N,N-双四唑胺的合成工艺改进与研究  

Study and Improvement of the Synthesis of N,N-Bis( 1H-tetrazol-5-yl) amine

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作  者:鲁学峰[1] 卫延安[1,2] 

机构地区:[1]南京理工大学化工学院,江苏南京210094 [2]国家民用爆破器材质量监督检验中心,江苏南京210094

出  处:《爆破器材》2015年第2期14-17,共4页Explosive Materials

摘  要:以双氰胺钠和叠氮化钠为主要原料,加热分子内环化得到N,N-双四唑胺,并采用IR、NMR、MS等方法,对产品结构表征。探讨了N,N-双四唑胺合成反应机理,考察了溶液酸碱性、反应温度及反应时间等关键因素对结果的影响,获得适宜反应条件:摩尔比为n(C2N3Na)n(Na N3)n(HCl)=121,在T=60℃,调节p H=3后,加热至100℃反应24 h,冷却至10℃左右,调节p H=2,产率达89.5%,纯度可达99%。N,N-Bis( 1H-tetrazol-5-yl) amine was synthesized via a novel route by intramolecular cyclization conditioning the reaction system,in which sodium dicyandiamide and sodium azide was used as the main raw materials. The result was characterized by IR,NMR,and MS etc. The mechanism of the reaction was proposed. The key factors affecting the yield,such as acidity or basicity of the reaction system,reaction temperature and time,were also investigated. The optimized procedures are as follows: the molar ratio of C2N3 Na,Na N3 and acid was 1 2 1; p H = 3 at 60℃,then T =100℃ for 24 h; at last,T = 10℃ and p H = 2. With this method,the yield was 89. 5% and the purity was 99%.

关 键 词:含能材料 N N-双四唑胺 气体发生剂 双四唑 重氮化 

分 类 号:TJ55[兵器科学与技术—军事化学与烟火技术] O621.3[理学—有机化学]

 

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