温和条件下Sc(OTf)3催化合成聚酯二元醇  

Synthesis of Polyester Diol under Mild Conditions Catalyzed by Sc(OTf)_3

作　　者：罗玉梅[1] 孙绪兵[1] 梁兵[1] 

机构地区：[1]高分子材料工程国家重点实验室,四川大学成都610065

出　　处：《应用化学》2008年第8期948-951,共4页Chinese Journal of Applied Chemistry

摘　　要：以三氟甲烷磺酸钪—Sc(CF3SO3)3(简称Sc(OTf)3)为催化剂,在低于120℃的温和条件下,合成了聚己二酸1,4-丁二醇酯二醇。研究了反应温度、催化剂用量、合成工艺等对酯化反应和缩聚反应的影响,并采用FT-IR、1H NMR、GPC等测试技术对合成的产物进行了结构表征。结果表明,不除水时的最佳反应条件为:温度90℃,催化剂用量占单体摩尔数的0.1%,n(醇)∶n(酸)=1.1∶1,回流11h,酯化率为93%;而减压除水时,在相同条件下,反应8h,酯化率可达到99%。不除水时酯化速率和缩聚速率均较慢,减压除水后速率明显加大,产物分子量增加,分子量分布变窄。FT-IR和1H NMR图谱分析表明,几乎无副产物生成。Esterification of adipic acid with 1,4-butanediol was carried out in the presence of scandium trifluoromethanesuffonate [ Sc（OTf） 3 ] as a Lewis acid catalyst under mild conditions. The effects of reaction temperature, catalyst dosage, and synthesis method on the esterification and the polycondensation were investigated. The product was characterized by FT-IR, ^1H NMR and GPC. Under the optimum conditions of 90 ℃, Sc （OTf） 3 0. 1%, molar ratio of 1,4-butanediol to adipic acid 1.1 ： 1, reflux time 11 h, the percent of esterification was 93% without removing water, over 99% with water removed. The esterification and the polycondensation were both slow without removing water. With water removed, the reaction rate was improved greatly. The molecular mass also increased, and the molecular mass distribution became narrow. FT-IR and ^1H NMR indicated that there was no by-product.

关 键 词：三氟甲烷磺酸钪 低温 酯化 聚酯二元醇 

分 类 号：O631.5[理学—高分子化学]