减压精馏-熔融结晶分离1,3-丙烷磺内酯的研究

Study on Separation of 1,3-Propanesultone by Vacuum Distillation and Melt Crystallization

为了达到锂离子电池电解液添加剂的品质要求,在制备电子级1,3-丙烷磺内酯的过程中,采用了减压蒸馏-熔融结晶的提纯工艺。工业级1,3-丙烷磺内酯通过减压蒸馏,在135～145℃之间得到了纯度为99. 0%～99. 5%的粗产品,经熔融结晶精制后,产品纯度可达99. 9%以上。另研究发现,1,3-丙烷磺内酯粗产品的纯度只有达到99. 0%以上时,通过一次熔融结晶后的纯度才能达到99. 9%以上,且收率可达90%以上。

To meet the quality requirements of electrolytic liquid additives in lithium-ion batteries,a vacuum distillation and molten crystallization purification process was used in the preparation of electron-grade 1,3-propanesultone.The industrial grade 1,3-propanesultone was distilled by vacuum distillation to obtain crude products with purity of 99.0%~99.5%between 135℃and 145℃.After refined by melt crystallization,the purity of the product could reach 99.9%or more.The results indicated that when the purity of 1,3-propanesultone crude products reached over 99.0%,the purity could reach 99.9%or more after refined by melt crystallization,and the yield could reach more than 90%.