二硫化四乙基秋兰姆的流动化学合成技术开发  

Development of Continuous-flow Synthesis Technology of Tetraethylthiuram Disulfide

作　　者：张雁 张智亮 宋士杰 王芳晓 付顺国 成兰兴 王艳利 ZHANG Yan;ZHANG Zhiliang;SONG Shijie;WANG Fangxiao;FU Shunguo;CHENG Lanxing;WANG Yanli(Hebi UHOO Rubber Chemicals Co.Ltd.,Hebi 458000,Henan China;Henan Chemical Industry Research Institute Co.Ltd.,Zhengzhou 450052,Henan China)

机构地区：[1]鹤壁元昊化工有限公司,河南鹤壁458000 [2]河南省化工研究所有限责任公司,郑州450052

出　　处：《河南科学》2021年第12期1941-1945,共5页Henan Science

基　　金：鹤壁市重大创新专项(20191210007)。

摘　　要：采用微通道连续流负载催化剂微填充固定床反应装置,对二硫化四乙基秋兰姆的合成进行了工艺探索.通过单因素实验,考察原料配比、反应温度、反应时间、体系压力、催化剂的影响.结果表明,最优工艺条件为:以二乙胺、二硫化碳、氧气为原料,其物质的量比1∶1∶0.36,中间体溶液合成温度为-10~10℃,固定床温度为60~65℃,体系压力为0.3~0.5 MPa,反应时间2 min,催化剂为Mn-Al;O;、Cu-Al;O;、Mn-C或Cu-C,即可得到外观好、收率高、纯度高的产品;利用微混合器、微反应器的协同耦合,反应时间可从几小时缩短到几十秒,成功解决了反应不彻底和传统工艺强放热带来的爆炸风险,实现化工过程的微型化、绿色化和本质安全化;以金属负载微填充固定床气液催化反应制备二硫化四乙基秋兰姆新工艺,实现了催化剂和产品的分离,且无副产物产生.By using the microchannel continuous flow load catalyst microfill fixed bed reaction device,the technological conditions for the synthesis of tetraethylthiuram disulfide was explored.By using a single factor experiment,the effects of the raw material ratio,reaction temperature,reaction time,catalysts were investigated.The optimum technological conditions are as follows:diethylamine,carbon disulfide,and oxygen as raw materials,the amount of substance 1∶1∶0.36,the synthesis temperature of the intermediate solution-10 to 10℃,the temperature of the fixed bed 60 to 65℃,the system pressure 0.3~0.5 MPa,the reaction time 2 min,Mn-Al;O;,Cu-Al;O;,Mn-C or Cu-C as catalyst.The products with good appearance,high yield,high purity can be obtained.By using the cooperative coupling of the micromixer and microreactor,the reaction time can be shortened from several hours to tens of seconds.It successfully solves the explosion risk caused by incomplete reaction and traditional process strong exothermic reaction,realizing the miniaturization,green development and essentially safe of the chemical process.A new process of tetraethylthiuram disulfide is prepared by gas and liquid catalytic reaction of metal load microfilled fixed bed,realizing the separation of catalyst and product,without by-product.

关 键 词：二乙胺 氧气 二硫化四乙基秋兰姆 微通道 固定床 

分 类 号：O622.7[理学—有机化学]