一种含氟和吡啶结构的双酚及其可溶性聚醚醚酮的合成与表征

A Soluble Poly(Aryl Ether Ether Ketone) Based on a New Bisphenol Containing Fluorine and Pyridine Groups

以4-三氟甲基苯甲醛、4'-羟基苯乙酮为主要原料,通过改进的Chichibabin反应合成了一种新型的双酚单体——4-(4-三氟甲基苯基)-2,6-二(4-羟基苯基)吡啶,继而将其与4,4'-二氟二苯酮进行缩聚反应,合成了一种主链含氟和2,6-二苯基吡啶结构的聚醚醚酮,并以FTIR、DSC、WAXD等对其结构和性能进行了表征.研究结果表明:聚合物的对数比浓黏度为0.65 dL·g-1,耐热性优异,所得聚醚醚酮玻璃化转变温度(T g)为178℃,在空气中,5%的热失重温度为556℃,拉伸强度为99.5 MPa,杨氏膜量为3.01 GPa,断裂伸长率为14%.同时,该聚合物为无定形结构,在常温下可溶于N-甲基吡咯烷酮、N,N-二甲基乙酰胺、四氢呋喃和氯仿等有机溶剂中,介电常数为2.62(1 MHz),吸水率为0.46%.

A new bisphenol monomer, 4-（ 4-trifluoromethylphenyl ） -2,6-bis （ 4-hydrophenyl ） pyridine was synthe- sized by a modified Chichibabin reaction using 4-trifluoromethylbenzaldehyde and 4＇-hydroacetophenone as main original materials, which was then employed to prepare a new poly （ aryl ether ether ketone） （PEKK） containing fluo- rine and 2,6-diphenylpyridine groups via aromatic nucleophilic substitution polycondensation with 4,4＇-difluoro- benzophenone,and their structure and properties were studied using analysis techniques such as FTIR, DSC and WAXD. The results indicated the resulting PEKK with inherent viscosities of 0.65 dL · g^-1 had excellent heat re- sistance with glass transition temperature of 178 ℃ ,5% weight loss decomposition temperature of 556 ℃ in air. In the meantime, the new fluorinated PEKK showed a 99.5 MPa tensile strengh,3.01 GPa Young＇ s modulus and 14% elongations at break. Besides,this new PEEK with lower dielectric constant of 2.62（ 100 MHz）and low water ab- sorption 0.46% was amorphous and was soluble in dipolar aprotic solvents such as N-methyl-2-pyrrolidone and N, N-dimethylacetamide, and some common organic solvents like chloroform and THF at room temperature.