| 第 52 卷第 3 期 |  | Vol. 52 No. 3 | | 2022 年 6 月 | Jun 2022 |
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所属栏目：农药及中间体
微通道反应器连续法合成异硫氰基甲酸甲酯 |
| 刘 伟1，2，李 敏1，2，钟 杰3，曾雪云1，2，陈 灿1，2，陈 明1，2，臧阳陵1，2
（1. 湖南化工研究院有限公司 国家农药创制工程技术研究中心，湖南 长沙 410014；2. 农用化学品湖南省重点实验室，湖南 长沙 410014；3. 湖南海利化工股份有限公司，湖南 长沙 410007） |
| 摘 要：以硫氰酸钠、氯甲酸甲酯为原料，N，N-二甲基苯胺为催化剂在微通道反应器中连续合成异硫氰基甲酸甲酯，对停留时间、反应温度、物料配比及催化剂用量进行优化。优化反应条件为：反应温度70 ℃，n（硫氰酸钠）∶n（氯甲酸甲酯）=1.00∶1.05，m（硫氰酸钠）∶m（催化剂）=1.000∶0.015，停留时间40 s。优化条件下，产品含量97.5%，收率98.7%。相较于间歇法，连续法合成异硫氰基甲酸甲酯具有物料在线量小、反应停留时间短、工艺稳定安全等优点，具有工业化应用前景。 |
| 关键词：异硫氰基甲酸甲酯；连续化合成；微通道反应器 |
| 中图分类号：TQ455.4 文献标识码：A 文章编号：1009-9212（2022）03-0012-04 |
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| Continuous Synthesis of Methoxycarbonyl Isothiocyanate in Microchannel Reactor |
| LIU Wei1,2, LI Min1,2, ZHONG Jie3, ZENG Xue-yun1,2, CHEN Can1,2, CHEN Ming1,2, ZANG Yang-ling1,2
(1. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry Co., Ltd., Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 3. Hunan Haili Chemical Industry Co., Ltd., Changsha 410007, China) |
| Abstract：Using sodium thiocyanate and methyl chloroformate as raw materials and N,N-dimethylaniline as catalyst a continuous synthetical method for methoxycarbonyl isothiocyanate in a microchannel reactor was desired. The residence time, reaction temperature, ratio of reactants and catalyst dosage were optimized. The optimal reaction conditions as follows: the reaction temperature of 70 ℃; n(sodium thiocyanates):n(methyl chloroformate) was of 1.00∶1.05; m(sodium thiocyanate)∶m(catalyst) was of 1.000∶0.015; and the residence time of 40 s. Under these conditions, the purity reached is of 97.5%; and the yield of process is 98.7%. Compared with the batch method, this continuous method for synthesizing methoxycarbonyl isothiocyanate has the advantages of small online amount of materials, short reaction residence time, stable and safe process, etc., and has a high industrial application prospect. |
| Key words：methoxycarbonyl isothiocyanate; continuous synthesis; microchannel reactor |
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基金项目：湖南省企业科技创新创业团队项目（湖南海利新材料科技创新创业团队）。
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作者简介：刘 伟（1985—），男，湖南张家界人，助理研究员，硕士，研究方向：有机合成（E-mail： 315352661@qq.com）。
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收稿日期：2022-04-28
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