采用二氯二苯基硅烷、硼酸、苯乙炔及正丁基锂为原料,氯铂酸催化法合成了三(二苯基苯乙炔硅氧)-硼烷(TSOB),采用红外光谱法对分子结构进行了表征;用差示扫描量热法和红外光谱对树脂固化反应进行了研究,其固化反应主要为苯乙炔基之间的Diels-Alder反应,生成了芳香稠环结构,赋予固化物高的热稳定性;采用热失重法对固化物耐热性能进行研究,结果表明,氮气和空气中Td10(质量损失10%的温度)分别为502℃和554℃,900℃的质量保留率分别为71%和31%。
Tri[diphenylphenylethynylsilyl-oxide]-borane(TSOB) was prepared based on dichlorodiphenylsilane,boric acid,phenylacetylene and n-butyllithium,catalyzed by chloroplatinic acid.The resulting product was characterized by FT-IR.Differential scanning calorimetry and FT-IR were used to study the curing mechanisms.The phenylethynyl groups underwent Diels-Alder reaction to form polycyclic aromatic hydrocarbon structures,which took benefit of high thermal stability for the thermoset.Thermogravimetric analysis was performed to characterize the heat-resistance of TSOB thermoset in nitrogen and air.The results show that Td10(the temperature of 10% mass loss) in nitrogen and in air is 502 ℃ and 554 ℃ respectively,the residue at 900 ℃ in nitrogen and air reaches 71% and 31% respectively.
参考文献
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