IR法和~1H-NMR法表征Bi(OAc)_3催化乙交酯和D,L-丙交酯共聚的单体转化率  

The Monomer Conversion of the Copolymer of Glycolide and D,L-lactide Catalyzed by Bi(OAc)_3 Using Methods of IR and ~1H-NMR

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作  者:高建 连明磊 吴红 李琳 GAO Jian;LIAN Ming-lei;WU Hong;LI Lin(School of Chemistry and Materials Engineering,Liupanshui Normal Unversity,Liupanshui 553004,China)

机构地区:[1]六盘水师范学院化学与材料工程学院,贵州六盘水553004

出  处:《遵义师范学院学报》2019年第1期86-88,95,共4页Journal of Zunyi Normal University

摘  要:本文给出了一种测定Bi(OAc)_3催化乙交酯(GA)和D,L-丙交酯(D,L-LA)共聚合单体转化率的方法。GA与D,L-LA物质的量比为1:1,单体与催化剂物质的量比为3000:1,150℃下Bi(OAc)_3催化单体共聚4h.聚合产物经CHCl3和MeOH抽提纯化,测定产物聚乙丙交酯(PLGA)的收率。使用IR法分析溶剂洗涤后的PLGA中GA和D,L-LA的残留量。然后对PLGA的1H-NMR谱进行分析,根据特征峰积分面积计算聚合物中GA片段和D, L-LA片段的含量,进一步推导出单体的转化率。产物PLGA的平均收率为66.85%,GA的平均转化率为84.18%,D,L-LA的平均转化率为52.88%.该方法适合于研究环酯开环聚合过程中单体的转化率。This paper studied the monomer conversion of glycolide(GA) and D,L-lactide(D,L-LA) catalyzed by Bi(OAc)3.The molar ratio of GA and D,L-LA was 1 :1,the molar ratio of monomer and catalyst was 3000:1,and the copolymerization was carried out at150℃ for a period of 4h intiated by Bi(OAc)3.The polymer was extracted and purified by CHCl3 and MeOH,then the yield of polyglycolide-lactide(PLGA) was determined.The amount of GA and D,L-LA left in the PLGA after washing of solvent was determined using IR method.We analyzed the 1H-NMR spectra of PLGA,the content of GA and D,L-LA in the polymer chain was calculated according to the integral of the characteristic peaks,at the end the conversion rate of monomer was deduced.The average yield of PLGA was 66.86%,the average conversion rate of GA was 84.18%,and the average rate of D,L-LA was 52.88%.This method was suitable for the study of conversion rate of monomer in ring-opening polymerization of cyclic ester.

关 键 词:乙交酯 D L-丙交酯 共聚合 核磁共振 转化率 

分 类 号:R318[医药卫生—生物医学工程]

 

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