高等学校化学学报 ›› 2014, Vol. 35 ›› Issue (5): 1086.doi: 10.7503/cjcu20131109

• 高分子化学 • 上一篇    下一篇

新型含硼聚芳醚酮的制备、性能及在偶氮聚芳醚酮合成中的应用

王永鹏, 刘梦竹, 张宇轩, 林英健, 商赢双, 朱轩伯, 张海博(), 姜振华   

  1. 吉林大学化学学院, 麦克德尔米德实验室, 长春 130012
  • 收稿日期:2013-11-15 出版日期:2014-05-10 发布日期:2014-03-05
  • 作者简介:联系人简介: 张海博, 男, 博士, 副教授, 主要从事多相高分子材料研究. E-mail:zhanghaib@jlu.edu.cn
  • 基金资助:
    国家自然科学基金(批准号: 51103056)资助

Synthesis and Properties of a Novel Boron-containing Poly(arylether ketone) and Its Application in the Preparation of Azo Poly(aryl ether ketone)

WANG Yongpeng, LIU Mengzhu, ZHANG Yuxuan, LIN Yingjian, SHANG Yingshuang, ZHU Xuanbo, ZHANG Haibo*(), JIANG Zhenhua   

  1. Alan. G. MacDiarmid Institute, College of Chemistry, Jilin University, Changchun 130012, China
  • Received:2013-11-15 Online:2014-05-10 Published:2014-03-05
  • Contact: ZHANG Haibo E-mail:zhanghaib@jlu.edu.cn
  • Supported by:
    † Supported by the National Natural Science Foundation of China(No.51103056)

摘要:

利用双酚A型聚芳醚酮与联硼酸频哪醇酯在[Ir(COD)Cl]2和4,4'-二叔丁基-2,2'-联吡啶催化下反应, 制备了新型含硼酸酯双酚A型聚芳醚酮, 通过控制联硼酸频哪醇酯的投入量来实现硼酸酯的定量引入. 再经过高碘酸钠作用得到含硼酸双酚A型聚芳醚酮, 最后, 通过高效Suzuki-Miyaura反应将偶氮定量引入到聚芳醚酮主链. 利用核磁共振(1H NMR)确定了聚合物的结构, 利用凝胶渗透色谱(GPC)确定了聚合物的分子量, 利用差示扫描量热分析(DSC)和热失重分析(TGA)研究了聚合物的热性能, 利用紫外-可见光谱(UV-Vis)研究了偶氮聚芳醚酮的光谱学性能.

关键词: 聚芳醚酮, 硼化, 硼酸酯, 硼酸, Suzuki-Miyaura反应, 偶氮

Abstract:

Novel poly(aryl ether ketone)s with pendant pinacolboronate groups(PAEK-Bpin) and boric acid groups(PAEK-BOH) were synthesized. PAEK-Bpin was prepared by the borylation of poly(aryl ether ketone) in the presence of [IrCl(COD)]2 and dtbpy. The quantitative introduction of borate can be controlled by the amount of Bis(pinacolato)diboron(B2pin2). PAEK-BOH was obtained under the action of NaIO4. Azo-PAEK was obtained via Suzuki-Miyaura reaction. The structure and property characterizations of all related products were carried out using 1H-nuclear magnetic resonance(1H NMR), ultraviolet and visible spectrophotometer(UV-Vis), gel permeation chromatography(GPC), differential scanning calorimetry(DSC) and thermogravimetric analysis(TGA). The results of structure characterization suggest that products are synthesized. The results of GPC show that Ir catalyst and Suzuki-Miyaura reaction do not affect the molecular weight of the polymers. DSC results indicate that the glass transition temperature of PAEK-Bpin increases with the increase of the amount of boronate. However, PAEK-Bpin has good solubility in most of polar aprotic solvents. The preparation of boron-containing poly(aryl ether ketone) provides more broad prospects for further functionalization of the poly(aryl ether ketone).

Key words: Poly(aryl ether ketone), Borylation, Borate, Boric acid, Suzuki-Miyaura Reaction, Azo

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