固相萃取法/全二维气相色谱-飞行时间质谱测定柴油及其加氢产品中的含硫化合物  

IDENTIFICATION AND CHARACTERIZATION OF SULFUR COMPOUNDS IN DIESEL AND ITS HYDROGENATION PRODUCTS BY SOLID PHASE EXTRACTION COMPREHENSIVE TWO-DIMENSIONAL GAS CHROMATOGRAPHY COUPLED WITH TIME-OF-FLIGHT MASS SPECTROMETRY

作　　者：刘明星[1] 刘泽龙[1] 李颖[1] 章然 Liu Mingxing;Liu Zelong;Li Ying;Zhang Ran(SINOPEC Research Institute of Petroleum Processing,Beijing 100083)

机构地区：[1]中国石化石油化工科学研究院,北京100083

出　　处：《石油炼制与化工》2020年第4期96-104,共9页Petroleum Processing and Petrochemicals

摘　　要：开发了两种PdCl2-Al2O3固相萃取法,用于分离高硫柴油及加氢柴油中的硫化物,并建立了全二维气相色谱-飞行时间质谱(GC×GC-TOF MS)定性分析柴油中硫化物的方法。该方法不仅能够有效去除柴油中其他组分对硫化物的干扰,清晰展现硫化物分布,还能够准确提供不同工艺生产的柴油及加氢前后柴油中硫化物类型及碳数分布信息。结果表明:高硫柴油及加氢柴油中近90%硫化物集中在分离出的含硫组分中,而且该组分中芳烃含量极少;直馏柴油和催化裂化柴油中分别归类并定性出8类757种硫化物和4类179种硫化物,在相应加氢产品中分别鉴定出4类98种硫化物和3类81种硫化物;加氢柴油中90%以上硫化物为二苯并噻吩类化合物,侧链碳数集中在低碳数段。Two solid phase extractions methods with PdCl 2-Al 2O 3 were developed for the separation of sulfur compounds in high sulfur-containing diesel and hydrofined diesel.A comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GC-TOF MS)method for the qualitative analysis of sulfur compounds in diesel was established.This method could effectively remove the interference of other components on sulfur compounds identification,and give the accurate data of compound types and carbon number distribution of sulfur compounds in diesels from different processing units and hydrofined diesels.The results showed that nearly 90%of sulfur compounds were concentrated in sulfur-containg component separated,with very little aromatic hydrocarbons.In straight-run high sulfur diesel and catalytic cracking diesel,8 kinds of 757 and 4 kinds of 179 sulfur compounds were classified and characterized,respectively.In corresponding diesel hydrogenation products,4 kinds of 98 and 3 kinds of 81 sulfur compounds were identified,respectively.More than 90%of sulfur compounds in hydrofined diesel were dibenzothiophenes with short side chain.

关 键 词：硫化物 柴油 固相萃取 全二维气相色谱 飞行时间质谱 

分 类 号：O657.63[理学—分析化学] TE626.24[理学—化学]