生物基1,3-丙二醇中微量杂质的气相色谱-质谱分析法  

Analytical method for trace impurity in bio-based 1,3-propanediol by gas chromatography-mass spectrometry

作　　者：朱欢银 张才亮[1] 冯连芳[1] 顾雪萍[1] ZHU Huan-yin;ZHANG Cai-liang;FENG Lian-fang;GU Xue-ping(State Key Laboratory of Chemical Engineering,Zhejiang University,Hangzhou 310027,China)

机构地区：[1]浙江大学化学工程联合国家重点实验室

出　　处：《现代化工》2020年第1期220-224,229,共6页Modern Chemical Industry

基　　金：国家重点研发计划(2017YFB0309401)

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。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 biobased 1,3-propanediol contains trace impurities such as 3-methoxy-1,2-propanediol,diethylene glycol and Dpantolactone.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 杂质分析 气相色谱-质谱联用 

分 类 号：TQ323.43[化学工程—合成树脂塑料工业]