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Method for separating and determining aromatic hydrocarbons and sulfur-containing aromatic hydrocarbons in heavy oil aromatic hydrocarbon component

A separation method and technology for sulfur aromatic hydrocarbons, which are used in material separation, measurement devices, analysis materials, etc., can solve the problems of ineffective vaporization of gas chromatography, crossover of fractions, inaccurate quantitative results, etc., and achieve the effect of shortening separation and identification time.

Active Publication Date: 2015-02-11
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0005] Nishioka et al. (Nishioka, M., et al., Isolation of sulfur heterocycles from petroleum-and coal-derived materials by ligand exchange chromatography. Fuel, 1986.65(2): p.270-273) used palladium chloride / silica gel coordination The chromatographic separation method is used to study the sulfur compounds in coal and petroleum. This method can effectively separate the 2-6 ring condensed aromatic hydrocarbons and sulfur-containing polycyclic aromatic hydrocarbons in the aromatic components of petroleum. However, this method has the following problems : ① part of PdCl 2 -PASHs (PASH-polycyclic sulfur heterocyclic aromatic hydrocarbons) complexes will flow out with the mobile phase, and there will be cross-cutting of sulfur-containing aromatic hydrocarbons and polycyclic aromatic hydrocarbons.
[0008] However, for heavy oil samples with high sulfur content, direct use of GC / FI-TOF MS will lead to inaccurate quantitative results
Moreover, gas chromatography cannot effectively vaporize samples such as residual oil with a high boiling point.

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  • Method for separating and determining aromatic hydrocarbons and sulfur-containing aromatic hydrocarbons in heavy oil aromatic hydrocarbon component
  • Method for separating and determining aromatic hydrocarbons and sulfur-containing aromatic hydrocarbons in heavy oil aromatic hydrocarbon component

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preparation example Construction

[0015] The preparation method of the stationary phase of the present invention is as follows: calcining alumina at 400-700° C. for 3-6 hours, and if silicon dioxide is used, calcining it at 120-300° C. for 3-6 hours in advance. Dissolve palladium chloride in water at 50-90°C, then add alumina or a mixture of alumina and silica, mix well and then impregnate for 10-30 hours, the liquid / solid ratio of impregnation is 1.5-4.0mL / g, Then dry the impregnated solid at 100-300° C. for 2-5 hours.

[0016] The invention firstly separates the heavy oil, and separates the saturated hydrocarbon, aromatic hydrocarbon and colloid components therein. The heavy oil is vacuum distillate oil, atmospheric residual oil, vacuum residual oil, deasphalted oil, catalytic cracking oil slurry or hydrotreated oil.

[0017] If the heavy oil is residual oil, according to the method of "Petrochemical Analysis Methods" (Science Press, 1990: 31) edited by Yang Cuiding et al., use n-heptane to precipitate asph...

example 1

[0042] Preparation of stationary phase: γ-alumina (produced by Sinopharm Chemical Reagent Co., Ltd.) was roasted at 500 °C for 5 hours, and 0.5 g of PdCl 2 Dissolve in 20mL of water at a temperature of 80°C, add to 9.5g of calcined γ-alumina after fully dissolving, stir evenly, let stand for immersion for 24 hours, and dry at 150°C for 3 hours to obtain the stationary phase A of the present invention , where PdCl 2 The content is 5% by mass.

[0043] The method of the invention is used to carry out solid phase extraction to separate aromatics and sulfur-containing aromatics in heavy oil.

[0044] (1) Separation of aromatic components in heavy oil

[0045] Separation of aromatics in heavy oil by alumina column chromatography. Take 3g of Saudi medium vacuum wax oil and dissolve it in 50mL of n-hexane to prepare a raw material solution, and add the raw material solution to a column chromatography filled with 100g of γ-alumina. Use normal hexane, dichloromethane and benzene / et...

example 2

[0055] Preparation of stationary phase: calcination of 6g γ-alumina at 550°C for 4 hours, 3.5g of silica at 120°C for 4 hours, 0.5g of PdCl 2 Dissolve in 20mL of water at a temperature of 80°C, add to the roasted γ-alumina and silica mixture after fully dissolving, stir evenly, let it stand for immersion for 24 hours, and dry at 300°C for 5 hours to obtain the stationary phase B. where PdCl 2 The content is 5% by mass.

[0056] (1) Separation of aromatic components in heavy oil

[0057] After deasphalting the Tahe vacuum residue oil with n-heptane, use silver nitrate modified silica gel (see CN102079987A for the preparation method) as the stationary phase to separate the aromatics in the deasphalted oil by solid phase extraction. The specific operation is as follows: take 3g of raw material The deasphalted oil was dissolved in 50mL of n-hexane to prepare a raw material solution, and the raw material solution was added to a solid-phase extraction column filled with 100g of si...

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Abstract

The invention relates to a method for separating aromatic hydrocarbons and sulfur-containing aromatic hydrocarbons in a heavy oil aromatic hydrocarbon component, which comprises the following steps: separating a aromatic hydrocarbon component from heavy oil, using inertia hydrocarbon to dissolve the obtained aromatic hydrocarbon component, adding a solid phase extraction column filled with a solid phase, using a weak polar solvent to flush aromatic hydrocarbons attached on the solid phase to obtain an eluate containing aromatic hydrocarbons, using a strong polar solvent to flush the sulfur-containing aromatic hydrocarbons attached on the solid phase to obtain an eluate containing the sulfur-containing aromatic hydrocarbons, removing the solvent in the eluate to obtain the aromatic hydrocarbons component and the sulfur-containing aromatic hydrocarbons component, wherein the solid phase is a mixture of palladium chloride-supported alumina or alumina and silica, and palladium chloride content in the solid phase is 3-10mass%. The method can effectively separate aromatic hydrocarbons and sulfur-containing aromatic hydrocarbons in the heavy oil aromatic hydrocarbon component, and operation is simple, convenient and fast. The aromatic hydrocarbons component and the sulfur-containing aromatic hydrocarbons component can be used for determining the compound types and carbon number distribution by field desorption / ionization-flight time mass spectrum.

Description

technical field [0001] The invention relates to a method for extracting and separating different types of compounds in hydrocarbons and a method for determining the separated compounds, specifically, a method for separating aromatics (hydrocarbons) and sulfur-containing compounds from aromatic components by using solid-phase extraction. Methods for aromatics and methods for the determination of isolated compounds. Background technique [0002] The main types of sulfur-containing compounds in heavy oil are sulfur-containing aromatics such as benzothiophene and dibenzothiophene. Therefore, a detailed type analysis of sulfur-containing aromatics is helpful for selecting a suitable sulfur reduction process, optimizing and developing new heavy oil reduction technologies. Sulfur processing technology. [0003] So far, the characterization of the composition and distribution of sulfur compounds in heavy distillates remains a difficult problem. For the characterization of complex ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 张文刘泽龙祝馨怡王威史延强田松柏
Owner CHINA PETROLEUM & CHEM CORP
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