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以联苯二甲酸二甲酯、二甘醇和9,10-二氢-9-氧杂-10磷酰杂菲-对苯二酚二羟乙基醚(DOPO-HQ-HE)为单体,通过无规共聚合成了一种新型含磷液晶共聚酯(PDEBP).用1H-NMR对共聚酯的结构进行了表征,用TGA、DSC和POM对其热性能及液晶行为进行了研究.结果表明,阻燃单体DOPO-HQ-HE的引入不会降低共聚酯的热稳定性,含7.5 mol%DOPO-HQ-HE的共聚酯PDEBP7.5在700℃的氮气氛中的残余物(Wt7R00)可达31.9 wt%,并且具有很好的阻燃性.DOPO-HQ-HE含量的增加对共聚酯的结晶性有较大的破坏,5 mol%DOPO-HQ-HE的共聚酯PDEBP5的清亮点温度为154.2℃,焓变为4.64 J/g,而PDEBP7.5在POM测试中在升温及降温过程中均难观察到液晶相的双折射现象.
In this study, dimethyl diphenyldicarboxylate, diethylene glycol and 9,10-dihydro-9-oxa-10-phosphorylphenyldihydroxyethyl ether (DOPO-HQ-HE) A novel phosphorus-containing liquid crystal copolyester (PDEBP) was synthesized by random copolymerization.The structure of the copolyester was characterized by1H-NMR and its thermal properties and liquid crystal behavior were studied by TGA, DSC and POM. The results showed that the introduction of the flame retardant monomer DOPO-HQ-HE did not reduce the thermal stability of the copolyester. The copolyester PDEBP7.5 with 7.5 mol% DOPO-HQ-HE remained in nitrogen atmosphere at 700 ℃ (Wt7R00) up to 31.9 wt%, and has good flame retardancy.The increase of DOPO-HQ-HE content has a great impact on the crystallinity of the copolyester, 5 mol% DOPO-HQ-HE Polyester PDEBP5 has a clearing point temperature of 154.2 ° C and an enthalpy of 4.64 J / g. PDEBP7.5 is hard to observe the birefringence of the liquid crystal phase during the POM test during heating and cooling.