油页岩CS_2-NMP萃取物中含氧化合物的分离与分析

Separation and structure analysis of oxygenous compounds extracted by CS_2- NMP from Yilan oil shale

为实现依兰油页岩萃取物中含氧化合物的分离与分析,采用索氏萃取法,在60℃条件下以CS2-NMP为萃取剂萃取依兰油页岩。用TiCl4/CuCl2两步络合法和硅胶柱色谱法对依兰页岩油中的含氧化合物进行富集,并对含氧洗脱组分进行了气相色谱-质谱串联(GC/MS)分析。结果表明:TiCl4/CuCl2两步络合法可以实现油页岩中含氮化合物的分离,脱氮率为82%,硅胶柱色谱可以实现对页岩油中含氧化合物的富集,富集组分中,氧元素的质量分数为10.69%;柱色谱富集组分中鉴定出32种含氧化合物,其组成以酚、酮、醚、酯以及有机硅氧化合物为主;在这些含氧化合物中发现了甾醇类、萜类化合物的衍生物以及酰胺基团,说明依兰油页岩中的氧可能来源于成矿的高等植物和蓝绿藻。该结果可以为依兰油页岩资源的合理利用、油页岩的成因和油母结构研究提供参考。

This paper is aimed at separating and analyzing the oxygenous compounds extracted from Yilan oil shale and introduces the extraction of Yilan oil shale by Saxhlet extraction device and using CS2- NMP at 60 ℃. The paper highlights the use of TiCl4/ CuCl2two-step complexometry and gel column chromatography to enrich oxygenous compounds in shale oil and analysis of the oxygenous fraction by GC / MS technology. The results suggest that TiCl4/ CuCl2two-step complexometry allows the nitrogen species in shale oil to be separated with the denitrification rate of 82%; gel column chromatography permits the oxygenous compounds to be enriched,with the mass percentage of oxygen element up to 10. 69%; 32 kinds of oxygenous compounds identified by GC / MS are dominated by phenols,ketones,ethers,esters and organic siloxane; and the presence of sterols,terpenoid＇s derivative and amide groups in these oxygenous compounds explains that oxygen element in Yilan oil shale may derive from higher plant and cyanobacteria. The study may provide references for rational utilization of oil shale resources in Yilan and investigating formation and structure of oil shale.