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作 者:黄超群[1] 徐少轶[1] 赵京波[1] 江盛玲[1] 杨万泰[1]
机构地区:[1]北京化工大学化工资源有效利用国家重点实验室材料科学与工程学院,北京100029
出 处:《高分子学报》2010年第5期574-581,共8页Acta Polymerica Sinica
基 金:国家自然科学基金项目(基金号50873013);教育部创新团队项目(项目号IRT0706);北京市教委高分子化学与物理重点学科共建项目(项目号XK100100540;XK100100640)资助
摘 要:利用脂肪族二元酸酯与乙醇胺反应容易获得的对称二酰胺二醇,经缩聚合成聚酯酰胺预聚体,并针对端羧基和端羟基同时扩链来提高分子量,获得可生物降解的聚酯酰胺.首先将N,N′-二(2-羟乙基)草酰胺(HEOA)或N,N′-二(2-羟乙基)己二酰胺(HEHA)与己二酸和丁二醇缩聚,制备同时带有端羧基及端羟基的脂肪族聚酯酰胺预聚体,通过1,4-双(2-噁唑啉)苯及己二酰双己内酰胺混合扩链剂扩链,获得高分子量脂肪族聚酯酰胺,并通过红外、1H-NMR、DSC及TGA对其结构和热性能进行了表征.结果表明,预聚体在制备过程发生了一定的酯-酰胺交换反应;扩链后聚合物的熔点、熔融焓和热稳定性有所下降;但热稳定性仍接近或略高于聚己二酸丁二酯.Polyesteramide (PEA(n,x /y))prepolymers with Mn from 4400 to 6400 were synthesized through melt polycondensation from adipic,butanediol and N,N'-bis(2-hydroxyethyl) oxalamide (0) or N,N'-bis(2-hydroxyethyl) adipamide ( 4 ) at different butanediol ( x) to bisamidediol ( y ) molar ratios. Chain extension reaction was performed with 2,2'-(1,4-phenylene)-bis(2-oxazoline) ( PBOX) and adipoyl biscaprolactamate (ABC)as combined chain extenders. High molecular weight PEA(n,x/y) with Mn up to 22500 and Mw up to 53100 was prepared. The PEA(n,x /y) prepolymers and the chain extended PEA(n,x /y) were characterized by FTIR and 1H-NMR spectroscopy,differential scanning calorimetry( DSC),and thermogravimetric analysis (TGA). 1H-NMR spectra revealed that during the preparation of the PEA(n,x/y) prepolymers,some esteramide exchange side reaction took place. DSC studies indicated that after chain extension the Tm and ΔHm of the polyesteramides decreased. TGA studies showed that after the chain extension,the thermal stability of the PEA(n,x /y)s slightly decreased,but still a little higher than that of poly(butylene adipate).
关 键 词:脂肪族聚酯酰胺 扩链反应 缩聚 N N′-二(2-羟乙基)草酰胺 N N′-二(2-羟乙基)己二酰胺 己二酸
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