【作者】 贺征华；

【导师】 唐旭东；

【作者基本信息】 天津科技大学 ， 材料加工工程， 2006， 硕士

【摘要】 本文首先合成了一种侧链含磷单体9，10-二氢-9-氧杂-10-磷酰杂菲-对苯二酚(DOPO-HQ)，对其合成方法进行了改进，通过红外光谱、核磁共振和DSC对其结构进行了表征；然后合成了一种新型的主链含磷单体1，4-双(对氟苯酰基苯基)苯基氧化膦(FPPPO)，并通过红外光谱、核磁共振、元素分析以及DSC等手段，对其结构进行了表征。 采用高温溶液缩聚反应，分别以4，4’-二氟二苯甲酮(DFK)或1，4-双(对氟苯甲酰基)苯(1，4-FBB)、双酚S和DOPO-HQ为共聚单体，通过改变双酚S与DOPO-HQ在体系中的配比，制备了两个系列的侧链含磷双酚S型聚芳醚酮。研究了合成条件，如反应温度、反应时间、反应浓度等因素对聚芳醚酮特性粘度的影响，用红外光谱、核磁共振对聚合物进行了结构分析，用DSC测定了聚合物的玻璃化转变温度，用TGA进行了热失重分析，测定聚合物在有机溶剂中的溶解性。结果发现，将侧链含磷单体DOPO-HQ引入聚芳醚酮主链结构中，提高了聚芳醚酮玻璃化温度，提高了其热稳定性，并改善了其在有机溶剂中的溶解性。 通过高温溶液缩聚反应，将主链含磷单体FPPPO与双酚S反应合成了主链含磷双酚S型聚芳醚酮。测定了聚合物的特性粘度，用红外光谱，核磁共振对聚合物进行了结构分析，用DSC测定了聚合物的玻璃化转变温度为235℃，使用TGA对聚合物进行了热失重分析，测试了聚合物在有机溶剂中的溶解性，另外还对聚合物进行了成膜性测试，发现具有良好的成膜性，对聚合物膜进行了一系列的性能测试，包括力学性能测试、电性能测试、氧指数测试(氧指数为45)，结果表明在主链上引入磷元素可以提高聚芳醚酮的玻璃化转变温度，改善了它的溶解性和阻燃性能，并赋予其良好的力学性能和热稳定性。更多还原

【Abstract】 2-（6-oxide-6H-dibenz<c, e><1, 2> oxa phosphorin-6-yl）-1,4-dihydroxy- phenylene （DOPO-HQ） which has P in its side chain was synthesized at first. We amended its synthesis ways, and the structure of the DOPO-HQ was characterized by FT-IR, ¹H-NMR and DSC, and then bis （4-chloroformyl） phenylphosphine oxide （FPPPO） which has P in its main chain was also synthesized and characterized by FT-IR, ¹H-NMR, ³¹P-NMR, element analysis and DSC.Two series of phosphorus-containing PAEKs with biphenyl-S moiety were synthesized by high-temperature solution polycondensation, which 1, 4-bis （4-fluoro-benzoyl） benzene （1, 4-FBB） or 4, 4’-diflourodiphenylketone （DFK）, DOPO-HQ, biphenol-S were used as monomer. The influences of reaction conditions such as reaction temperature, reaction time, and concentration of reactants on polymerization were studied. The PAEKs were characterized by FT-IR, ¹H-NMR and DSC, the thermal stabilities of PAEKs were measured by TGA. The solvencies of phosphorus-containing PAEKs were measured also. The results indicate that introducing DOPO-HQ into PAEKs’ structure can increase its Tg and thermal stability and improve its solvencies in organic solvent.A novel phosphorus-containing-in-main-chain PAEK with biphenyl-S moiety （PEEKKS-MP） was synthesized by FPPPO and bisphenol-S through high-temperature solution polycondensation. The structure and properties of the PEEKKS-MP were characterized by FT-IR,¹H-NMR, ³¹P-NMR and DSC and TGA, and the solvency of the PEEKKS-MP was also measured. The results indicate that the Tg of PEEKKS-MP was 235℃, and it can be soluble in most ordinary solvents. The PEEKKS-MP possessed good film ability and the properties of thin film of PEEKKS-MP was tested, such as mechanics property, electrical property and oxygen index, the LOI of PEEKKS-MP was 45, which indicates it possessed excellent flame retardancy.更多还原