重油中含硫芳烃二维液相色谱分离平台开发及应用

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。

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

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.