芴基苯并噁嗪单体的合成及热性能研究

Synthesis and Thermal Properties of a Fluorene-containing Benzoxazine

以双酚芴、环己胺和甲醛为原料,采用混合溶剂法合成了一种新型双官能度芴基苯并噁嗪单体,利用FTIR,1H NMR和13C NMR对产物结构进行了表征,以差式扫描量热仪(DSC)研究了芴基苯并噁嗪单体的固化行为,通过DSC和热重(TGA)分析了聚苯并噁嗪的热性能.结果表明,芴基聚苯并噁嗪树脂呈现出典型的热开环固化特征,放热峰顶温度为251℃,玻璃化转变温度Tg为189.4℃,初始热分解温度(热失重5%)达329℃,800℃时的残碳率达到31%.

A new difunctional fluorene-based benzoxazine monomer was synthesized through the reaction of 9,9-bis-（4-hydroxyphenyl）-fluorene with formaldehyde and cyclohexylamine.The chemical structure was confirmed through FTIR,1H NMR and 13C NMR analyses.The polymerization reaction of the precursor was monitored with Differential Scanning Calorimetry（DSC） and FTIR.The thermal properties of cured polymers were evaluated through DSC and Thermo Gravimetric Analysis（TGA）.The fluorene-based polybenzoxazine showed that the typical curing characteristic of the oxazine ring-opening for difunctional benzoxazine centred at 251 ℃,with remarkably higher glass transition temperature（189.4 ℃） and better thermal stability than traditional biphenol A polybenzoxazines.The thermal decomposition temperature（5% weight loss） and the char yield of fluorene based polybenzoxazine at 800 ℃ is 329 ℃ and 31%,respectively.