N,N-双四唑胺的合成工艺改进与研究-《爆破器材》

文章信息/Info

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

作者:: 鲁学峰^①; 卫延安^①②; 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）

Author(s):: LU Xuefeng^①; WEI Yanan^①②; ①School of Chemical Engineering，Nanjing University of Scienceand Technology (Jiangsu Nanjing，210094)
②National Quality Supervisionand Inspection Center for Industrial Explosive Materials(Jiangsu Nanjing，210094)

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(NaN₃)∶n(HCl) = 1∶2∶1，在T=60℃，调节pH=3后，加热至100 ℃反应24 h，冷却至10 ℃左右，调节pH=2，产率达89.5%，纯度可达99%。

Abstract:: 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 C₂N₃Na, NaN-3 and acid was 1∶2∶1; pH=3 at 60℃, the n=100℃ for 24 h; at last, T=10℃ and pH=2. With this method, the yield was 89.5% and the purity was 99%.