高等学校化学学报 ›› 2011, Vol. 32 ›› Issue (5): 1216.

• 研究论文 • 上一篇    下一篇

双酚芴双胺型苯并噁嗪树脂的合成、结构及热性能

孙建新,史铁钧,徐慧,吴星林   

  1. 合肥工业大学化工学院, 合肥 230009
  • 收稿日期:2010-05-24 修回日期:2010-11-28 出版日期:2011-05-10 发布日期:2011-04-11
  • 通讯作者: 史铁钧 E-mail:stjhfut@163.com
  • 基金资助:

    国家自然科学基金(批准号: 50973024)资助.

Synthesis, Structure and Thermal Properties of Bisphenol Fluorene Diamine Benzoxazine

SUN Jian-Xin, SHI Tie-Jun*, XU Hui, WU Xing-Lin   

  1. School of Chemical Technology, Hefei University of Technology, Hefei 230009, China
  • Received:2010-05-24 Revised:2010-11-28 Online:2011-05-10 Published:2011-04-11
  • Contact: SHI Tie-Jun E-mail:stjhfut@163.com
  • Supported by:

    国家自然科学基金(批准号: 50973024)资助.

摘要: 首先以9-芴酮、苯酚为原料,98%浓硫酸做催化剂、2-巯基丙酸为助催化剂,合成了双酚芴[学名9,9-双(4-羟苯基)芴],再由其与乙二胺和多聚甲醛合成了线形双酚芴双胺型苯并噁嗪树脂(BF-eda树脂)。采用FT–IR, 1H–NMR和13C–NMR等分析手段对BF-eda树脂的化学结构进行了表征;用凝胶渗透色谱法测得BF-eda树脂的数均分子量为4690,分子量分布PDI为2.93;利用DSC对BF-eda树脂的热固化行为进行了研究,并使用TGA分析了所得聚苯并噁嗪的热稳定性。在氮气氛中,BF-eda树脂在253℃左右开环聚合,聚苯并噁嗪的分解温度为344℃,失重5%时的温度为357℃,900℃时的残炭率为51%。

关键词: 双酚芴, 苯并噁嗪, 线形双酚芴双胺型苯并噁嗪, 耐热性能

Abstract: 9,9-bis(4-hydroxyphenyl)-fluorene (Bisphenol Fluorene,BHPF) was synthesized from phenol and 9-fluorenone using 98% sulfuric acid as catalyst and 2-mercaptopropionic as promoter, and then a liner BHPF-diamine benzoxazine (BF-eda resin) was synthesized using BHPF, ethylenediamine and paraformaldehyde. Chemical structure of the BF-eda resin were verified by Fourier transform infrared spectroscopy (FT-IR), 1H and 13C nuclear magnetic resonance spectroscopies(NMR). The GPC analysis presents the number average molecular weight of BF-eda resin is 4690,and the polydispersity index (PDI) is 2.93. The curing behavior of BF-eda resin was studied by differential scanning calorimetry (DSC) and the thermal stabilization of polybenzoxazine was evaluated with thermogravimetric analysis (TGA).The ring-opening polymerization temperature of BF-eda resin is about 253℃, the thermal decomposition temperature of polybenzoxazine is 344℃, the temperature at 5% weight loss is 357℃, and the char yield ratio is 51% at 900℃.

Key words: 9,9-bis(4-hydroxyphenyl)-fluorene(BHPF), benzoxazine, liner bisphenol fluorene-diamine benzoxazine, thermal resistance

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