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使用气相色谱 - 质谱联用仪和电喷雾电离高分辨率质谱仪对合成气基乙交酯进行成分表征

Compositional Characterization of Syngas-Based Glycolide Using Gas Chromatogram-Mass Spectrometry and Electrospray Ionization High-Resolution Mass Spectrometry.

作者信息

Zhang Yachun, Chen Junyang, He Jianhua, Li Shuofan, Wang Yuanfeng, Zhang Yahe, Shi Quan

机构信息

CHN Energy Yulin Chemical Co., Ltd., Yulin 719000, China.

State Key Laboratory of Heavy Oil Processing, China University of Petroleum, Beijing 102249, China.

出版信息

Molecules. 2024 Aug 8;29(16):3759. doi: 10.3390/molecules29163759.

Abstract

Polyglycolic acid (PGA) is a biologically friendly material with a wide range of applications. The production of dimethyl oxalate using coal-based syngas and the hydrogenation of dimethyl oxalate can produce the polymerization raw material of PGA, glycolide, which requires a methyl glycolate polymerization and depolymerization process. The intermediate products of the production process were analyzed using gas chromatogram-mass spectrometry (GC-MS) and Orbitrap mass spectrometry (Orbitrap MS), which revealed the presence of cyclic and linear PGAs with different capped ends. The impurities present in the oligomer were mostly methyl-capped PGA and were retained in the subsequent depolymerization process to glycolide, solvent washing can be used to remove this part of the impurity and ultimately obtain a refined glycolide product. Furthermore, it is proposed that the use of the specialized Kendrick Mass Defect (KMD) to plot and analyze PGA compounds obtained using mass spectrometry can enable the direct classification of PGAs without the need for exact molecular formula assignment.

摘要

聚乙醇酸(PGA)是一种具有广泛应用的生物友好型材料。利用煤基合成气生产草酸二甲酯以及草酸二甲酯的氢化反应能够生成PGA的聚合原料乙交酯,这需要一个乙醇酸甲酯的聚合和解聚过程。使用气相色谱 - 质谱联用仪(GC - MS)和轨道阱质谱仪(Orbitrap MS)对生产过程中的中间产物进行分析,结果显示存在具有不同封端的环状和线性PGA。低聚物中存在的杂质大多是甲基封端的PGA,并且在随后向乙交酯的解聚过程中会残留,可通过溶剂洗涤去除这部分杂质,最终获得精制的乙交酯产品。此外,有人提出使用专门的肯德里克质量亏损(KMD)对通过质谱获得的PGA化合物进行绘制和分析,能够直接对PGA进行分类,而无需精确的分子式赋值。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/013b/11356849/f597c484588a/molecules-29-03759-g001.jpg

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