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A method for the enrichment and separation of basic nitrogen compounds in shale diesel oil

A technology for shale diesel oil and nitrogen compounds, which is applied in the petroleum industry, processing hydrocarbon oil, hydrocarbon oil processing products, etc., to achieve the effects of simple and feasible operation, lower production cost, and favorable processing.

Active Publication Date: 2018-05-04
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 trace separation and analysis method. It has the advantages of simple equipment, fast speed, good separation effect and high sensitivity, but it is only suitable for the separation of small amounts of samples.

Method used

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  • A method for the enrichment and separation of basic nitrogen compounds in shale diesel oil
  • A method for the enrichment and separation of basic nitrogen compounds in shale diesel oil
  • A method for the enrichment and separation of basic nitrogen compounds in shale diesel oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Mix 90ml of N,N-dimethylformamide with 300ml of shale diesel (the molar ratio is 0.3:1), heat and stir in a water bath, set the heating temperature to 50°C, and pour it into a separatory funnel after stirring The sample was separated into layers, and after standing for 10 minutes, the oil product in the lower layer was distilled to obtain extracted oil and N,N-dimethylformamide, and N,N-dimethylformamide was recycled. The extracted oil was separated by column chromatography, 50g of silica gel was weighed, and chromatographically eluted with 80mL of petroleum ether and 80mL of benzene / methanol mixed solution (1:1 by volume) in sequence. The obtained benzene / methanol eluate was extracted 3 times with water to separate the benzene layer solution, then extracted the benzene layer solution with 3mol / L HCl to obtain the inorganic layer, and neutralized the inorganic layer with 6mol / L NaOH solution to PH = 11, then adding n-hexane for extraction three times, extracting the bas...

Embodiment 2

[0027] Mix the extractant dimethyl sulfoxide and shale diesel at a molar ratio of 0.5:1 for a stirring reaction. The stirring reaction temperature is 50°C. After standing and settling for 20 minutes, the oil product is divided into two layers. Recover by vacuum distillation and recycle; the lower layer removes the extractant to obtain the extracted oil that is initially enriched with basic nitrogen compounds; the extracted oil is concentrated and separated by column chromatography, acid extraction of basic compounds, alkali neutralization of acid, and solvent back extraction Basic nitrides, solvent removal, and vacuum drying to obtain basic nitrides. 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 Example 1.

Embodiment 3

[0029] The extraction agent N-methylpyrrolidone and shale diesel are mixed in a molar ratio of 1:1 for stirring reaction. The stirring reaction temperature is 70°C. After standing for 50 minutes, the oil product is divided into two layers. Recover by vacuum distillation and recycle; the lower layer removes the extractant to obtain the extracted oil that is initially enriched with basic nitrogen compounds; the extracted oil is concentrated and separated by column chromatography, acid extraction of basic compounds, alkali neutralization of acid, and solvent back extraction Basic nitrides, solvent removal, and vacuum drying to obtain basic nitrides. 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 1.2:1; other steps are the same as in Example 1.

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Abstract

The invention relates to an enrichment and separation method for basic nitrides in shale diesel oil. The key of the method refers to adoption of a separation method combining solvent refining and column chromatography. An extracting agent and shale diesel oil fractions are proportionally mixed and subjected to solvent refining, and extract oil with primarily enriched basic nitrides is obtained after refining; the extract oil is taken as a raw material for deep enrichment of the basic nitrates and is subjected to further concentration and separation with column chromatography, solvent removing and vacuum drying, and the basic nitrides are obtained.

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 basic nitrides in shale diesel 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 of 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. Nitrogen compounds in oil products can generally be divided into basic nitrogen compounds and non-basic nitrogen compounds. The existence of basic nitrogen compounds has a direct impact on the reprocessing and utilization of shale oil, and is a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10G53/04
CPCC10G53/04C10G2300/202C10G2400/04
Inventor 韩冬云金阳曹祖宾
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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