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Separation and characterization methods for heavy oil aromatic hydrocarbon components, two-dimensional liquid chromatography, and device

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 equipment, and can solve problems such as complex operation, cumbersome steps, and large amount of calculation

Active Publication Date: 2020-03-10
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 methods for heavy oil aromatic hydrocarbon components, two-dimensional liquid chromatography, and device
  • Separation and characterization methods for heavy oil aromatic hydrocarbon components, two-dimensional liquid chromatography, and device
  • Separation and characterization methods for heavy oil aromatic hydrocarbon components, two-dimensional liquid chromatography, and device

Examples

Experimental program
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Effect test

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 separation and characterization methods for heavy oil aromatic hydrocarbon components, two-dimensional liquid chromatography, and a device. The separation method includes: 1)dissolving the aromatic hydrocarbon components, and loading the sample to a coordination exchange chromatographic column of the two-dimensional liquid chromatography, the two-dimensional liquid chromatography further including a normal-phase chromatographic column at the downstream of the coordination exchange chromatographic column; 2) successively washing a first stationary phase of the coordination exchange chromatographic column and a second stationary phase of the normal-phase chromatographic column by means of a first moving phase, and bypassing the coordination exchange chromatographiccolumn, continuously washing the second stationary phase by means of the moving phase; 3) connecting the coordination exchange chromatographic column and bypassing the normal-phase chromatographic column, and washing the first stationary phase, in which sulfur-containing aromatic hydrocarbon, by using a second moving phase. By means of the separation method, light aromatic hydrocarbon components,medium aromatic hydrocarbon components, heavy aromatic hydrocarbon components and sulfur-containing aromatic hydrocarbons in heavy oil aromatic hydrocarbon components are separated high-effectively. The characterization method and device are high in speed and are high in automation degree.

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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IPC IPC(8): B01D15/26G01N27/62G01N30/88
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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