Separation and Characterization Method, Two-dimensional Liquid Chromatography and Device of Heavy Oil Aromatic Components

A technology of two-dimensional liquid chromatography and separation method, which is applied in the field of separation and characterization of heavy oil aromatic components, two-dimensional liquid chromatography and devices, and can solve the problems of slow data processing speed, large amount of calculation, complicated operation, etc., and achieve Improve data processing speed, high degree of automation, and good repeatability

Active Publication Date: 2021-12-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN102428059A discloses a method for separating saturated hydrocarbons, aromatics, sulfides and polar substances in heavy oil by multidimensional liquid chromatography, but the method is complicated to operate and has cumbersome steps, and due to the limitation of the liquid chromatography itself, there is a lack of detection Efficient molecular-level characterization of separated components and therefore not widely used
This method is relatively straightforward to implement and does not require too much manual intervention, but it has a large amount of calculation and slow data processing speed.

Method used

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  • Separation and Characterization Method, Two-dimensional Liquid Chromatography and Device of Heavy Oil Aromatic Components
  • Separation and Characterization Method, Two-dimensional Liquid Chromatography and Device of Heavy Oil Aromatic Components
  • Separation and Characterization Method, Two-dimensional Liquid Chromatography and Device of Heavy Oil Aromatic Components

Examples

Experimental program
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Embodiment 1

[0116] This example is used to illustrate the effect of using two-dimensional liquid chromatography to separate the aromatic components of medium-weight vacuum gas oil in Saudi Arabia.

[0117] First, solid-phase extraction was used to separate the heavy oil aromatic components in Saudi medium vacuum gas oil. Take 0.1g of Saudi Arabian medium-weight vacuum wax oil (see Table 3 for properties), dissolve it in 2mL of n-hexane, and then pour it into a solid-phase extraction column with silica gel and alumina packing as the stationary phase in a mixing volume ratio of 7:3 Above, wash the solid-phase extraction column with n-hexane, dichloromethane and dichloromethane-ethanol solution with a mixing volume ratio of 1:1 in sequence. The solvent in the desorption liquid is evaporated to dryness to obtain separated saturated hydrocarbon components, heavy oil aromatic components and colloidal components in sequence. The distillation range of the heavy oil aromatic components is 350-540°...

Embodiment 2

[0124] The characterization method of the high-resolution mass spectrum of the present invention is described.

[0125] (1) High-resolution mass spectrometry characterization conditions for aromatic components

[0126] Take 10 mg of the light component aromatics separated in Example 1 and dissolve them in 1 mL of chromatographically pure toluene to prepare a mother liquor. Dilute to 0.2 mg / mL with chromatographically pure toluene to obtain a sample solution to be tested, and use 15T SolariX FT-ICR MS from Bruker Dalton Company to test, and the test conditions are the same as in Example 1.

[0127] (2) List A of mass spectrometry data obtained from high-resolution mass spectrometry characterization of light aromatics

[0128] According to the light component aromatics high-resolution mass spectrogram (see Figure 4 ) had a total of 7488 mass spectral peaks with a signal-to-noise ratio (S / N) higher than 5.5. The data processing software that comes with the instrument can give...

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Abstract

The invention relates to a separation and characterization method, two-dimensional liquid chromatography and device of heavy oil aromatic components. The separation method comprises: dissolving the heavy oil aromatic components and injecting samples into the coordination exchange column of two-dimensional liquid chromatography In; the two-dimensional liquid chromatography also includes a normal phase chromatographic column positioned downstream of the coordination exchange chromatographic column; the first mobile phase is used to wash the first stationary phase of the coordination exchange chromatographic column and the second stationary phase of the normal phase chromatographic column in sequence , then cut out the coordination exchange chromatography column, and continue to use the first mobile phase to wash the second stationary phase; cut in the coordination exchange chromatography column, and cut out the normal phase chromatography column, and use the second mobile phase to flush the enriched sulfur-containing The first stationary phase for aromatic hydrocarbons. The separation method of the present invention can efficiently separate light aromatic components, medium aromatic components, heavy aromatic components and sulfur-containing aromatic components in heavy oil aromatic components, and the characterization method and device of the present invention have high speed and high degree of automation.

Description

technical field [0001] The invention relates to a separation and characterization method, a two-dimensional liquid chromatography and a device for heavy oil aromatic components. Background technique [0002] Polycyclic aromatic hydrocarbons and sulfur-containing aromatic hydrocarbons are the most difficult components to remove in heavy oil hydrodearomatization and hydrodesulfurization processes, especially dibenzothiophene and its alkyl substitutes with large steric hindrance, even in harsh Under hydrogenation conditions, a considerable part still exists in the hydrogenation product. Therefore, deepening the molecular level understanding of polycyclic aromatic hydrocarbons and sulfur-containing aromatic hydrocarbons in heavy distillate oil has important theoretical guiding significance and practical value for selecting a suitable dearomatization and desulfurization process, optimizing and developing new heavy oil processing technology. [0003] With the rise of the concept ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/26G01N27/62G01N30/88G01N27/64
CPCB01D15/265G01N30/88G01N27/62
Inventor 宋春侠王威刘泽龙刘颖荣蔡新恒
Owner CHINA PETROLEUM & CHEM CORP
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