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摘要
建立了一种聚合级生物基丙二醇中微量杂质的定性、定量GC-MS分析方法。使用HP-INNOWAX极性色谱柱，升温程序为50℃保持2 min、10℃/min升温至130℃并保持3 min、5℃/min升温至190℃并保持3 min、10℃/min升温至230℃并保持5 min，能有效分离杂质。结果表明，聚合级生物基丙二醇中含有微量3-甲氧基-1，2-丙二醇、二乙二醇、D-泛酸内酯，其中D-泛酸内酯含量2.14×10-5，为以生物基丙二醇制备聚酯工艺提供指导。
Abstract
An analytical method by gas chromatography-mass spectrometry is developed for determining qualitatively and quantitatively trace impurity in bio-based 1,3-propanediol.HP-INNOWAX polar column is used to separate impurities effectively with a temperature program that the temperature is held at 50℃ for 2 minutes,then lifted at a speed of 10℃/min to 130℃,held at 130℃ for 3 minutes,lifted at a speed of 5℃/min to 190℃,held at 190℃ for 3 minutes,lifted at a speed of 10℃/min to 230℃ and held at 230℃ for 5 minutes.The results show that polymerization grade bio-based 1,3-propanediol contains trace impurities such as 3-methoxy-1,2-propanediol,diethylene glycol and D-pantolactone.The content of D-pantolactone is 21.4 ppm.It can provide guidance for the preparation of polyester from bio-1,3-propanediol.
关键词
生物基1,3-丙二醇
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气相色谱-质谱联用
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杂质分析
Key words
bio-based 1,3-propanediol
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gas chromatography-mass spectrometry
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trace impurity
Author summay
生物基1,3-丙二醇中微量杂质的气相色谱-质谱分析法[J].
现代化工, 2020, 40(1): 220-224,229 DOI:10.16606/j.cnki.issn0253-4320.2020.01.047
