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Method for directly separating phenols from coal pyrolytic oil

A technology of pyrolysis of phenolic substances and coal, applied in chemical instruments and methods, preparation of organic compounds, liquid solution solvent extraction, etc., can solve the problem of low extraction rate of phenols, achieve reduced production costs, mild conditions, and avoid strong The effect of acid-base corrosion equipment and phenolic wastewater

Inactive Publication Date: 2015-02-04
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN 101143805A utilizes the mixed reaction of phenol and saturated ammonia solution, and then utilizes carbon dioxide and ammonium salt to react to form ammonium carbonate, and frees the method for crude phenol, and the extraction rate of phenol is low in this method

Method used

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  • Method for directly separating phenols from coal pyrolytic oil
  • Method for directly separating phenols from coal pyrolytic oil
  • Method for directly separating phenols from coal pyrolytic oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] m-cresol was dissolved in n-hexane to prepare model oil solution, the concentration was 200.2g / L, and the amides were nicotinamide (C 6 h 6 N 2 O), the molar ratio of nicotinamide to m-cresol is 0.4:1, the separation temperature is 30°C, and the reaction time is 30min.

[0025] At 30°C, 4.523g of nicotinamide was added to 50ml of model oil solution, stirred for 30 minutes, and left to stand for 10 minutes. The volume of the upper oil phase and the concentration of m-cresol in it were measured by GC. The removal rate of m-cresol was 92.00%. Remove the upper oil phase, add 50mL stripping agent diethyl ether into the lower eutectic phase, stir for 20min, let stand for 10min, perform suction filtration, put the solid obtained by vacuum filtration into a vacuum drying oven at 80°C for 1h, weigh and calculate the recovery rate . The above process was repeated 4 times, the removal rate of m-cresol was 95.32%, and the recovery rate of nicotinamide in 4 cycles was 90.15%.

Embodiment 2

[0027] Phenol was dissolved in n-hexane to prepare simulated oil solution, the concentration was 20.36g / L, the amide substance was urea, the molar ratio of urea to phenol was 1:1, the separation temperature was 30°C, and the stirring time was 30min.

[0028] At 30°C, 0.4680g urea was added to 30mL model oil solution, stirred for 30min and then allowed to stand for 5min to measure the volume and phenol content of the upper oil phase. After suction filtration and drying, the mass of the complex was 0.8133g, and the removal rate of phenol was 85.06 %.

[0029] Remove the upper oil phase, add 20ml of diethyl ether to the dried complex, stir for 15min and let stand for 5min, vacuum filter the obtained solid into a vacuum drying oven at 70°C for 1h, weigh and calculate the recovery. The above process was repeated three times, the removal rate of phenol was 85.00%, and the recovery rate of urea in three cycles was 85.50%.

Embodiment 3

[0031] m-cresol was dissolved in n-hexane to prepare model oil solution, the concentration was 210.0g / L, and the amides were pyrazinamide (C 5 h 5 N 3 O), the molar ratio of pyrazinamide and m-cresol is 0.5:1, the separation temperature is 35°C, and the reaction time is 40min.

[0032] At 35°C, 1.253g of nicotinamide was added to 10mL of model oil solution, stirred for 20 minutes, and left to stand for 10 minutes. The concentration of m-cresol in the upper oil phase was measured by GC, and the volume of the upper oil phase was measured. The removal rate of m-cresol was 90.01%. The upper oil phase was removed, and 20 mL of stripping agent diethyl ether was added to the lower eutectic phase, stirred for 30 min, allowed to stand for 10 min, and subjected to suction filtration, and the solid obtained by vacuum filtration was dried at 60°C for 1 h in a vacuum drying oven, and the recovery was calculated by weighing. The above process was repeated twice, the removal rate of m-cres...

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Abstract

The invention discloses a method for directly separating phenols from coal pyrolytic oil. Amide compounds are taken as extracting agents and form eutectic solvent solvents or solid complexes insoluble in the oil phases with phenols in oil, and therefore, the phenols are separated from the oil phases. Ether compounds are adopted to recycle the extracting agents by virtue of reverse extraction; the recycled extracting agents can be continuously applied to the extraction process. The phenols can be one or more of phenol, o-cresol, p-cresol, m-cresol, ethyl phenol, naphthol, butyl phenol, propyl phenol, dihydroxyl phenol and polyhydroxyl phenol; the oil includes model oil and pyrolytic oil; the concentration range of the phenols is 10-400g / L; the molar ratio of the amide compounds to the phenols is within the range of 0.1-2.0; the separation temperature ranges from 0 to 100 DEG C and the separation time ranges from 1 to 100 minutes. The removal rate of the phenols under appropriate reaction conditions is above 90%.

Description

technical field [0001] The invention relates to the field of separation of coal chemical industry and petrochemical industry, in particular to a method for separating various phenols from oil. Background technique [0002] Phenolic compounds are the basic raw materials of the chemical industry. They can be used to synthesize organic intermediates, and can also be used as important chemical raw materials for plastics, pesticides, fibers and other fields. Their main sources are coal liquefaction products, coal pyrolysis oil and petroleum products. The content of phenolic products in low-temperature coal tar is relatively high, and the total phenolic content is about 25% to 30%. It is particularly important to make full use of this part of phenolic substances. [0003] The main methods for separating phenolic substances from pyrolysis oil include chemical method, selective solvent extraction method, ion exchange resin adsorption separation method, supercritical extraction and ...

Claims

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Application Information

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IPC IPC(8): B01D11/04C07C37/72C07C39/07C07C39/04
Inventor 李春山焦甜甜庄绪磊陈洪楠张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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