端羟基超支化聚酯分子结构的表征  

Molecular Structure Characterization of Hydroxyl-Terminated Hyperbranched Polyester

作　　者：张杰[1] 杨康[1] 张志平[1] 胡春圃[1] ZHANG Jie;YANG Kang;ZHANG Zhiping;HU Chunpu(School of Materials Science and Engineering,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学材料科学与工程学院,上海200237

出　　处：《功能高分子学报》2019年第2期206-211,254,共7页Journal of Functional Polymers

摘　　要：采用一维~1H-NMR、^(13)C-NMR、无畸变极化转移增强(DEPT)谱、二维核磁异核单量子相干谱(HSQC)和~1H-^(13)C异核远程相关谱(HMBC)等方法,对第2代超支化脂肪族聚酯HB-20的分子结构进行了表征。~1H-NMR和^(13)C-NMR谱图中各出峰得到归属,同时HB-20的分子骨架结构得以明确解析;由~1H-NMR中树枝状、线形和端基甲基(D-CH_3、L-CH_3和T-CH_3)三种结构相对峰面积计算得到HB-20的平均支化度为0.47;由羟值测试和核磁共振结果分别计算得到HB-20的数均分子量为1 878、1 876,两者接近。HB-20的分子结构得到明确的表征。The molecular structure of second generation hydroxyl terminated aliphatic hyperbranched polyester(HB-20)was characterized by nuclear magnetic resonance(NMR)analyses,including one-dimensional(1D)NMR technique(1H-NMR,13C-NMR and distortionless enhancement by polarization transfer(DEPT)NMR spectra)and two-dimensional(2D)NMR technique(heteronuclear single quantum coherence(HSQC)NMR and heteronuclear multipe bond coherence(HMBC)NMR spectra).Firstly,the peaks of the 1H-NMR and 13C-NMR spectra were initially assigned,and the four types of carbon atoms(CH3,CH2,CH,and quaternary carbon atom C*)in the HB-20 were distinguished by DEPT NMR spectra.Secondly,the detailed molecular structure information was further obtained by 2D NMR analysis.From the HSQC spectrum,the 13C-1H chemical shift correlation spectroscopy spectrum contained all the directly linked 13C-1H coupling relationships,and the positions of the related 1H and 13C in the molecular structure were determined;from the HMBC spectrum,the 13C and 1H coupling information separated by 2-3 chemical bonds was obtained,and the C-C correlation was confirmed to determine the molecular skeleton information of HB-20.According to the NMR analysis,the three relative peak areas of the confirmed T-CH 3,L-CH 3,and D-CH 3 structures in the 1H-NMR spectrum were determined to be 2.55,3.97 and 1.00 respectively,and the average degree of branching(DB)of HB-20 was calculated as 0.47.Moreover,the average molecular weight of HB-20 was calculated as 1 876 by NMR analysis,which was closed to that obtained from the hydroxyl value titration,about 1878.In summary,the molecular structure of HB-20 was clearly characterized.

关 键 词：超支化 HB-20 二维核磁共振 支化度 

分 类 号：O631[理学—高分子化学]