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Method for enriching and separating phenolic compounds in shale oil

A technology for phenolic compounds and shale oil, which is applied in the petroleum industry, hydrocarbon oil treatment, and multi-stage series refining process treatment, etc., to achieve the effects of simple and feasible operation, lower production costs, and effective enrichment and separation.

Active Publication Date: 2017-05-10
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Thin-layer chromatography belongs to solid-liquid adsorption chromatography. It is a micro separation and analysis method. It has the advantages of simple equipment, fast speed, good separation effect, high sensitivity and the ability to use corrosive color reagents, but it is only suitable for small amounts of samples. separation

Method used

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  • Method for enriching and separating phenolic compounds in shale oil
  • Method for enriching and separating phenolic compounds in shale oil
  • Method for enriching and separating phenolic compounds in shale oil

Examples

Experimental program
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Effect test

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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Abstract

The invention relates to a method for enriching and separating phenolic compounds in shale oil. The core of the method is a separation method combining solvent refining and column chromatography. The method comprises the following steps: mixing an extracting agent with whole fractions of the shale oil at a ratio, and carrying out the solvent refining; after refining, obtaining extracted oil for primarily enriching the phenolic compounds; cutting fractions of the extracted oil with the temperature, smaller than or equal to 280 DEG C, as raw materials for deeply enriching the phenolic compounds; and furthermore, concentrating and separating through the column chromatography, removing a solvent and drying in vacuum to obtain the phenolic compounds.

Description

technical field [0001] The application belongs to the technical field of shale oil processing, and in particular relates to a method for enriching and separating phenolic compounds in shale oil. Background technique [0002] Shale oil is a potential energy source with abundant reserves in the world, and its total storage capacity far exceeds that of petroleum. Compared with natural petroleum, shale oil contains a large amount of unsaturated hydrocarbons and non-hydrocarbon compounds such as N, S, and O. In my country, most shale oil is used as fuel for extensive combustion, and a large amount of NO is produced during the combustion process. x and SO 2 , while causing environmental pollution and low energy utilization value. Although non-hydrocarbon compounds in shale oil are toxic substances to be removed or converted, they are very useful chemical raw materials in their own right. Among them, phenolic compounds are widely used in synthetic fibers, medicine, pesticides, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G53/04
CPCC10G53/04C10G2300/1033C10G2300/202
Inventor 韩冬云金阳曹祖宾
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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