重油中含硫芳烃二维液相色谱分离平台开发及应用

doi:10.3724/SP.J.1123.2019.01014

色谱 ›› 2019, Vol. 37 ›› Issue (7): 750-758.DOI: 10.3724/SP.J.1123.2019.01014

重油中含硫芳烃二维液相色谱分离平台开发及应用

宋春侠, 王威, 刘泽龙, 刘颖荣, 蔡新恒

中国石化石油化工科学研究院, 北京 100083

收稿日期:2019-01-11 出版日期:2019-07-08 发布日期:2015-05-21
通讯作者: 宋春侠.Tel:(010)82368819,E-mail:songchunxia.ripp@sinopec.com.
基金资助:
中国石化石油化工科学研究院院控课题（R16023）.

Development and application of two-dimensional liquid chromatography for the analysis of polycyclic aromatic sulfur heterocycles in heavy oil

SONG Chunxia, WANG Wei, LIU Zelong, LIU Yingrong, CAI Xinheng

Research Institute of Petroleum Processing, SINOPEC, Beijing 100083, China

Received:2019-01-11 Online:2019-07-08 Published:2015-05-21
Supported by:
Research Project of Research Institute of Petroleum Processing, SINOPEC (No. R16023).

摘要/Abstract

摘要： 基于氯化钯配位交换色谱柱和氨基键合正相色谱柱，利用自动阀切换系统，构建了在线二维液相色谱分离平台。通过优化液相色谱分离条件，实现减压蜡油样品中含硫芳烃的在线富集与多环芳烃的环数分离。利用傅里叶变换离子回旋共振质谱对分离后的含硫芳烃和芳烃组分进行分子水平表征，得到更为详细的化合物类型与碳数分布信息。根据计算得到的平均结构信息，可以提供分离后组分典型的分子结构式，并对芳环结构和侧链位置进行了推测。建立的分析表征方法可以加深对重馏分油中含硫芳烃化合物的分子水平认识，为重油加工过程的原料选择与工艺条件优化提供技术支持。

关键词: 多环芳烃, 二维液相色谱, 傅里叶变换离子回旋共振质谱, 含硫芳烃, 重油

Abstract: A two-dimensional liquid chromatographic (2D LC) system was developed for the analysis of polycyclic aromatic sulfur heterocycles (PASHs) in heavy oil. The first dimension is a ligand-exchange chromatographic column packed with a palladium chloride/silica (PdCl₂-SiO₂) stationary phase, while the second dimension is a Spherisorb-NH₂ column. The PASHs in vacuum gas oil were enriched online, and polycyclic aromatics hydrocarbons (PAHs) were separated according to their aromatic ring numbers. These separated fractions were analyzed by Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS), and detailed molecular characterization of PASHs and PAHs was achieved. Typical molecular structures of PASHs and PAHs in these fractions could be provided, and the side chain as well as the core structures were predicted. It is significant for the feedstocks selection and optimization of the hydrodesulfurization process by using these molecular characterization information.

Key words: Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS), heavy oil, polycyclic aromatic hydrocarbons (PAHs), polycyclic aromatic sulfur heterocycles (PASHs), two-dimensional liquid chromatography (2D LC)

中图分类号:

O658

宋春侠, 王威, 刘泽龙, 刘颖荣, 蔡新恒. 重油中含硫芳烃二维液相色谱分离平台开发及应用[J]. 色谱, 2019, 37(7): 750-758.

SONG Chunxia, WANG Wei, LIU Zelong, LIU Yingrong, CAI Xinheng. Development and application of two-dimensional liquid chromatography for the analysis of polycyclic aromatic sulfur heterocycles in heavy oil[J]. Chinese Journal of Chromatography, 2019, 37(7): 750-758.

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重油中含硫芳烃二维液相色谱分离平台开发及应用

Development and application of two-dimensional liquid chromatography for the analysis of polycyclic aromatic sulfur heterocycles in heavy oil

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