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含磷固化剂及固化环氧树脂的合成及表征 被引量:15

Synthesis and Characterization of Phosphorus-Containing Curing Agent and Cured Epoxy Resins
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摘要 以4,4′-二氨基二苯基甲烷(DDM)、苯甲醛和亚磷酸二乙酯为原料,合成了两种含磷固化剂PM1和PM2,用红外光谱、核磁共振氢谱对PM1和PM2的结构进行了表征。用DDM,PM1,PM2分别固化双酚A型(DGEBA)环氧树脂,得到DGEBA-DDM,DGEBA-PM1,DGEBA-PM2树脂,采用示差扫描量热法、热重分析(TGA)和极限氧指数(LO I)对DGEBA-DDM,DGEBA-PM1,DGEBA-PM2树脂的玻璃化转变温度(Tg)、反应活性、热稳定性和阻燃性能进行了表征。实验结果表明,PM2的反应活性比PM1低;DGEBA-DDM,DGEBA-PM1,DGEBA-PM2树脂的Tg分别为178,112,145℃;TGA结果表明,700℃时DGEBA-PM1和DGEBA-PM2树脂的成炭率分别为29%和35%,而700℃时DGEBA-DDM树脂的成炭率只有19%;DGEBA-PM1和DGEBA-PM2树脂的LO I值由DGEBA-DDM树脂的24%分别增至30%和35%,且阻燃性能大幅度提高。 Phosphorus-containing curing agents ( PM1 and PM2 ) for epoxy resins were synthesized from 4,4'-diamino-diphenyl-methane ( DDM ), benzaldehyde and diethyl phosphite. Their structures were characterized by means of IR and ^1H NMR. Diglycidyl ether of bisphenol A resin (DGEBA) was cured by using PM1, PM2 and DDM. DGEBA-PM1, DGEBA-PM2 and DGEBA-DDM resins were obtained. Glass transition temperature ( Tg ), reactivity, thermal stability and fire resistance properties of resins were investigated by means of DSC, thermogravimetric analysis (TGA)and limiting oxygen index (LOI) analysis. As curing agent, PM1 is more reactive than PM2. Tg values of DGEBA-PM1 and DGEBA-PM2 are 112℃ and 145℃, respectively, lower than that of DGEBA-DDM. TGA reveals that char yields of DGEBA-PM1 and DGEBA-PM2 resins are 29% and 35% at 700℃ respectively ,whereas DGEBA-DDM resin is 19% at same temperature. LOI values of DGEBA-PM1 and DGEBA-PM2 resins are 30% and 35% ,respectively. The high char yield and LOI indicate that inflaming-retardance of resins is greatly improved.
出处 《石油化工》 EI CAS CSCD 北大核心 2006年第8期774-777,共4页 Petrochemical Technology
关键词 4 4’-二氨基二苯基甲烷 环氧树脂 阻燃 固化剂 4,4'-diamino-diphenyl-methane epoxy resin phosphorus inflaming-retarding curing agent
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