离子淌度-飞行时间质谱测定减压蜡油芳香分及胶质中的碱性氮化物

石油炼制与化工 ›› 2021, Vol. 52 ›› Issue (1): 103-110.

离子淌度-飞行时间质谱测定减压蜡油芳香分及胶质中的碱性氮化物

窦民娜^1,2,喻昊¹,刘为民³,曹青¹,陈菲¹,余颖龙¹,张占全¹,王延飞¹

1. 中国石油石油化工研究院
2. 中国石油大学（北京）
3. 中国石油大庆石化分公司质量检验中心

收稿日期:2020-05-20 修回日期:2020-09-14 出版日期:2021-01-12 发布日期:2020-12-29
通讯作者: 曹青 E-mail:caoqing010@petrochina.cn
基金资助:

CHARACTERIZATION OF BASIC NITROGEN COMPOUNDS IN AROMATIC AND RESIN FRACTIONS IN VACCUM GAS OILS BY ION MOBILITY-TIME-OF-FLIGHT MASS SPECTROMETRY

Received:2020-05-20 Revised:2020-09-14 Online:2021-01-12 Published:2020-12-29
Supported by:

摘要/Abstract

摘要： 采用柱层析法将减压蜡油（VGO）分离为饱和分、芳香分和胶质，然后用电喷雾电离源（ESI）离子淌度-飞行时间质谱（IMS-TOF MS）对其芳香分与胶质中的碱性氮化物进行了表征，对不同来源的VGO中碱性氮化物的结构差异进行了分析。结果表明：对于不同来源的VGO样品，即使碱性氮化物不饱和程度接近，其芳环的连接方式也存在明显差异；而对于同一样品的芳香分和胶质，则存在碳数相近，但胶质中等效双键数稍低的现象。以核磁共振波谱仪异核单量子相干试验和加氢脱氮反应评价作为辅证，进一步推测了VGO中碱性氮化物的芳环侧链长度与其脱除难度之间的关联。将柱层析分离技术与ESI IMS-TOF MS联用，可以解决高蜡含量样品难以溶解的问题，并减弱强极性组分的离子化抑制作用，得到比直接进样更为全面的质谱信息。

关键词: 减压蜡油, 氮化物, 离子淌度, 飞行时间质谱, 层柱析, NMR

Abstract: Vacuum gas oil (VGO) samples were separated into saturates, aromatics and resin by column chromatography，then the basic nitrides in aromatics and resin fractions were characterized by electrospray ionization source (ESI) ion mobility-time-of-flight mass spectrometry (IMS-TOF MS), and the structural differences of the basic nitrides in VGOs from different sources were analyzed. The results showed that for VGO samples from different sources, even if the unsaturated degree of basic nitride was close, there were obvious differences in the connection mode of aromatic ring; however, for the aromatic components and resin of the same sample, the carbon number was similar, and the number of equivalent double bonds in resin was slightly lower. Taking the heteronuclear single quantum coherence test of NMR spectrometer and the evaluation of hydrodenitrogenation reaction as the auxiliary evidence, the relationship between the side chain length of aromatic ring of basic nitride in VGO and its removal difficulty was further speculated. Combining column chromatography with ESI IMS-TOF MS can solve the problem that samples with high wax content are difficult to dissolve, and weaken the ionization inhibition of strong polar components, thus obtaining more comprehensive mass spectrum information than direct injection.

Key words: vacuum gas oil, nitrogen compounds, ion mobility, TOF mass spectrometry, column chromatography, NMR

中图分类号:

窦民娜喻昊刘为民曹青陈菲余颖龙张占全王延飞. 离子淌度-飞行时间质谱测定减压蜡油芳香分及胶质中的碱性氮化物[J]. 石油炼制与化工, 2021, 52(1): 103-110.

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