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Enrichment and separation method for basic nitrides in shale diesel oil

A shale diesel and nitride technology, applied in the petroleum industry, processing hydrocarbon oil, hydrocarbon oil treatment products, etc., to achieve the effects of reducing production costs, facilitating processing, and improving comprehensive utilization value

Active Publication Date: 2017-04-26
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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  • Enrichment and separation method for basic nitrides in shale diesel oil
  • Enrichment and separation method for basic nitrides in shale diesel oil
  • Enrichment and separation method for basic nitrides 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 oil (the molar ratio is 0.3:1), heat and stir in a water bath, and set the heating temperature to 50℃. After stirring, pour into a separatory funnel for testing The samples are separated into layers, and after standing for 10 minutes, the oil in the lower layer is distilled to obtain the extracted oil and N,N-dimethylformamide, and the N,N-dimethylformamide is recycled. The extracted oil was separated by column chromatography, 50 g of silica gel was weighed, and the chromatographic column was chromatographed and eluted with 80 mL petroleum ether and 80 mL benzene / methanol mixed solution (volume ratio 1:1). The obtained benzene / methanol flushing solution was extracted three times with water, and then the benzene layer solution was separated. Then the benzene layer solution was extracted with 3mol / L HCl to obtain the inorganic layer, and the inorganic layer was neutralized with 6mol / L NaOH solution After reaching...

Embodiment 2

[0027] The extractant dimethyl sulfoxide is mixed with shale diesel at a molar ratio of 0.5:1 for stirring reaction. The stirring reaction temperature is 50°C. After standing for 20 minutes, the oil is divided into two layers. The upper and lower extractants can be It is recovered by vacuum distillation and recycled; the extracted oil is initially enriched in basic nitrogen compounds after the lower layer is de-extracted; the extracted oil is concentrated and separated by column chromatography, acid extraction of basic compounds, alkali neutralization acid, and solvent reverse extraction Basic nitride, solvent removal, vacuum drying to obtain basic nitride. 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] Mix the extractant N-methylpyrrolidone and shale diesel at a molar ratio of 1:1 for stirring reaction. The stirring reaction temperature is 70°C. After 50 minutes of standing and settling, the oil is divided into two layers. The upper and lower extractants can be It is recovered by vacuum distillation and recycled; the extracted oil is initially enriched in basic nitrogen compounds after the lower layer is de-extracted; the extracted oil is concentrated and separated by column chromatography, acid extraction of basic compounds, alkali neutralization acid, and solvent reverse extraction Basic nitride, solvent removal, vacuum drying to obtain basic nitride. 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] This application belongs to the technical field of shale oil processing, and specifically relates to a method for enriching and separating basic nitrides in shale diesel. Background technique [0002] Shale oil is a very rich potential energy source in the world, and its total storage capacity far exceeds that of petroleum. Compared with natural petroleum, shale oil contains a lot of unsaturated hydrocarbons and non-hydrocarbon compounds such as N, S, O and so on. 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 , Causing environmental pollution and low energy utilization value. Nitrogen-containing compounds in oil can generally be divided into basic nitrides and non-alkaline nitrides. The presence of basic nitrides has a direct impact on the reprocessing and utilization of shale oil. They are toxic substances to be removed or transformed, but they are...

Claims

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Application Information

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Patent Type & Authority Applications(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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