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呋喃基磷杂菲阻燃剂的合成及在阻燃环氧树脂中的应用

Synthesis of Furan-based Phosphaphenanthrene Flame Retardant and Its Application in Anti-flammable Epoxy Thermosets

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【作者】 唐刚陶熠邓丹张冬欣张诗华刘秀玉伍强沈海峰孙俊杰

【Author】 TANG Gang;TAO Yi;DENG Dan;ZHANG Dongxin;ZHANG Shihua;LIU Xiuyu;WU Qiang;SHEN Haifeng;SUN Junjie;School of Architecture and Civil Engineering, Anhui University of Technology;Department of Polymer Science and Engineering, Jiaxing University;Institute of Molecular Engineering and Applied Chemistry,Anhui University of Technology;

【通讯作者】 刘秀玉;

【机构】 安徽工业大学建筑工程学院嘉兴学院高分子材料与工程系安徽工业大学分子工程与应用化学研究所

【摘要】 以5-羟甲基糠醛、糠胺、三氯氧磷和9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)为原料合成了一种呋喃基磷杂菲阻燃剂(Furan-2DOPO),并利用傅里叶变换红外光谱(FTIR)、核磁共振波谱(1H NMR和31P NMR)对其结构进行了表征.进一步利用Furan-2DOPO对环氧树脂进行阻燃改性,得到一系列阻燃环氧固化物.考察了Furan-2DOPO的用量对阻燃环氧固化物的力学性能、热稳定性以及阻燃性能的影响.研究结果表明,当Furan-2DOPO的添加量(质量分数)仅为5%时(磷质量分数为0.47%),环氧固化物的氧指数达到31.0%,且能够通过UL-94垂直燃烧V-0级测试.与未改性环氧树脂相比,添加2.5%和5%Furan-2DOPO的环氧固化物的最大热释放速率分别下降了31%和35%.此外,2种添加Furan-2DOPO的环氧固化物的拉伸强度均比未改性环氧树脂提升了约28%.炭层分析结果表明,Furan-2DOPO具有良好的催化成炭性能,有利于减少燃烧过程中可燃性气体的逸出,从而提升阻燃性能.

【Abstract】 A novel bio-based flame retardant(Furan-2DOPO) was synthesized from 5-hydroxymethylfurfural,furfuramine,phosphorus oxychloride and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide(DOPO).Its structure was characterized by Fourier transform infrared spectroscopy,proton-and phosphorus-nuclear magnetic resonance spectroscopy.A series of cured flame retarded epoxy products was obtained by modification of epoxy resin with Furan-2DOPO.The effects of the loading of Furan-2DOPO on the mechanical properties,thermal stability and flame retardant properties of the cured epoxy products were investigated.The results showed that when the addition amount of Furan-2DOPO was only 5%(mass fraction,phosphorus mass fraction was 0.47%),the oxygen index of the cured epoxy product reached 31.0%,and can pass the UL-94 V-0 test;compared with the unmodified epoxy resin,the peak heat release rate of the cured epoxy products containing 2.5%(mass fraction) and 5%(mass fraction) Furan-2DOPO was decreased by 31%and 35%,respectively.In addition,the tensile strength of the cured epoxy products containing 2.5%and 5%Furan-2DOPO was about 28%higher than that of the unmodified epoxy resin,respectively.The results of char analysis indicated that Furan-2DOPO possessed excellent catalytic charring performance,which was conducive to reducing the escape of combustible gases during combustion,so as to improve the flame retardant performance.

【基金】 国家自然科学基金(批准号:51403004);安徽省自然科学基金(批准号:2108085ME178,2008085ME176);安徽省科技重大专项(批准号:202203a06020003)资助~~
  • 【文献出处】 高等学校化学学报 ,Chemical Journal of Chinese Universities , 编辑部邮箱 ,2024年04期
  • 【分类号】TQ323.5
  • 【下载频次】117
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