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作 者:于玉建 梁雨涛 张陆军 王金良[1] Yu Yujian;Liang Yutao;Zhang Lujun;Wang Jinliang(Institute of Chemistry Co.,Ltd.,Henan Academy of Sciences,Zhengzhou 450002,Henan,China)
机构地区:[1]河南省科学院化学研究所有限公司,河南郑州450002
出 处:《中国胶粘剂》2022年第6期48-51,共4页China Adhesives
基 金:河南省科学院资助项目(220403012、220203003、210403020、210603034)
摘 要:针对4-二甲氨基吡啶—乙酸酐—丁酮(MEK)法测试聚醚多元醇羟值存在的结果误差大和溶液黄变等问题,进行了操作步骤和条件的优化。研究了反应温度、酰化时间、水解时间等对测试结果的影响,并对测试结果的准确性和平行度与咪唑—苯酐—吡啶法进行了比较。研究结果表明:4-二甲氨基吡啶—乙酸酐—MEK法的优化条件为反应温度5~35℃,酰化反应30 min,水解反应10 min。该优化方法能够很好地适用于分析羟值≤1000的聚醚多元醇,具有分析范围广、操作简单快捷、结果准确稳定和环保安全等优点,能够满足实际生产测试的要求。In order to solve the problems of large deviation of test results and yellowing of solution in the measurement of hydroxyl value of polyether polyols by 4-dimethylaminopyridine—acetic anhydride—methyl ethyl ketone(MEK)method,the operation steps and conditions were optimized.The effects of reaction temperature,acylation time and hydrolysis time on the test results were studied.The accuracy and parallelism of the test results were compared with that of imidazole—phthalic anhydride—pyridine method.The research results showed that the optimum conditions of 4-dimethylaminopyridine—acetic anhydride—MEK method were as follows:reaction temperature 5-35℃,acylation reaction 30 min,hydrolysis reaction 10 min.The optimization method could be well applied to the analysis of polyether polyols with hydroxyl value≤1000.It had the advantages of wide analysis range,simple and fast operation,accurate and stable results,environmental protection and safety,which could meet the requirements of actual production and testing.
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