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以己二酸、1,4-丁二醇和尿素为原料,在氩气环境下,通过高温熔融缩聚反应合成了一种新型可降解的己二酸-丁二醇-尿素共聚物,并对反应时间、催化剂种类及其用量、原料配比、反应温度等因素对聚合产物的影响进行了研究。采用红外光谱(FT-IR)、核磁共振(1H-NMR)、凝胶渗透色谱(GPC)、热重分析(TG)、差示量热扫描(DSC)对产物的结构与性能进行了表征。结果表明,当丁二醇和尿素的总量与己二酸(n(丁二醇+尿素)∶n(己二酸))的摩尔比为1.16∶1,丁二醇和尿素(n(1,4-丁二醇)∶n(尿素))的摩尔比为5∶1,最高反应温度为220℃,二月桂酸二丁基锡为催化剂且用量为原料总量的0.03%,总反应时间10h,所得到产物的重均分子量(Mw)可达12700,其颜色、热稳定性和降解性能等较好。

A novel adipic acid copolymer was synthesized via condensation polymerization with adipic acid, urea and, 1,4-butanediol as the raw materials. The influences of reaction time, catalyst, mass ratio of raw materials and the temperature on the property of copolymer were investigated. The structure, thermodynamic perform- ance and the molecular weights of the eopolymer were characterized by fourier transform infrared (FT-IR), 1 H- NMR spectrum, gel permeation chromatography (GPG) and thermogravimeter-differential scanning calorimeter (TG-DSC) respectively. The results show that under the condition of 220℃, 10h, the optimal feed molar ratios n (1,4-butanediol and urea)/n (adipic acid) == 1.16 : 1, n (adipie acid)/n (urea) = 5 : 1, the amount of catalyst was 0.03wt %), a desired adipic acid copolymer whose weight-average molecular weight reaches 12700 could be obtained. The prepared copolymer has higher thermostability, degradability and good appearance.

参考文献

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