含硅磷杂化物环氧树脂固化物性能研究

PROPERTIES OF CURED EPOXY RESIN CONTAINING PHOSPHORUS-AND SILICA-CONTAINING HYBRIDS

首先用γ-环氧丙氧基三甲氧基硅烷(KH-560)和亚磷酸二乙酯(DEP)反应的中间产物进行水解缩合反应,合成了一种含磷低聚硅氧烷杂化物.并用FTIR,NMR,GPC对其结构及分子量进行了表征.然后将含磷低聚硅氧烷引入到双酚A环氧树脂(E-54)制备硅磷杂化物环氧树脂的固化物.对这种含硅磷杂化物环氧树脂固化物的性能研究发现其极限氧指数为23～29,DSC分析结果玻璃化转变温度(Tg)可以达到204℃,失重5%的温度(Td)5%比纯E-54提高近20℃.该固化物具有阻燃性能,同时具有较好的热性能。

A series of phosphorus-and silica-containing hybrids（DPS） with different molecular weight was synthesized by hydrolysis condensation of intermediate products and various amounts of water.The intermediate was formed by the reaction between 3-glycidyloxypropyltrimethaxysilane（KH-560） and diethyl phosphate（DEP） in different weight ratios.The structure of DPS was determined by Fourier transform infrared（FTIR）,nuclear magnetic spectrum（NMR） and element analysis,while molecular weight and distribution of DPS were measured by gel permeation chromatography（GPC）.Then,a cured epoxy resin containing phosphorus-and silica-containing hybrid was prepared by the in situ curing of the bisphenon A type epoxy resin and 4,4＇diaminodiphenylmethane with the phosphorus-and silica-containing hybrid.The flame retardation was investigated by the limited oxygen index（LOI）,and the thermal properties of the cured epoxy resin were characterized by differential scanning calorimetry（DSC） and thermogravimetric analysis（TGA）.Studies on the characteristics of cured epoxy resin containing a phosphorus-and silica-containing hybrid showed that the flame retardant and the thermal properties were enhanced.The flame resistance was indicated by the limited oxygen index in the ranges of 23 ～ 29,which was higher than that of the pure epoxy resin（22）.The glass translation temperature for E54-Si-3H-20 sample was 204℃ and the temperature of 5% weight loss was about 20℃ higher than that of the pure epoxy resins.Compared to the pure epoxy resin,not only the flame resistance of the cured epoxy resin containing phosphorus-,silica-containing hybrid was enhanced,but also the thermal properties were improved.