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作 者:宋琤[1] 余雯雯[2] 钟鸣[2] 祝志芳[2] 易志群[2] 宋才生[1,2]
机构地区:[1]南昌航空大学材料科学与工程学院,南昌330063 [2]江西师范大学化学化工学院,南昌330022
出 处:《高分子学报》2011年第1期70-75,共6页Acta Polymerica Sinica
基 金:江西省自然科学基金(基金号2007GZW0175);科技型中小企业技术创新基金(基金号06C26213601342);江西师范大学研究生创新基金(基金号JXSD-Y-09084)资助项目
摘 要:以偏苯三甲酸酐酰氯(TMAc),对苯二甲酰氯(TPC),1,4-二(4-苯氧基苯甲酰基)苯(p-EKKE)为单体,采用亲电溶液共缩聚,通过改变TMAc、TPC的摩尔比,制备了系列含羧基侧基的聚芳醚酮树脂(PEK-A).在对甲苯磺酸催化下与苯酚进行酯化反应合成了系列主链带芳酯侧基的聚芳醚酮树脂(PEK-COO-Ar).用红外光谱(FTIR),广角X射线衍射(WAXD),热失重(TGA),示差量热扫描(DSC)等技术对聚合物的结构和性能进行表征,考察了聚合物的溶解性能.结果表明,随着主链中芳酯侧基比例的增加,聚合物的Tg提高(195~219℃),而Tm降低.当TPC/TMAc摩尔比小于1∶1时,树脂呈非晶态结构.当TPC/TMAc摩尔比为50/50和60/40时,树脂经等温结晶后,具有优良的机械力学性能.A series of novel poly(aryl ether ketone) s containing pendant aryl ester groups(PEK-COO-Ar) were prepared from poly(aryl ether ketone)s containing pendant carboxyl acid groups(PEK-A) and phenol in the presence of 1,1,2,2-tetrachloroethane and by using p-toluenesulfonic acid as a catalyst.The PEK-A was synthesized from trimellitic anhydride chloride(TMAc),terephthaloyl chloride(TPC) and 1,4-bis(4-phenoxybenzoyl)benzene(p-EKKE) by low temperature solution poly-condensation.By changing the molar ratio of TMAc and TPC a series of PEK-A polymers were prepared.The PEK-COO-Ars were characterized by Fourier transform infrared spectroscopy(FTIR),wide-angle X-ray diffraction(WAXD),thermal gravimetric analysis(TGA) and differential scanning calorimetry(DSC).The results showed that the glass transition temperature(Tg) of the PEK-COO-Ar was in the range of 195 ~ 219℃ and the decomposition temperature(Td) at 5% weight loss was from 416℃ to 447℃ and the melting temperature(Tm) was between 325℃ and 345℃.The Tg of the PEK-COO-Ar increased by increasing the mole ratio of aryl ester groups in the polymer,while the Td deceased.The polymers were readily soluble in N-methly-2-pyrrodine,chloroacetic acid and concentrated sulfuric acid at room temperature.They were swelling or soluble in the strong polar aprotic solvent such as N,N-dimethylformamide(DMF),N,N-dimethylacetamide(DMAc) and dimethyl sulfoxide(DMSO) by heating.The polymers converted to amorphous when the molar ratio of TPC to TMAc was less than 1.The polymers had good mechanical properties after being isothermally crystallization.The tensile strength,elongation at break and elastic modulus of S2’(TPC/TMAc = 60/40) and S3’(TPC/TMAc = 50/50) were 112.1 MPa,27%,2.9 GPa and 130.3 MPa,24.2%,2.4 GPa,respectively.
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