一种改进的3-氨基-4-硝基呋咱合成方法

Synthesis of 3-Amino-4-nitrofurazan by an Improved Method

以3,4-二氨基呋咱(DAF)为原料,过氧化氢为氧化剂,以钨酸钠-草酸为共催化剂,代替传统合成方法的钨酸钠-浓硫酸共催化剂,合成了3-氨基-4硝基呋咱(ANF)。采用正交设计的方法,考察了反应时间、反应温度和共催化剂用量对产率的影响,最终得到ANF合成的较佳工艺条件:反应时间6h,反应温度30℃,共催化剂与原料摩尔比1∶1,在上述条件下ANF产率可达33.7%。

3-Amino-4-nitrofurazan（ANF） was successfully synthesized from 3,4-diamino-furazan（DAF） by an improved method. In the synthesis,oxalic acid was employed with sodium tungstate as a cocatalyst instead of sulfuric acid,and 30% H2O2 was employed as the oxider instead of 50% H2O2. The effects of reaction temperature,reaction time and quantity of catalyst on the conversion of DAF to ANF was studied by orthogonal design. The optimal reaction conditions were obtained as follows： reaction temperature 30 ℃ ,reaction time 6 h,the mole ratio of eocatalyst to DAF 1 ： 1. The conversion of DAF was about 33.70% under the optimal reaction conditions.