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A method for extracting phenolic compounds from phenolic oil with inner salt

A technology for phenolic compounds and phenolic oils, applied in the field of extraction of phenolic compounds, can solve the problems of loss of halogen anions, influence of the efficiency of oil hydrogenation catalysts, etc., and achieve the effects of avoiding acid-base solutions, reducing equipment requirements and production costs

Active Publication Date: 2019-06-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This extraction method may cause the loss of halogen anions, which will adversely affect the subsequent treatment (such as hydrotreatment) of the dephenolized oil, such as the corrosion of equipment by halogens, which may affect the efficiency of oil hydrogenation catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 10.0g of phenol, dissolve it in the toluene solution in a beaker, and then prepare a toluene solution with a phenol concentration of 100g / L in a volumetric flask. Take 10 mL of the solution and add 1.03 g of L-carnitine (the molar ratio of L-carnitine to phenol is 0.6), stir at 25° C. for 2 min, and let stand for 30 min. The deep eutectic solvent formed by L-carnitine and phenol is separated from the oil phase. Get 0.2mL upper layer oil phase with pipette gun, adopt gas chromatography to analyze the concentration of phenol to be 30.2g / L, measure the volume of upper layer oil phase with graduated cylinder, calculate the removal rate of phenol to be 72.6%. The above-mentioned gas chromatographic analysis conditions for phenol concentration are as follows: the gas chromatograph used is Shimadzu 2014 gas chromatograph, the gas chromatograph adopts FID detector, and the separation column is capillary column RTX-5 (30m * 0.25mm * 0.25 μm), the carrier gas is nitrogen. ...

Embodiment 2

[0025] Weigh 10.0g of phenol, dissolve it in the toluene solution in a beaker, and then prepare a toluene solution with a phenol concentration of 100g / L in a volumetric flask. Take 10 mL of the solution and add 1.03 g of L-carnitine (the molar ratio of L-carnitine to phenol is 0.6), stir at 25°C for 15 min, and let stand for 30 min. The deep eutectic solvent formed by L-carnitine and phenol is separated from the oil phase. Take 0.2mL upper layer oil phase with pipette gun, adopt gas chromatography to analyze the concentration of phenol to be 14g / L, measure the volume of upper layer oil phase with graduated cylinder, calculate the removal rate of phenol to be 88.0%. Refer to Example 1 for the analysis method of phenol concentration.

Embodiment 3

[0027] Weigh 10.0g of phenol, dissolve it in the toluene solution in a beaker, and then prepare a toluene solution with a phenol concentration of 100g / L in a volumetric flask. Take 10 mL of the solution and add 1.03 g of L-carnitine (the molar ratio of L-carnitine to phenol is 0.6), stir at 35°C for 15 min, and let stand for 30 min. The deep eutectic solvent formed by L-carnitine and phenol is separated from the oil phase. Get 0.2mL upper layer oil phase with pipette gun, adopt gas chromatography to analyze the concentration of phenol to be 16.0g / L, measure the volume of upper layer oil phase with graduated cylinder, calculate the removal rate of phenol to be 86.6%. Refer to Example 1 for the analysis method of phenol concentration.

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Abstract

The invention relates to a method for separating a phenolic compound from phenol-containing oil. The method comprises the following steps of adding an inner-salt extracting agent containing acid radicals into oil containing the phenolic compound, agitating an obtained first mixture, making the inner salt and the phenolic compound in the oil form a eutectic solvent phase which is not intermiscible with an oil phase, and realizing the separation between the phenolic compound and the oil; collecting a eutectic solvent, reducing pressure to remove a small quantity of neutral oil entrained in the eutectic solvent, adding a stripping agent into the eutectic solvent, agitating an obtained second mixture, dissolving the phenolic compound in the stripping agent, and separating the inner-salt extracting agent out in a solid manner; distilling a stripping agent solution containing the phenolic compound, so as to obtain the phenolic compound and the stripping agent. In a separation process, the extracting agent and the stripping agent can be recycled. The extracting agent used in the method is nontoxic and environment-friendly; by using the method, the use of large amount of acidic and alkaline solutions and the generation of phenol-containing wastewater in a conventional alkaline washing method are avoided; no halide ion is introduced in an extraction process; the method is an economical and environment-friendly method for extracting the phenolic compound from the phenol-containing oil.

Description

technical field [0001] The invention relates to a method for extracting phenolic compounds from phenolic oil by using internal salt as an extractant. Background technique [0002] Phenolic compounds are important chemical basic raw materials, widely used in synthetic fibers, pesticides, medicine, explosives and other fields, and have a large market demand. Coal tar, coal direct liquid oil and biomass pyrolysis oil all contain a large amount of phenolic compounds. Proposing the phenolic compounds in these oils can not only obtain high value-added phenolic compounds, but also reduce the problems in the subsequent treatment of these oils, such as instability (storage), high hydrogen consumption (hydrogenation processing), etc. [0003] At present, the industrial separation of phenolic compounds from phenolic oils is the alkaline washing method. The principle of the alkali washing method is to use the weak acidity of the phenolic compound to add an alkaline solution to neutra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/68C07C37/72C07C39/04
CPCC07C37/685C07C37/72C07C39/04
Inventor 吴卫泽么聪菲任树行
Owner BEIJING UNIV OF CHEM TECH