4,4′-偶氮-1,2,4-三唑的合成工艺改进

Synthesis Improvement for 4,4'-Azobis(1,2,4-triazole)

采用次氯酸钠代替二氯异氰尿酸钠作为氧化剂对4,4′-偶氮-1,2,4-三唑的合成工艺进行了改进。研究了光照时间、有效氯与乙酸的摩尔比和反应温度三种不同条件对于反应工艺的影响。所得产品的结构和性能与文献结果进行了对比。结果表明,在避光的条件下,有效氯与乙酸的摩尔比为1∶2.5,反应温度为7℃时,收率为78%;与二氯异氰尿酸钠相比,以次氯酸钠作为氧化剂合成4,4′-偶氮-1,2,4-三唑的工艺不仅省略了4,4′-偶氮-1,2,4-三唑的分离提纯步骤,而且有效地解决了处理异腈尿酸的难题。

Sodium dichloroisocyanurate was replaced by sodium hypochlorite as the oxidant for improving the synthetic method of 4,4′-azobis（1,2, 4-triazole）. Three different factors, the illumination time, the molar ratio available chlorine to acetic acid and the reaction temperature, were studied for the influence of the reaction process. The structure and properties of the product obtained were compared with literature ones. Results show that under the condition of dark （0h illumination time）, the molar ratio available chlorine to acetic acid 1∶2.5 and 7 ℃, the yield is 78%. Compared with sodium dichloroisocyanurate, sodium hypochlorite used as the oxidizing agent to synthesize 4,4′-azobis（1,2,4-triazole） can not only omit the separation and purification of 4,4′-azobis（1,2,4-triazole）, but also solve the problem of processing the isocyanuric acid.