利用DSC法研究了双环笼状取代倍半硅氧烷/环氧树脂的固化过程,根据Kissinger'S方程计算出固化反应表观活化能和表观指前因子分别为52.6kJ·mol-1和1.44×103min-1.利用热重分析和氧指数法研究了材料的热稳定和阻燃性能,磷硅两元素的协同阻燃效应及笼状骨架的共同作用提高了材料的热稳定性和阻燃性,在700℃时成炭量高达24.5%,氧指数为25.通过动态热机械分析仪表征了材料的玻璃化温度和储能模量.双环笼状取代倍半硅氧烷固化环氧树脂具有较好的低温韧性,在14℃时冲击韧度为3.63kJ·m-2,洛氏硬度为76.结果表明双环笼状取代倍半硅氧烷是一种兼具增韧和阻燃性能的多功能环氧树脂固化剂.
The curing system of diglycidyl ether of bisphenol A (DGEBA) with octa (1-oxo-1-phospha-2, 6, 7-trioxabicyclo [2.2.2]-4-methylene) silsesquioxane (OSSQ) was studied by the differential scanning calorimetry (DSC). The activation energy (E.) and the pre-exponential factor (A0) of curing reaction, determined according to the Kissinger's method, were found to be 52.6kJ·mol-1 and 1.44 ×103 min-1. The thermal stability and flame retardancy of DGEBA/OSSQ were evaluated by thermogravimetry analysis (TGA) and Limiting Oxygen Index (LOI). Synergistic effect between phosphorus and silicon combined with the rigid structure of silsesquioxane resulted in good flame retardaney and thermal stability, the charred residue of DGEBA/OSSQ kept as high as 24.5% at the 700℃, the value of LOI was 25. The glass transition temperature (Tg) and storage modulus (E') were measured by dynamical mechanical analysis (DMA). DGEBA/ OSSQ possessed good low temperature toughness, the impact strength was 3.63kJ·m-2 and the Rockwell hardness was 76 at 14℃. Results demonstrate that OSSQ serviced as a multifunctional curing agent of epoxy resin with the properties of toughening and flame retarding.
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