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松香基超支化聚酯的合成及其端基改性研究

Synthesis and Terminal Modification of Rosin Based Hyperbranched Polyester

  • 摘要: 以马尾松松香树脂酸和顺丁烯二酸酐合成了马来海松酸(MPA),通过马来海松酸与环氧丙醇的开环聚合,采用"一步法"合成了松香基超支化聚酯(RHBPE),采用 FT-IR、凝胶色谱(GPC)、1HNMR对聚酯的结构进行了表征。FT-IR分析结果表明马来海松酸和环氧丙醇反应良好,产物分子中有大量酯基和羟基,得到的超支化聚酯最大相对分子质量为5170,数均相对分子质量(Mn)为2547,重均相对分子质量(Mw)为2670,以1HNMR分析技术测得其支化度为0.54,该超支化产物具有较好的溶解性能和优越的热稳定性。用丙烯酰氯对松香基超支化聚酯进行改性,合成了端乙烯基松香基超支化聚酯(VRHBP),FT-IR和1HNMR分析结果表明松香基超支化聚酯的部分端基已经由羟基转变成为双键基团,其改性度为75%。

     

    Abstract: Maleopimaric acid (MPA) was synthesized from Pinus massoniana Lamb rosin and maleic anhydride. A hyperbranched polyester (RHBPE) was synthesized based on one-pot esterification between maleopimaric acid and glycidol. The RHBPE was characterized by FT-IR, GPC and 1HNMR. FT-IR analysis indicated that MPA reacted completely with glycidol, and RHBPE contained large number of ester and hydroxyl groups. GPC analysis indicated that the largest molecular weight of RHBPE is 5 170, number average molecular weight Mn is 2 547, and weight average molecular weight Mw is 2 670. DB was determined as 0.54 by 1HNMR proton integrating process. Dissolution experiment and TG analysis indicated that RHBPE had good solubility and thermal stability. RHBPE was modified with acryloyl chloride to give a modified rosin-based hyperbranched polymers (VRHBP) which contained terminal vinyl group. FT-IR and 1HNMR spectra indicated that the terminal hydroxyl groups of RHBPE have been partially changed into terminal vinyl groups, i.e. 75% of modification degree of RHBPE.

     

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