-1,2,4-triazole(DNT-TNB) were synthesized via condensation of 3-amino-5-nitro-1,2,4-triazole(ANTA)(or ammonium 3,5-dinitro-1,2,4-triazole(ADNT)) with 2,4,6-trinitrochlorobenzene. The condensation mechanism was explored and discussed. The effects of some key reaction conditions,such as media,temperature,time and catalysts,on condensation were investigated. The explosive synthesis was carried out at 70 ℃,8 h in DMF and NaF as catalyst. IR,NMR and elemental analysis confirmed the synthesized compound structures. In addition,we imroved the synthetic process of 2,4,6-tris(3-amino-5-nitro-1,2,4-triazole-1-yl)-1,3,5-triazine by means of direct reaction of ANTA with 2,4,6-trichloro-1,3,5-triazine omitting the preparation of ANTA-Na and without using phase transfer catalyst,lowering the production cost,simplifing the procedure,and improving the reaction safety.
