聚合物共混物的超高效液相色谱-空间排阻色谱在线联用分离与表征  

Separation and Characterization of Polymer Blends Using Online Ultra-high Performance Liquid Chromatography-Size Exclusion Chromatography

作　　者：汪明芳 付华[2] 付志博 王月荣 章弘扬 张敏 胡坪 WANG Mingfang;FU Hua;FU Zhibo;WANG Yuerong;ZHANG Hongyang;ZHANG Min;HU Ping(Shanghai Key Laboratory of Functional Materials Chemistry,School of Chemistry&Molecular Engineering,East China University of Science and Technology,Shanghai 200237,China;School of Chemistry Engineering,Qinghai University,Xining 810016,China;Shanghai Key Laboratory of New Drug Design&Modern Engineering Center for TCM,School of Pharmacy,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学化学与分子工程学院,上海市功能性材料化学重点实验室,上海200237 [2]青海大学化工学院,西宁810016 [3]华东理工大学药学院,上海市新药设计重点实验室,上海200237

出　　处：《高等学校化学学报》2022年第4期24-32,共9页Chemical Journal of Chinese Universities

基　　金：国家自然科学基金(批准号:81973285)资助。

摘　　要：黏合剂和涂料行业中,聚合物共混物表征是分析的难题,分离技术的研究一直备受关注.本文设计并搭建了超高效液相色谱-空间排阻色谱在线联用系统(UHPLC-SEC),采用羟基聚丁二烯(HTPB)考察了二维色谱系统的溶剂兼容性及正交性,以苯乙烯-丁二烯嵌段共聚物(SBS)、苯乙烯-异戊二烯嵌段共聚物(SIS)和聚甲基丙烯酸酯(PMMA)共混物研究了二维色谱系统的适用性.结果表明,HTPB分子量及分布的UHPLC-SEC测定结果与SEC测定结果一致,峰尖分子量(M_(p))为3407 Da,重均分子量(M_(w))为6573 Da,分散系数(PDI)为2.36,相对标准偏差(RSD)均小于5.7%,系统的溶剂兼容性和正交性良好.UHPLC-SEC法测得聚合物共混物中PMMA,SBS和SIS的M_(p),M_(w)和PDI与单个聚合物的SEC测定结果的相对误差均小于7.1%.PMMA,SBS和SIS共混物在200℃加热3 h后,PMMA稳定不变,SBS和SIS组分明显降解.UHPLC-SEC在线联用方法对聚合物共混物的表征结果准确、重复性好,为聚合物配方产品的失效分析提供了一种重要且有效的手段.The characterization of polymer blends is a difficult problem in adhesives and coatings industry,and the studies on the separation of complex mixtures are always popular.In this paper,an online ultra-high performance liquid chromatography-size exclusion chromatography(UHPLC-SEC)system was designed and set up.The solvent compatibility and orthogonality of the two-dimensional chromatography system were investigated using the hydroxyl polybutadiene(HTPB).The applicability of the two-dimensional chromatography was studied in the separation and characterization of each fraction from the styrene-butadiene block copolymer(SBS),styrene-isoprene block copolymer(SIS)and polymethacrylate(PMMA)blends.The results showed that the molecular weight and distribution of HTPB were determined by UHPLC-SEC,which were consistent with those determined by SEC.The peak molecular weight(Mp),the weight average molecular weight(Mw)and the polymer dispersity index(PDI)of HTPB were 3407 Da,6573 Da and 2.36,respectively,and the relative standard deviations(RSDs)were less than 5.7%.Moreover,the solvent compatibility and orthogonality of the system were good.Compared to the existing SEC method,the relative errors of Mp,Mw and PDI of PMMA,SBS and SIS fraction measured by UHPLC-SEC were all less than 7.1%.The PMMA remained stable after the mixture of PMMA,SBS and SIS was heated at 200℃for 3 h,while SBS and SIS components degraded significantly.Due to the good accuracy and reproducibility of the UHPLC-SEC method in the characterization of the polymer blends,it is suitable for the failure analysis of the polymer formulations.

关 键 词：超高效液相色谱 空间排阻色谱 二维色谱 聚合物共混物 

分 类 号：O657[理学—分析化学] O631.6[理学—化学]