化工进展

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新型含磷阻燃环氧树脂的合成与表征

夏新年;张小华;陈义红;熊远钦;徐伟箭   

  1. 湖南大学化学化工学院
  • 出版日期:2007-01-25 发布日期:2007-01-25

Synthesis and characterization of phosphorus- containing
epoxy resin for flame retardance

XIA Xinnian;ZHANG Xiaohua;CHEN Yihong;XIONG Yuanqin;XU Weijian   

  1. Department of Chemical and Engineering,Hunan University
  • Online:2007-01-25 Published:2007-01-25

摘要: 以2-(5,5-二甲基-4-苯基-2-氧代-1,3,2-二氧磷杂环已烷膦酸酯基)-对苯二酚和双酚A 二缩水甘油酯合成了一新型的含环状膦酸酯结构的阻燃环氧树脂(DPODB-EP)。采用元素分析、红外光谱(FTIR)和凝胶渗透色谱(GPC)对该含磷环氧树脂的结构和相对分子质量分布进行了表征。采用示差扫描量热法(DSC))和热失重法(TG)对DPODB-EP/PN固化物热性能进行了测试,发现该固化物具有较高的玻璃化转变温度(165℃)和较高的燃烧残炭率(700℃,31%)。阻燃性能测试表明该固化物具有较好的阻燃效果,在磷的质量分数为2.25%时其极限氧指数可达29.5%。

Abstract: A novel phosphorus-containing epoxy resin with good solubility and high thermal stability was obtained via the reaction of diglycidyl ether of bisphenol A with 2-(5,5-dimethyl-4-phenyl-2-oxy- 1,3,2-dioxa- phosphorin-6-yl)1,4-benzenediol, and its structure and relative molecular weight distrubutuin were characterized with elemental analysis, FTIR and gel permeation chromatography (GPC). A phenol formaldehyde novolac resin (PN) was used as curing agent to prepare a thermoset resin with the phosphorus-containing epoxy resin. The thermal properties and thermal degradation behavior of the thermoset resin was investigated by using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Phosphorus-containing cured resin exhibited higher glass transition temperature (165℃) than the ordinary disphenol-A epoxy resins (129℃) due to the high rigidity of its molecular chain. TGA studies showed high residue (700℃ 31%) of the PN-cured epoxy resin due to the presence of phosphorous in the main chain. A sample containing 2.25% (mass ratio) phosphorus had limiting oxygen index values of 29.5. The developed resin may be used potentially in electronic industries.

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