第 49 卷第 3 期 Vol. 49 No. 3 2019 年 6 月 Jun 2019

所属栏目：农药及中间体 提高1氢-1，2，4-三氮唑收率及品质的研究

朱 鹏，徐刚亮，刘志勇* （江苏剑牌农化股份有限公司，江苏 建湖 224700）

摘　要：以甲酰胺与水合肼为原料，采用液面下滴加水合肼、引入乙二醇作为反应溶剂、应用结晶-过滤-漂洗-烘干的后处理方式，合成了1氢-1，2，4-三氮唑，并对其合成工艺条件进行了研究。优化的反应条件为：m（乙二醇）＝50% m（水合肼），n（甲酰胺）∶n（水合肼）＝2.1∶1.0，反应温度为168℃，反应时间为120 min。优化条件下，三氮唑收率为86.8%（以甲酰胺计三氮唑）或91.1%（以水合肼计），产品含量为98%，m.p.120~121℃。副产氨水中甲酰胺的含量为0.2%，水合肼的含量为0.1%。

关键词：三氮唑；甲酰胺；水合肼；乙二醇

中图分类号：TQ21　　文献标识码：A　　文章编号：1009-9212（2019）03-0007-05

Improvement of Yield and Quality of 1H-1,2,4-Triazole

ZHU Peng, XU Gang-liang, LIU Zhi-yong* (Jiangsu Sword Agrochemicals Co., Ltd., Jianhu 224700, China)

Abstract：1H-1,2,4-Triazole was synthesized as follows: formamide and hydrazine hydrate were used as raw materials, the hydrazine hydrate was added under the liquid surface, ethylene glycol was used as the reaction solvent, and crystallization-filtration-rinsing-drying was applied as the post-processing method. The parameters of the reaction were optimized. Optimal conditions were as followings: m(ethylene glycol) = 50% m(hydrazine hydrate), n(formamide)∶n(hydrazine hydrate)=2.1:1.0, reaction temperature of 168℃, reaction time of 120 min. The experimental results showed that the yield of triazole calculated based on the amount of formamide was up to 86.8%, the yield of triazole calculated based on the amount of hydrazine hydrate was up to 91.1%, the purity of product was of 98% with a melting point range of 120 to121℃. The concentrations of formamide and hydrazine hydrate were 0.2% and 0.1% in the by-product ammonia water, respectively.

Key words：triazole; formamide; hydrazine hydrate; ethylene glycol

作者简介：朱 鹏（1989-），男，江苏滨海人，硕士研究生，研究方向：农药合成及工艺研究（E-mail：zhupeng@swordchem.com）。

联 系 人：刘志勇，高级工程师，研究方向：农药合成及工艺研究（E-mail：liuzhiyong@swordchem.com）。

收稿日期：2019-05-29