【摘要】：以吉林樺甸油頁(yè)巖為研究對(duì)象，通過(guò)二氯甲烷、石油醚兩級(jí)萃取，對(duì)油頁(yè)巖原礦、兩級(jí)萃余物進(jìn)行SEM拍照，對(duì)二氯甲烷萃取液、石油醚萃取液進(jìn)行GC/MS檢測(cè)，研究樺甸油頁(yè)巖在兩級(jí)溶液的溶解行為以及各級(jí)萃余物表面物理形貌。結(jié)果表明：隨著萃取的加深，油頁(yè)巖顆粒相對(duì)光滑的片層結(jié)構(gòu)逐漸消失，顆粒粒徑趨于細(xì)小，表面溝壑逐漸增多，后級(jí)萃取時(shí)液固接觸面積增加。二氯甲烷和石油醚對(duì)油頁(yè)巖中烷烴溶出能力較強(qiáng)。兩級(jí)萃取物組分主要由C15至C28飽和烷烴構(gòu)成。溶劑萃取法可以有效地的提取油頁(yè)巖中一類或相似的化合物群，對(duì)研究油頁(yè)巖構(gòu)成及提取高經(jīng)濟(jì)價(jià)值成分有重要意義。 以廣東茂名和遼寧撫順油頁(yè)巖為樣品，，對(duì)其進(jìn)行鹽酸酸洗，利用兩種溶劑二氯甲烷和四氫呋喃對(duì)酸洗前后的油頁(yè)巖進(jìn)行索氏萃取，并利用GC/MS對(duì)萃取液進(jìn)行分析，得出兩種溶劑在酸洗前后萃取到的物質(zhì)種類。研究油頁(yè)巖在有機(jī)溶劑萃取條件下，小分子化合物的溶出規(guī)律。結(jié)果表明：酸洗更有利于油頁(yè)巖中的小分子溶出，可以提高萃取率。酸洗對(duì)于萃取物組分中的烷烴化合物組分影響較小而對(duì)含氧小分子化合物組分影響相對(duì)較大。對(duì)比同一樣品酸洗前后的萃取液，一些重復(fù)出現(xiàn)的物質(zhì)的相對(duì)含量或檢出物的個(gè)數(shù)發(fā)生了變化。二氯甲烷的溶出物主要是烷烴，四氫呋喃的溶出物主要是含氧小分子化合物。 利用二氯甲烷和四氫呋喃對(duì)酸洗前后的油頁(yè)巖進(jìn)行索氏萃取，對(duì)萃取液進(jìn)行GC/MS檢測(cè)，分析溶出物的組成。對(duì)萃取物進(jìn)行孔隙結(jié)構(gòu)測(cè)試，分析酸洗及萃取前后吸附量和孔徑結(jié)構(gòu)的變化。通過(guò)溶劑作用溶出小分子化合物并改變油頁(yè)巖孔隙結(jié)構(gòu)，進(jìn)而得出可溶小分子的賦存方式。結(jié)果表明：二氯甲烷主要溶出物種類為烷烴，四氫呋喃主要溶出物種類為含氧小分子化合物。酸洗會(huì)使得孔隙結(jié)構(gòu)更加豐富，有利于可溶小分子的溶出。油頁(yè)巖經(jīng)過(guò)溶劑萃取后會(huì)使得中（2-50nm）、大孔(50nm)數(shù)量增多。油頁(yè)巖孔隙結(jié)構(gòu)中可以貯存可溶小分子，富集在油頁(yè)巖表面的可溶小分子在溶出時(shí)會(huì)產(chǎn)生孔洞�？扇苄》肿釉谌艹鲞^(guò)程中會(huì)使得油頁(yè)巖產(chǎn)生新孔或擴(kuò)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.
【學(xué)位授予單位】：東北電力大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TE662.3

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