含三苯基氧磷结构聚芳醚醚酮酮的合成与表征

doi:10.11944/j.issn.1000-0518.2018.11.170409

摘要/Abstract

摘要：

以苯酚、对二溴苯及苯基磷酰二氯为原料合成出二(4-苯氧基苯基)苯基氧磷(BPOPPO)。三氯化铝(AlCl₃)为催化剂,通过缩聚反应,BPOPPO与对苯二甲酰氯(TPC)反应制备出一种含有三苯基氧磷结构的聚醚醚酮酮(P-PEEKK)树脂。采用傅里叶变换红外光谱仪(FT-IR)、差示扫描量热仪(DSC)、热重分析仪(TGA)和广角X射线衍射(WAXD)等技术手段对P-PEEKK树脂的结构和性能进行表征。结果表明,P-PEEKK树脂属于非晶聚合物,玻璃化转变温度(T_g)较高,为190.5 ℃;热分解温度(T_5%)为515 ℃,耐热性能较好;极限氧指数(LOI)为42,阻燃性能好,为难燃材料;易溶解于氯仿、1,2-二氯乙烷、N,N-二甲基乙酰胺等有机溶剂中,溶解性能较好,便于涂膜加工;拉伸强度为62 MPa,力学性能较好。

关键词: 二(苯氧基苯基)苯基氧磷, 对苯二甲酰氯, 聚芳醚醚酮酮

Abstract:

A kind of poly(aryl ether ether ketone ketone) containing phenyl phosphine oxide structure(P-PEEKK) was synthesized by polycondensation of bis(4-phenoxy phenyl) phenyl phosphine oxide(BPOPPO) synthesized from phenol, 1,4-dibromobenzene and phenylphosphonic dichloride as raw materials and terephthaloyl chloride(TPC) with aluminum chloride(AlCl₃) as the catalyst. The structure and properties of P-PEEKK resin were characterized by Fourier transform infrared spectroscopy(FT-IR), differential scanning calorimetry(DSC), thermogravimetric analyzer(TGA) and wide-angle X-ray diffraction(WAXD), etc. The results show that P-PEEKK resin is amorphous with a high glass transition temperature(T_g) of 190.5 ℃, a thermal decomposition temperature(T_5%) of 515 ℃ , limiting oxygen index(LOI) of 42 and tensile strength of 62 MPa, and is soluble in chloroform, 1,2-dichloroethane, N,N-dimethylacetamide and other organic solvents for coating film.

Key words: bis(phenoxy phenyl) phenyl phosphine oxide, terephthaloyl chloride, poly(aryl ether ether ketone ketone)

刘勇军,钟鸣,宋琤,盛寿日,侯豪情,宋才生. 含三苯基氧磷结构聚芳醚醚酮酮的合成与表征[J]. 应用化学, 2018, 35(11): 1289-1294.

LIU Yongjun,ZHONG Ming,SONG Cheng,SHENG Shouri,HOU Haoqing,SONG Caisheng. Synthesis and Characterization of Poly(aryl ether ether ketone ketone) Containing Phenyl Phosphine Oxide[J]. Chinese Journal of Applied Chemistry, 2018, 35(11): 1289-1294.

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