摘要
提供了一种高效的乙二醇(双丙腈)醚的合成方法,该方法是在催化剂二-(三甲基硅基)胺基锂(20%四氢呋喃溶液)作用下,以乙二醇和丙烯腈为原料一步法反应得到。该反应条件温和,反应温度控制在35℃左右,反应结束后,先用稀硫酸调节pH值至6左右,然后减压蒸馏除去未反应的丙烯腈、四氢呋喃以及少量水分,再经过高真空精馏即可得到纯度大于99.9%的产品乙二醇(双丙腈)醚。该合成方法的物质的量收率以乙二醇计大于90%,并且中间体单醚经回收套用后,物质的量收率可达到95%,该工艺既可满足作为高品质锂离子电池电解液添加剂的应用要求,又可用于大规模的工业化生产。
This paper presents an efficient synthesis method of ethylene glycol bis(propionitrile)ether,which is obtained by one-step reaction of ethylene glycol and acrylonitrile under the action of Di-(trimethylsilyl)amine lithium(20%tetrahydrofuran solution)as catalyst.The reaction conditions are mild,the temperature is controlled at about 30℃.After the reaction,the pH is adjusted to about 6 with dilute sulfuric acid,and then the unreacted acrylonitrile,tetrahydrofuran and a small amount of water are removed by vacuum distillation.After high vacuum rectification,ethylene glycol(dipropanitrile)ether with purity greater than 99.9%can be obtained.The molar yield of the method is more than 90%(in glycol terms),and the molar yield can reach 95%after of the intermediate mono-ether was recycled and applied to reaction.This synthesis technology can not only meet the application requirements of high quality lithium-ion battery electrolyte additives,but also can be used in large-scale industrial production.
作者
周怡
王怡然
孔祥儒
胡成楠
杨千镱
Zhou Yi;Wang Yiran;Kong Xiangru;Hu Chengnan;Yang Qianyi(Fushun Shunheg Chemical Co.,Ltd.,Fushun113006,China;College of Food Science and Nutrition Engineering,China Agricultural University,Beijing 100091,China;Fushun Petrochemical Company of Petro China,Fushun 113099,China)
出处
《山东化工》
CAS
2024年第16期66-69,共4页
Shandong Chemical Industry