A method for the enrichment and separation of phenolic compounds in shale oil
A technology of phenolic compounds and shale oil, which is applied in the petroleum industry, hydrocarbon oil treatment, and multi-stage serial refining process treatment, etc., to achieve the effects of reducing production costs, simple and feasible operation, and effective enrichment and separation
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Embodiment 1
[0025] Mix 99ml of furfural with 330ml of shale oil whole fraction (molar ratio is 0.3:1), heat and stir in a water bath, set the heating temperature to 50°C, after stirring, pour it into a separating funnel until the samples are separated, and let stand After 10 minutes, the oil in the lower layer was distilled to obtain extracted oil and furfural, and the furfural was recycled. The extracted oil is distilled and cut according to one fraction per 20°C, and divided into ≤260°C, 260°C~280°C, 280°C~300°C, 300°C~320°C, 320°C~340°C, 340°C~360°C ,> 360 ℃ seven fractions, for phenol content analysis. Take fractions ≤ 280°C for column chromatography, weigh 50g of silica gel, and sequentially use petroleum ether and benzene / methanol mixed solution (volume ratio 1:1) to chromatographically elute the column. The obtained benzene / methanol eluate was extracted 3 times with water to separate the benzene layer solution, and then the benzene layer solution was extracted with 3mol / L HCl to o...
Embodiment 2
[0027] Mix the extraction agent dimethyl sulfoxide and the whole fraction of shale oil at a molar ratio of 0.5:1 for stirring reaction. The stirring reaction temperature is 50°C. After standing and settling for 20 minutes, the oil product is divided into two layers. The extraction of the upper layer and the lower layer The extraction agent can be recovered by vacuum distillation and recycled; after the lower layer removes the extraction agent, the extracted oil that is initially enriched in phenolic compounds is obtained; the fraction of the extracted oil ≤ 280 ° C is concentrated and separated by column chromatography, acid washed to remove alkaline compounds, and alkali extracted Extraction of phenolic compounds, acid neutralization of phenate, solvent back extraction of phenolic compounds, solvent removal, and vacuum drying to obtain phenolic compounds. The column chromatography solid adsorbent is silica gel; the column chromatography mobile phase is petroleum ether, benzene...
Embodiment 3
[0029] Mix the extractant furfural with the whole fraction of shale oil in a molar ratio of 1:1 for a stirring reaction. The stirring reaction temperature is 60°C. After standing and settling for 30 minutes, the oil product is divided into two layers. Recovery by pressure distillation and recycling; the lower layer removes the extractant to obtain the extracted oil that is initially enriched in phenolic compounds; the fraction of the extracted oil ≤ 280 ° C is concentrated and separated by column chromatography, acid-washed to remove alkaline compounds, and alkali-extracted phenolic compounds , acid neutralization of phenate, solvent back extraction of phenolic compounds, solvent removal, and vacuum drying to obtain phenolic compounds. The column chromatography solid adsorbent is silica gel; the column chromatography mobile phase is petroleum ether, benzene / methanol mixed solution; the volume ratio of benzene / methanol mixed solution is 1:1; other steps are the same as in Exampl...
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