应用化学 ›› 2010, Vol. 27 ›› Issue (04): 404-408.DOI: 10.3724/SP.J.1095.2010.90390

• 研究论文 • 上一篇    下一篇

六苯氧基环三磷腈的合成及其在层压板中的阻燃应用

唐安斌*,黄杰,邵亚婷,刘锋   

  1. (四川东材科技股份有限公司,国家绝缘材料工程技术中心 绵阳 621000)
  • 收稿日期:2009-06-09 修回日期:2009-08-18 出版日期:2010-04-10 发布日期:2010-04-10
  • 通讯作者: 唐安斌,男,博士,研究员; E-mail:scdctab@163.com; 研究方向:新型绝缘和阻燃材料
  • 作者简介:唐安斌,男,博士,研究员;E-mail:scdctab@163.com;研究方向:新型绝缘和阻燃材料
  • 基金资助:
    “十一五”国家科技支撑计划项目(2007BAE50B03);四川省青年科技基金项目(08JJ0100)

Synthesis of Hexaphenoxycyclotriphosphazene and Its Application in Laminate

TANG An-Bin*, HUANG Jie, SHAO Ya-Ting, LIU Feng   

  1. (Sichuan EM Technology Co.,Ltd.  National Insulating Material Engineering Research Center,Mianyang 621000)
  • Received:2009-06-09 Revised:2009-08-18 Published:2010-04-10 Online:2010-04-10
  • Supported by:

    National Technology R&D Program in the 11th Five year Plan of china;Science and Technological Fund of Sichuan Province for Outstanding Youth

摘要:

以六氯环三磷腈(HCCTP)粗产物、苯酚、NaOH为反应原料,四丁基氯化铵(TBAC)为相转移催化剂,氯苯和水为溶剂,合成了六苯氧基环三磷腈(HPCTP),考察了反应温度、反应时间、反应溶剂、物料配比对收率的影响。结果表明,在最佳原料配比n(NaOH): n(苯酚): n(TBAC): n(HCCTP粗产物)=7.5: 6.3: 0.15: 1,30 ℃反应4 h,回流反应6 h,HPCTP的收率达到75%。采用红外光谱、核磁氢谱、碳谱、磷谱、X射线衍射分析、示差扫描量热分析、热重分析测试技术对产物进行了表征分析,并首次用于苯并噁嗪树脂玻璃布层压板,当HPCTP的质量分数为10%时,燃烧等级达到V-0级,平行击穿电压为47 kV,热态弯曲强度为596 MPa。

关键词: 六苯氧基环三磷腈, 阻燃剂, 层压板, 合成, 应用

Abstract:

Hexaphenoxycyclotriphosphazene(HPCTP)was synthesized by the reaction of crude hexachlorocyclotriphosphazene(HCCTP) with phenol and sodium hydroxide,with tetrabutylammonium chloride(TBAC) as phase transfer catalyst and chlorobenzene/water as solvent. Effects of reaction temperature, reaction time, solvent and molar ratio of raw materials on the yield of HPCTP were investigated. Under the optimized reaction conditions of n(sodium hydroxide)∶n(phenol)∶n(TBAC)∶n(crude HCCTP)=7.5∶6.3∶0.15∶1, reaction time of 4 h at 30 ℃ plus 6 h at reflux temperature, the yield was 75%. The product was characterized by FTIR, 1H NMR, 13C NMR, 31P NMR, XRD, DSC and TGA. The product has been firstly applied in benzoxazine resin glass cloth laminate. The flammability class of the laminate was in the rank of V-0, the breakdown voltage of the laminate was 47 kV, and the thermal state flexural strength of the laminate was 596 MPa when the mass fraction of HPTCP in the laminate was 10%.

Key words: hexaphenoxycyclotriphosphazene, flame retardant, laminate, synthesis;application

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