合成了9,9’-二（3-苯基-2,4-二氢-1,3-苯并噁嗪）芴（简称BFA）、9,9’-二（3-烯丙基-2,4-二氢-1,3-苯并噁嗪）芴（BFB）和大分子苯并噁嗪单体（BFC）。分别用核磁共振仪（1H-NMR）和红外光谱仪（FT-IR）对它们的结构进行了鉴定。差示扫描量热（DSC）对三种芴基苯并噁嗪的固化反应研究结果表明,它们的固化反应发生在180℃～280℃之间。三种单体的固化物都表现出很高的玻璃化转变温度,其中BFB的固化物的玻璃化温度已经超过300℃,BFA和BFC的玻璃化温度也分别达到202℃和263℃。它们在N2氛围中5%分解温度分别达到325℃、331℃和359℃,体现出较好的热稳定性。
Three difunctioned fluorene-based benzoxazine monomers（BFA,BFB and BFC） were synthesized via Mannich condensation among 9,9′-bis-（4-hydroxyphenyl）-fluorene,paraformaldehyde and primary amines including aniline,allylanline and 4,4′-diaminodiphenylmethane.Their chemical structures were confirmed by 1H nuclear magnetic resonance spectroscopy（NMR） and Fourier transform infrared spectroscopy（FT-IR）.The curing reactions of benzoxazine monomer were investigated under nonisothermal differential scanning calorimetry（DSC） and the results show that the polymerization temperature of three fluorene-based benzoxazines is mainly at 180 ℃～280 ℃.Thermal properties of three fluorene-based polybenzoxazine were studied by thermogravimetric analysis（TGA） and DSC,and results indicate that thermal stability of polybenzoxazine is notable improved with introducing fluorene moiety into its skeleton.The glass transition temperature（Tg） of the cured of three monomers is 202（BFA）,263（BFC） and above 300 ℃（BFB）,respectively.The 5% weight loss temperature of three corresponding polybenzoxazines in N2 atmosphere is 331 ℃,325 ℃ and 359 ℃,respectively.
参考文献
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