油页岩小分子溶剂溶出特性研究

发布时间：2018-09-12 07:44

【摘要】：以吉林桦甸油页岩为研究对象，通过二氯甲烷、石油醚两级萃取，对油页岩原矿、两级萃余物进行SEM拍照，对二氯甲烷萃取液、石油醚萃取液进行GC/MS检测，研究桦甸油页岩在两级溶液的溶解行为以及各级萃余物表面物理形貌。结果表明：随着萃取的加深，油页岩颗粒相对光滑的片层结构逐渐消失，颗粒粒径趋于细小，表面沟壑逐渐增多，后级萃取时液固接触面积增加。二氯甲烷和石油醚对油页岩中烷烃溶出能力较强。两级萃取物组分主要由C15至C28饱和烷烃构成。溶剂萃取法可以有效地的提取油页岩中一类或相似的化合物群，对研究油页岩构成及提取高经济价值成分有重要意义。以广东茂名和辽宁抚顺油页岩为样品，，对其进行盐酸酸洗，利用两种溶剂二氯甲烷和四氢呋喃对酸洗前后的油页岩进行索氏萃取，并利用GC/MS对萃取液进行分析，得出两种溶剂在酸洗前后萃取到的物质种类。研究油页岩在有机溶剂萃取条件下，小分子化合物的溶出规律。结果表明：酸洗更有利于油页岩中的小分子溶出，可以提高萃取率。酸洗对于萃取物组分中的烷烃化合物组分影响较小而对含氧小分子化合物组分影响相对较大。对比同一样品酸洗前后的萃取液，一些重复出现的物质的相对含量或检出物的个数发生了变化。二氯甲烷的溶出物主要是烷烃，四氢呋喃的溶出物主要是含氧小分子化合物。利用二氯甲烷和四氢呋喃对酸洗前后的油页岩进行索氏萃取，对萃取液进行GC/MS检测，分析溶出物的组成。对萃取物进行孔隙结构测试，分析酸洗及萃取前后吸附量和孔径结构的变化。通过溶剂作用溶出小分子化合物并改变油页岩孔隙结构，进而得出可溶小分子的赋存方式。结果表明：二氯甲烷主要溶出物种类为烷烃，四氢呋喃主要溶出物种类为含氧小分子化合物。酸洗会使得孔隙结构更加丰富，有利于可溶小分子的溶出。油页岩经过溶剂萃取后会使得中（2-50nm）、大孔(50nm)数量增多。油页岩孔隙结构中可以贮存可溶小分子，富集在油页岩表面的可溶小分子在溶出时会产生孔洞。可溶小分子在溶出过程中会使得油页岩产生新孔或扩大孔尺寸。
[Abstract]:Taking Huadian oil shale in Jilin province as the research object, through two-stage extraction of dichloromethane and petroleum ether, the oil shale raw ore and two-stage extraction residues were photographed by SEM, and the dichloromethane extract and petroleum ether extract were detected by GC/MS. The dissolution behavior of Huadian oil shale in two-stage solution and the physical morphology of the surface of the residue were studied. The results showed that the relatively smooth lamellar structure of oil shale particles gradually disappeared with the deepening of extraction, the particle size tended to be small, the surface gully increased, and the liquid-solid contact area increased during the later stage extraction. Dichloromethane and petroleum ether have strong ability to dissolve alkanes from oil shale. The components of the two-stage extracts are mainly composed of C 15 to C 28 saturated alkanes. Solvent extraction method can effectively extract a class or similar compound groups from oil shale, which is of great significance to the study of oil shale composition and extraction of high economic value components. The oil shale of Maoming and Fushun of Liaoning Province was pickled with hydrochloric acid. The oil shale before and after pickling was extracted by Soxhlet extraction with dichloromethane and tetrahydrofuran, and the extraction solution was analyzed by GC/MS. The kinds of substances extracted from the two solvents before and after pickling were obtained. The dissolution law of small molecular compounds in oil shale was studied under the condition of organic solvent extraction. The results show that pickling is more favorable to the dissolution of small molecules in oil shale and can improve the extraction rate. The effect of pickling on the alkane components in the extracts was less than that on the oxygen-containing small molecular compounds. The relative content of some repeated substances or the number of the detected substances were changed compared with the extraction solution before and after pickling of the same sample. The dissolution of dichloromethane is mainly alkane, and that of tetrahydrofuran is mainly oxygen-containing small molecule compound. The oil shale before and after pickling was extracted with dichloromethane and tetrahydrofuran by Soxhlet extraction. The extraction solution was detected by GC/MS to analyze the composition of the dissolution. The pore structure of the extract was tested and the changes of adsorption capacity and pore structure before and after pickling and extraction were analyzed. Small molecular compounds were dissolved by solvent and the pore structure of oil shale was changed, and the occurrence mode of soluble small molecules was obtained. The results showed that the main dissolved compounds of dichloromethane and tetrahydrofuran were alkanes and small molecular compounds containing oxygen respectively. Pickling will enrich the pore structure and facilitate the dissolution of soluble small molecules. Oil shale will increase the number of 2-50nm and 50nm after solvent extraction. Soluble small molecules can be stored in the pore structure of oil shale. Soluble small molecules cause oil shale to produce new or enlarged pore sizes during dissolution.
【学位授予单位】：东北电力大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TE662.3

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