Synthesis and Characterization of Hyperbranched Poly(ester-amide)s from Commercially Available Dicarboxylic Acids and Multihydroxyl Primary Amines

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• 作者：Xiuru Li ; Xianfeng Lu ; Ying Lin ; Jie Zhan ; Yuesheng Li ; Zhiqiang Liu ; Xuesi Chen ; Shuying Liu
• 刊名：Macromolecules
• 出版年：2006
• 出版时间：November 14, 2006
• 年：2006
• 卷：39
• 期：23
• 页码：7889 - 7899
• 全文大小：274K
• 年卷期：v.39,no.23(November 14, 2006)
• ISSN：1520-5835

文摘

A new method for syntheses of hyperbranched poly(ester-amide)s from commercially availableA₂ and CB_x type monomers has been developed on the basis of a series of model reactions. The aliphatic andsemiaromatic hyperbranched poly(ester-amide)s with multihydroxyl end groups are prepared by in situ thermalpolycondensation of intermediates obtained from dicarboxylic acids (A₂) and multihydroxyl primary amines (CB_x)in N,N-dimethylformamide. Analyses of FTIR, ¹H NMR, and ¹³C NMR spectra revealed the structures of thepolymers obtained. The MALDI-TOF MS of the polymers indicated that cyclization side reactions occurredduring polymerization. The hyperbranched poly(ester-amide)s contain configurational isomers observed by ¹³Cand DEPT ¹³C NMR spectroscopy. The DBs of the polymers were determined to be 0.38-0.62 by ¹H NMR orquantitive ¹³C NMR and DEPT 135 spectra. These polymers exhibit moderate molecular weights, with broaddistributions determined by size exclusion chromatography (SEC), and possess excellent solubility in a varietyof solvents such as N,N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, and ethanol, and display glass-transition temperatures (T_gs) between -2.3 and 53.2 C, determined by DSC measurements. The thermogravimetricanalytic measurement revealed that the decomposition temperature of the polymers at 10% weight-loss temperature(T_d¹⁰) ranged from 333 to 397 C in nitrogen.