摘要
在邻苯二甲酸丁苄酯存在下,将乙醇酸低聚物加热解聚生成乙交酯和该有机溶剂的共沸物,通过环己烷洗涤后,过滤得到乙交酯粗品。研究结果表明,解聚溶剂与低聚物的质量比为2∶1,助溶剂用量为低聚物质量的25%,解聚温度为250℃,真空压力为3 kPa,催化剂Sb2O3用量为低聚物质量的1%时,条件最优。粗乙交酯的收率可达92.2%,苯酐质量分数低于2%,3次重结晶后乙交酯纯度超过99.5%,并通过核磁共振氢谱、紫外光谱、差示扫描量热仪等对乙交酯进行了表征与纯度分析。
The crude glycolide is synthesized by heating a mixture containing a glycolic acid oligomer and a high boiling polar organic solvent and then purified by washing with eyclohexane. The optimized conditions are as follows ：2：1 ratio of solvent and oligomer,0. 25% （ based on glycolic acid oligomer） of solubilizing agent,250~C of depolymerization temperature,3kPa of the reduced pressure and 1.0% of Sb203 catalyst. Under the optimal conditions ,the crude yield of glycolide can reach 92. 2%. After three times of recrystallization, the purity is higher than 99. 5%. The obtained glycolide has been identified by UVS, DSC and NMR.
出处
《现代化工》
CAS
CSCD
北大核心
2013年第12期79-82,共4页
Modern Chemical Industry
基金
江苏省高校自然科学研究重大项目(11KJA430007)
关键词
乙醇酸
聚乙交酯
乙交酯
溶液解聚
glycolic acid
polyglycolic acid
glycolide
solution-phase depolymerization
