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Separation method of sulfurized alkylphenol

A technology of sulfurized alkyl phenol and separation method, which is applied in the preparation of test samples, etc., to achieve the effect of strong versatility

Inactive Publication Date: 2014-01-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for separating sulfurized alkylphenols in order to overcome the defect that the existing separation of sulfurized alkylphenols can only aim at the defect of calcium sulfurized alkylphenols in a single additive raw material

Method used

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  • Separation method of sulfurized alkylphenol
  • Separation method of sulfurized alkylphenol
  • Separation method of sulfurized alkylphenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Step 1: Accurately weigh 8g of composite additive A and place it in a rubber film, then fix it in a Soxhlet extractor, add two-thirds of petroleum ether with a boiling range of 60-90°C into the extraction bottle, heat and reflux until it seeps The solution was colorless, and the solvent was evaporated to dryness to obtain the membrane inner substance and the outer membrane substance respectively.

[0038] Step 2: Accurately weigh 2g of the film contents, and use petroleum ether as the shower agent to perform column chromatography on a silica gel column. The specific experimental conditions are as follows:

[0039] Adsorbent: 120g of silica gel for column chromatography, activated at 120°C; adsorption column: 130cm×1.5cm; rinse agent: 200ml of petroleum ether with a boiling range of 60-90°C. The solution obtained after column chromatography was evaporated to dryness to obtain column chromatography fraction 1.

[0040] Step 3: Acidification of column chromatography compo...

Embodiment 2

[0049]Step 1: Accurately weigh 8g of composite additive B and place it in a rubber film, then fix it in a Soxhlet extractor, add two-thirds of the petroleum ether with a boiling range of 60-90°C into the extraction bottle, heat and reflux until it seeps The solution was colorless, and the solvent was evaporated to dryness to obtain the membrane inner substance and the outer membrane substance respectively.

[0050] Step 2: Accurately weigh 2g of the film contents, and use petroleum ether as the shower agent to perform column chromatography on a silica gel column. The specific experimental conditions are as follows:

[0051] Adsorbent: 120g of silica gel for column chromatography, activated at 120°C; adsorption column: 130cm×1.5cm; rinse agent: 200ml of petroleum ether with a boiling range of 60-90°C. The solution obtained after column chromatography was evaporated to dryness to obtain column chromatography fraction 1.

[0052] Step 3: Acidification of column chromatography co...

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Abstract

The invention discloses a separation method of sulfurized alkylphenol. The separation method comprises following steps: (1) thin film dialysis, wherein a lubricating oil composite additive encapsuled in a thin film is added into petroleum ether, the mixture is subjected to heating reflux so as to obtain a product encapsuled in the thin film; (2) the product encapsuled in the thin film is subjected to column chromatography, and eluent is collected and is dried by distillation so as to obtain compound 1, wherein activated silica gel is used as adsorbent, and petroleum ether is used as eluent; (3) diethyl ether solution of the compound 1 is hydrolyzed in hydrochloric acid so as to obtain an acidized product; and (4) the acidized product obtained in step (3) is subjected to column chromatography, and ethyl acetate and petroleum ether mixed eluent is collected, wherein activated silica gel is used as adsorbent, and petroleum ether, and a mixture of ethyl acetate and petroleum ether are used as eluent successively. The separation method is suitable for lubricating oil composite additives, and possesses relatively high versatility.

Description

technical field [0001] The invention relates to the field of substance separation and detection, in particular to a method for separating sulfurized alkylphenols. Background technique [0002] The main function of marine cylinder oil is to ensure the lubrication between the piston, piston ring and piston bushing in the marine diesel engine cylinder. The problems to be solved and the functions to be played determine that it must have some specific properties. Among these properties, high temperature Detergency and acid neutralization properties are especially important. Therefore, the compound additive used to blend cylinder oil must contain detergent. Sulfurized calcium alkyl phenate is widely used in marine cylinder oil compound additives because of its excellent high-temperature detergency and acid neutralization ability. In addition, sulfurized calcium alkyl phenate has good anti-oxidation and anti-corrosion properties. And its acid neutralization rate has obvious advan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34
Inventor 李少萍彭来刘扬扬金球林孙杨常俊辉吴玉
Owner EAST CHINA UNIV OF SCI & TECH
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