化学工程2023,Vol.51Issue(12):15-19,55,6.DOI:10.3969/j.issn.1005-9954.2023.12.004
精馏-熔融结晶耦合分离乙二醇-碳酸乙烯酯
Separation of ethylene glycol and ethylene carbonate by distillation and melt crystallization
林杰 1仇玉静 1刘畅 1罗国华 2戴晓兵3
作者信息
- 1. 北京石油化工学院 新材料与化工学院,北京 102617
- 2. 北京石油化工学院 新材料与化工学院,北京 102617||燃料清洁化及高效催化减排技术北京市重点实验室,北京 102617
- 3. 珠海市赛纬电子材料股份有限公司,广东珠海 519000
- 折叠
摘要
Abstract
EC(ethylene carbonate)was produced in Ca-Zn composite oxide catalytical alcoholysis process using urea and EG(ethylene glycol)as raw materials,and the crude product was separated by distillation-melt crystallization method.An efficient separation process was developed by studying the effects of distillation,crystallization final temperature,sweating final temperature and crystal seed.As a result,optimal technological conditions to refine EC from EC-EG system is acquired and they are listed as follows.Initially,the remaining catalyst in the crude product is removed by flash evaporation.Then the byproduct(2-oxazolidone)is removed by preliminary distillation and the product with EC mass fraction at 80% is collected for further refinement.The melting crystallization is employed to thoroughly separated EC from this product and the optimized operations are listed as follows.It is kept at 34 ℃ for 20 min and then cooled down to 30 ℃ at 0.05 ℃/min.Subsequently,pure EC seed is added to start slow crystallization.The whole crystallization procedure is conducted at 16 ℃ for 20 min and the EC crystals are separated from mother liquor for final refinement.Purification for these crystals reaches to 95.49% by sweating.It is conducted at 32 ℃ for 20 min after the temperature rising from 16 ℃ to 32 ℃ at 0.05 ℃/min.Finally,the purity of EC is increased to more than 99.9% after purification in distillation tower under high reflux-ratio operation.关键词
乙二醇/碳酸乙烯酯/分离/蒸馏/熔融结晶Key words
ethylene glycol/ethylene carbonate/separation/distillation/melt crystallization分类
化学化工引用本文复制引用
林杰,仇玉静,刘畅,罗国华,戴晓兵..精馏-熔融结晶耦合分离乙二醇-碳酸乙烯酯[J].化学工程,2023,51(12):15-19,55,6.