化工学报 ›› 2014, Vol. 65 ›› Issue (9): 3705-3711.DOI: 10.3969/j.issn.0438-1157.2014.09.055

• 材料化学工程与纳米技术 • 上一篇    下一篇

含DOPO的双酚A-单苯并(口恶)嗪合成、表征及其固化特性

刘建华1, 史铁钧1, 徐国梅1,2, 王权1, 王启东1   

  1. 1 合肥工业大学化工学院, 安徽 合肥 230009;
    2 皖西学院材料与化工学院, 安徽 六安 237012
  • 收稿日期:2013-12-30 修回日期:2014-03-14 出版日期:2014-09-05 发布日期:2014-09-05
  • 通讯作者: 史铁钧
  • 基金资助:

    国家自然科学基金项目(51273054)。

Synthesis, characterization and curing characteristics of single benzoxazine containing DOPO based on bisphenol A

LIU Jianhua1, SHI Tiejun1, XU Guomei1,2, WANG Quan1, WANG Qidong1   

  1. 1 School of Chemical Engineering, Hefei University of Technology, Hefei 230009, Anhui, China;
    2 Department of Materials and Chemical Engineering, West Anhui University, Lu'an 237012, Anhui, China
  • Received:2013-12-30 Revised:2014-03-14 Online:2014-09-05 Published:2014-09-05
  • Supported by:

    supported by the National Natural Science Foundation of China (51273054).

摘要: 以双酚A、苯胺、多聚甲醛为原料,合成了双酚A-双苯并(口恶)嗪(DBOZ),再用其与DOPO(9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物)反应,合成了含DOPO的双酚A-单苯并(口恶)嗪(DBDO)。采用红外、核磁共振(氢谱核磁共振和碳谱核磁共振)等分析手段对DBOZ和DBDO的化学结构进行了表征;采用差示扫描量热仪对DBOZ和DBDO的固化特性进行研究,使用热重分析分析了所得聚苯并(口恶)嗪的热稳定性。结果表明:在N2气氛中,DBOZ在205℃左右开环聚合,热分解温度为312℃,在373℃分解速度达到最快,在800℃时的残碳率为37.19%;在N2气氛中,DBDO的热分解温度为353℃,在443℃分解速度达到最快,在800℃时的残碳率为39.60%。

关键词: 合成, 聚合, 热稳定性, 核磁共振, 双酚A-双苯并(口恶)嗪, 含DOPO的双酚A-单苯并(口恶)嗪

Abstract: Double benzoxazine based on bisphenol A(DBOZ)was synthesized from bisphenol A, aniline and paraformaldehyde, and the single benzoxazine containing DOPO based on bisphenol A(DBDO)was synthesized from DBOZ and DOPO. FT-IR, NMR (1H NMR and 13CNMR) were used to characterize the chemical structure of DBOZ and DBDO. Curing characteristics were studied with DSC and thermostability was studied with TG. In N2 atmosphere, the ring opening polymerization of DBOZ took place at about 205℃, and initial decomposition temperature was 312℃. At 373℃, the fastest decomposition was achieved. At 800℃, carbon residue was 37.19%. In N2 atmosphere, initial decomposition temperature of DBDO was 353℃. At 443℃, the fastest decomposition was achieved. At 800℃, carbon residue was 39.60%.

Key words: synthesis, polymerization, thermostability, NMR, double benzoxazine based on bisphenol A, single benzoxazine containing DOPO based on bisphenol A

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