Separation method for alkali nitrogen compounds in coal liquefaction oil

A separation method and technology for coal liquefied oil, which are applied in the direction of refining with acid-containing liquid and only multi-stage series refining process treatment, can solve the problem of inaccurate analysis results of basic nitrogen compounds, high content of impurities in extracts, and alkali Incomplete separation of nitrogen compounds, etc., to achieve the effect of thorough extraction, high separation degree and good separation selectivity

Active Publication Date: 2013-11-20
CHNA ENERGY INVESTMENT CORP LTD +2
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Problems solved by technology

[0004] The invention provides a method for separating basic nitrogen compounds in coal liquefied oil to solve the problem of incomplete separation of basic nitrogen compounds in coal liquefied oil and the high impurity content in the extract, which leads to inaccurate analysis results of basic nitrogen compounds The problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Toluene is used as solvent to prepare model compounds with mass fractions of 0.0296% pyridine, 0.0388% aniline, 0.0267% quinoline and 0.0123% acridine (to simulate coal liquefied oil).

[0031] Get 30g of the model compound and place it in a separatory funnel, add 5g of hydrochloric acid aqueous solution of 10% mass concentration and shake and mix for 10 minutes, separate the lower aqueous phase after standing still for 10 minutes, and continue to shake and mix with the same amount of hydrochloric acid aqueous solution for 10 minutes for the upper organic phase. After standing still for 10 minutes, separate the lower water phase; add 12g of sodium hydroxide with 10% mass concentration to the collected water phase, adjust the pH value of the water phase solution to 8~10, add dichloromethane after cooling to extract (dichloromethane The volume ratio of methane to water phase is 1:2), each extraction time is 20 minutes, and the lower organic phase obtained after repeated fo...

Embodiment 2

[0034] Same as in Example 1, using toluene as a solvent, a model compound with a mass fraction of 0.0296% of pyridine, 0.0388% of aniline, 0.0267% of quinoline, and 0.0123% of acridine (to simulate coal liquefied oil) was prepared.

[0035]Get 30g model compound and place in the separatory funnel, add 3g of hydrochloric acid aqueous solution of 36% mass concentration and shake and mix for 30 minutes, separate the lower floor water phase after standing still for 30 minutes, the upper organic phase continues to shake and mix with the same amount of hydrochloric acid aqueous solution for 30 minutes and After standing still for 30 minutes, separate the lower water phase; add 8 g of sodium hydroxide of 36% mass concentration to the collected water phase, adjust the pH value of the water phase solution to 8~10, add dichloromethane after cooling to extract (dichloromethane The volume ratio of methane to water phase is 1:1), each extraction time is 20 minutes, and the lower organic pha...

Embodiment 3

[0038] Same as Example 1, with the coal liquefied naphtha which does not contain nitrogen after hydrogenation and upgrading as a solvent, it is prepared with a mass fraction of 0.0443% of pyridine, 0.0482% of aniline, 0.0502% of quinoline, and 0.0168% of acridine model compound.

[0039] Take 30g of standard-added modified naphtha and place it in a separatory funnel, add 5g of sulfuric acid aqueous solution of 10% mass concentration and shake and mix for 10 minutes, and then separate the lower water phase after standing still for 10 minutes, and add 10% mass concentration Potassium hydroxide 12g, the pH value of aqueous phase solution is adjusted to 8~10, after cooling, add the dichloromethane of 10 milliliters and carry out extraction, and extraction time is 20 minutes, and the lower organic phase that obtains is collected, gas chromatography analysis.

[0040] The recoveries of basic nitrogen compounds (pyridine, aniline, quinoline, acridine) after pickling and extraction we...

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PUM

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Abstract

The invention discloses a separation method for alkali nitrogen compounds in coal liquefaction oil. The separation method comprises the following steps of: acid pickling: mixing the coal liquefaction oil with an acidic solution, carrying out vibrating, standing and layering, and separating to obtain a water phase solution; and organic solvent extraction: regulating the pH value of the water phase solution to be 8-10, adding organic solvents after cooling, carrying out mixing, vibrating, standing and layering, and separating to obtain an organic phase solution rich in the alkali nitrogen compounds. By utilizing the separation method disclosed by the invention, the alkali nitrogen compounds in the coal liquefaction oil are processed by utilizing an acid pickling method and an organic solvent extraction method, the effects that the alkali nitrogen compounds in the coal liquefaction oil are good in separation selectivity and high in separation degree and are thoroughly extracted are achieved, and the obtained organic phase solution can be directly used for carrying out sample injection analysis on the alkali nitrogen compounds.

Description

technical field [0001] The invention relates to the field of coal-to-oil coal chemical industry, in particular to a method for separating basic nitrogen compounds in coal liquefied oil. Background technique [0002] As an efficient and clean coal technology that can partially alleviate the contradiction between the supply and demand of my country's petroleum resources, direct coal liquefaction has entered the stage of commercial demonstration operation. The crude coal liquefied oil produced by the direct coal liquefaction process contains a certain amount of nitrogen-containing compounds, a considerable part of which is basic nitrogen compounds. When coal liquefied oil is further hydrotreated to produce diesel fuel, basic nitrogen compounds are one of the main factors causing catalyst deactivation. In order to understand the catalyst deactivation mechanism, it is necessary to analyze the structure of the basic nitrogen compound components; when purifying and converting nitr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G17/06C10G17/07C10G53/10
Inventor 姜元博李克健高山松李延红杨葛灵章序文李永伦向春兰
Owner CHNA ENERGY INVESTMENT CORP LTD
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