新型含磷腈环氧树脂的合成及其阻燃性能  

Synthesis and Flame Retardant Properties of a Novel Cyclotriphosphazene-based Epoxy Resin

作　　者：徐广锐 许苗军[1] 赖涛[1] 李斌[1] 

机构地区：[1]东北林业大学理学院黑龙江省阻燃材料分子设计与制备重点实验室,黑龙江哈尔滨150040

出　　处：《合成化学》2014年第3期331-334,共4页Chinese Journal of Synthetic Chemistry

基　　金：国家自然科学基金资助项目(21174025)

摘　　要：六氯环三磷腈与对羟基苯甲醛经亲核取代反应制得六对醛基苯氧基环三磷腈(HAPCP);HAPCP经高锰酸钾氧化得六对羧基苯氧基环三磷腈(HCPCP);以苄基三乙基氯化铵为催化剂,HCPCP与环氧氯丙烷经开环闭环反应合成了一种新型的含磷环氧树脂(PN-EP),其结构和热稳定性经1H NMR,IR和TGA表征。结果表明,PN-EP的初始分解温度为278℃,在700℃时残炭量为40.5 wt%,具有很好的热稳定性和成炭性能。采用二氨基二苯甲烷对PN-EP进行固化,并通过极限氧指数(LOI)和垂直燃烧(UL-94)对其阻燃性能进行测试。结果表明:PN-EP固化物通过UL-94 V-0级测试,氧指数33%。Hexa-（4-aldehyde-phenoxy）-cyclotriphosphazene （HAPCP） was obtained by nucleophilic substitution reaction of hexachlorocyclotriphosphazene with p-hydroxybenzaldehyde.Hexa-（4-carboxyl-phenoxy）-cyclotriphosphazene （HCPCP） was synthesized by oxidation reaction of HAPCP with KMnO4.A novel phosphorus-containing flame retardant epoxy resin（PN-EP） based on cyclotriphosphazene was successfully synthesized by ring opening and closing reaction of HCPCP with epichlorohydrin using benzyltriethylammonium chloride as the catalyst.The structure and thermal stability were characterized by 1H NMR,IR and TGA.PN-EP was cured by diaminodiphenyl methane and the flame retardant properties of the thermoset were investigated through limiting oxygen index （LOI） and vertical burning test （UL-94）.The results showed that the initial thermal decomposition temperature of PN-EP was 278 ℃ and the char residue remained 40.5 wt% at 700 ℃ and PN-EP had a high thermal stability and charting forming ability.The cured sample can successfully pass UL-94 V-0 rating with the LOI value of 33%.

关 键 词：六氯环三磷腈 含磷环氧树脂 合成 热稳定性 阻燃性能 

分 类 号：O626.4[理学—有机化学] O625[理学—化学]