Sulfonation method and analysis method for aromatic hydrocarbon compounds in petroleum products
A technology for aromatic hydrocarbons and compounds, applied in the field of petroleum composition analysis, can solve problems such as poor selectivity, excessive sulfonation of aromatic hydrocarbons, and affecting the accuracy of quantitative analysis data, etc.
Pending Publication Date: 2022-02-25
CHINA UNIV OF PETROLEUM (BEIJING)
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Problems solved by technology
The traditional sulfonation reaction uses sulfur trioxide as the sulfonating agent, the reaction conversion rate is high, but the selectivity is poor, and some cycloalkanes undergo sulfonation reaction, which makes the mass spectrometry analysis results unresolved
Compared with sulfur trioxide, chlorosulfonic acid shows good selectivity for aromatics, but the side reaction is difficult to suppress, resulting in excessive sulfonation of some aromatics, which seriously affects the accuracy of quantitative analysis data
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Embodiment 1
[0098] This embodiment provides a method for the sulfonation of aromatic hydrocarbons in vacuum distillate oil, the process of which is as follows figure 1 As shown, the method includes the following steps:
[0099] Preparation of solid-phase extraction column: Take 20 grams of chromatographic silica gel and pour it into a 500-ml beaker, add 100 ml of dichloromethane, and stir; then slowly add 20 grams of chlorosulfonic acid dropwise under stirring conditions, and stir for 2 hours; The product obtained by the reaction was transferred to a rotary evaporator to remove the solvent, and then the product after the solvent removal was transferred to a beaker and heated in an oven at 175°C for 8 hours; then the beaker was taken out and naturally cooled to room temperature to obtain silica gel sulfonic acid; take 1.25 grams Silica gel sulfonic acid and 0.15 grams of 100 mesh anhydrous sodium sulfate particles are evenly mixed, and packed into a 6 ml solid phase extraction column to co...
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The invention provides a sulfonation method and an analysis method for aromatic hydrocarbon compounds in petroleum products. The sulfonation method comprises the following steps: reacting chromatographic silica gel with chlorosulfonic acid in an organic solvent A to obtain silica gel sulfonic acid, and mixing the silica gel sulfonic acid with anhydrous sodium sulfate to prepare a solid-phase extraction column; adding a to-be-analyzed petroleum product into the solid-phase extraction column, and carrying out sulfonation reaction on the petroleum product entering the solid-phase extraction column in an organic solvent B environment by virtue of the solid-phase extraction column. The analysis method comprises the following steps: reacting chromatographic silica gel with chlorosulfonic acid in an organic solvent A to obtain silica gel sulfonic acid, and mixing the silica gel sulfonic acid with anhydrous sodium sulfate to prepare a solid-phase extraction column; adding a to-be-analyzed petroleum product into the solid-phase extraction column, and carrying out sulfonation reaction on the petroleum product entering the solid-phase extraction column in an organic solvent B environment by virtue of the solid-phase extraction column; extracting a sulfonated product from the solid-phase extraction column; representing the molecular composition of the sulfonated product by an electrospray ionization mass spectrometer, and then analyzing the aromatic hydrocarbon compounds in the to-be-analyzed petroleum product sample are analyzed.
Description
technical field [0001] The invention belongs to the technical field of petroleum composition analysis, in particular to a sulfonation method and analysis method of aromatic hydrocarbon compounds in petroleum oil products. Background technique [0002] Electrospray ionization technology combined with high-resolution mass spectrometry has realized the molecular composition analysis of polar compounds in petroleum, but it is difficult for electrospray technology to directly ionize hydrocarbon compounds. Although aromatic hydrocarbons can be detected by atmospheric pressure photoionization technology, the ionization efficiency of aromatic hydrocarbons with different condensation degrees varies greatly, making quantitative analysis impossible. To solve the problem of mass spectrometry analysis of aromatic hydrocarbons, the molecular composition of aromatic hydrocarbons can be analyzed by electrospray mass spectrometry by converting aromatic hydrocarbons into sulfonates. Since su...
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Patent Timeline
Login to View More IPC IPC(8): G01N27/62G01N1/28C07C303/08C07C309/30
CPCG01N27/62G01N1/28C07C303/08C07C309/30
Inventor 史权李硕凡周麒麟李海栋吴建勋张亚和梁咏梅
Owner CHINA UNIV OF PETROLEUM (BEIJING)