聚酯多元醇的合成与表征
Synthesis and characterization of polyester polyols
张小凡 1朱文杰 1徐守斌 2罗金安 2陈良 1李劲超 1张亚萍1
作者信息
- 1. 西南科技大学材料与化学学院,生物质材料教育部工程研究中心,四川 绵阳 621010
- 2. 禾大西普化学(四川)有限公司,四川 绵阳 621011
- 折叠
摘要
为探究不同二元酸对聚酯多元醇性能的影响,以壬二酸、己二酸、1,4-丁二醇为原料,通过酯化-缩聚反应制得聚酯多元醇,利用红外光谱、核磁共振氢谱、凝胶色谱、热质量分析、旋转流变等测试手段对合成产物的结构进行表征,并研究醇酸摩尔比和合成工艺对合成产物酸值、羟值的影响.通过调控反应温度、反应时间等参数,确定不同反应条件下制得的聚酯多元醇的酸值、羟值,以获得最佳工艺条件,再进行减压脱醇处理后,对最终产物进行性能测试.结果表明,壬二酸聚酯多元醇的酸值为0.520 mg KOH/g、羟值为39.0 mg KOH/g、分子量为19 421、完全分解的温度为514 ℃;己二酸聚酯多元醇的酸值为0.830 mg KOH/g、羟值为46.6 mg KOH/g、分子量为19 219、完全分解的温度为438 ℃,说明壬二酸聚酯多元醇比己二酸聚酯多元醇有更低的酸值、羟值,更好的热稳定性和更低的黏度.因此,使用壬二酸比己二酸更适合作为原料来合成聚酯多元醇.
Abstract
Polyester polyols were prepared through esterification and polycondensation reactions using azelaic acid,adipic acid,and 1,4-butanediol as raw materials to investigate the effects of different dibasic acids on the properties of polyester polyols.The structures of the synthesized products were characterized by infrared spectroscopy,hydrogen NMR spectroscopy,gel chromatography,thermogravimetric analysis,and rotational rheology.The effects of the mole ratio of alcohol to acid and synthesis process on the acid and hydroxyl values of the synthesized product were studied.The acid and hydroxyl values of polyester polyols prepared under different reaction conditions were determined to obtain the optimal process conditions by adjusting parameters including reaction temperature and duration.The performance of the final products was tested after dealcoholization under reduced pressure.The results showed that the acid values of azelaic acid polyester polyols and adipic acid polyester polyols were 0.520 mg KOH/g and 0.830 mg KOH/g respectively.Their respective hydroxyl values were 39.0 mg KOH/g and 46.6 mg KOH/g;molecular weights were 19,421 and 19,219;and the temperatures for complete decomposition were 514 ℃ and 438 ℃.These findings suggest that azelaic acid polyester polyols have lower acid and hydroxyl values,better thermal stability,and lower viscosity than adipic acid polyester polyols.Therefore,azelaic acid is more suitable for the synthesis of polyester polyols than adipic acid.
关键词
聚酯多元醇/酯化-缩聚/壬二酸/己二酸/合成工艺Key words
polyester polyol/esterification and polycondensation/azelaic acid/adipic acid/synthesis technology引用本文复制引用
基金项目
国家自然科学基金(21878250)
禾大西普化学(四川)有限公司委托项目(23zh0156)
出版年
2024
国家科技期刊平台
NSTL
万方数据