| 第 52 卷第 3 期 |  | Vol. 52 No. 3 | | 2022 年 6 月 | Jun 2022 |
|
所屬欄目：農藥及中間體
微通道反應器連續法合成異硫氰基甲酸甲酯 |
| 劉 偉1，2，李 敏1，2，鐘 杰3，曾雪云1，2，陳 燦1，2，陳 明1，2，臧陽(yáng)陵1，2
（1. 湖南化工研究院有限公司 國家農藥創(chuàng )制工程技術(shù)研究中心，湖南 長(cháng)沙 410014；2. 農用化學(xué)品湖南省重點(diǎn)實(shí)驗室，湖南 長(cháng)沙 410014；3. 湖南海利化工股份有限公司，湖南 長(cháng)沙 410007） |
| 摘 要：以硫氰酸鈉、氯甲酸甲酯為原料，N，N-二甲基苯胺為催化劑在微通道反應器中連續合成異硫氰基甲酸甲酯，對停留時(shí)間、反應溫度、物料配比及催化劑用量進(jìn)行優(yōu)化。優(yōu)化反應條件為：反應溫度70 ℃，n（硫氰酸鈉）∶n（氯甲酸甲酯）=1.00∶1.05，m（硫氰酸鈉）∶m（催化劑）=1.000∶0.015，停留時(shí)間40 s。優(yōu)化條件下，產(chǎn)品含量97.5%，收率98.7%。相較于間歇法，連續法合成異硫氰基甲酸甲酯具有物料在線(xiàn)量小、反應停留時(shí)間短、工藝穩定安全等優(yōu)點(diǎn)，具有工業(yè)化應用前景。 |
| 關(guān)鍵詞：異硫氰基甲酸甲酯；連續化合成；微通道反應器 |
| 中圖分類(lèi)號：TQ455.4 文獻標識碼：A 文章編號：1009-9212（2022）03-0012-04 |
|
| 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 |
|
基金項目：湖南省企業(yè)科技創(chuàng )新創(chuàng )業(yè)團隊項目（湖南海利新材料科技創(chuàng )新創(chuàng )業(yè)團隊）。
|
作者簡(jiǎn)介：劉 偉（1985—），男，湖南張家界人，助理研究員，碩士，研究方向：有機合成（E-mail： 315352661@qq.com）。
|
收稿日期：2022-04-28
|
|