Method for extracting phenolic substances from phenol-containing raw oil

A technology of phenolic substances and raw oil, applied in the field of coal chemical industry, can solve the problem of high energy consumption of extractant recovery, achieve the effects of reduced extraction rate, high solubility, and reduced consumption

Active Publication Date: 2019-05-21
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the technical problem of high energy consumption in the recovery of existing extractants, the invention provides a method for extracting phenolic substances from phenolic raw material oil, which comprises the following steps:

Method used

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  • Method for extracting phenolic substances from phenol-containing raw oil

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Comparison scheme
Effect test

Embodiment 1

[0045] Add 241.99g of ammonia solution with a concentration of 10% and 40.13g of overhead oil with a distillation range of 70-180°C and a total phenol content of 56.82% into a 500mL single-necked flask with stirring, and fully stir for 30min at normal temperature and pressure. , after liquid separation, 29.76g dephenolized oil and 251.21g phenolic-rich extract phase were obtained, and the phenolic-rich extract phase was mixed with 41.8g tower top oil to obtain 252.64g secondary phenolic-rich The extract phase of the substance and 39.43g of dephenolized oil; the phenol-containing ammonia solution is placed in a 500ml stirred flask, and 42.13g of nonylphenol is added at normal temperature and pressure for back extraction, and stirred for 20min to obtain 52.76g of The back-extraction phase rich in phenolic substances and 238.93g of ammonia-containing aqueous phase; the back-extraction phase was placed in a 150mL three-necked flask, heated to 240°C, and distilled to obtain 13.03g o...

Embodiment 2

[0047] The ammonia solution with a concentration of 10% and the overhead oil with a distillation range of 70-180°C and a total phenol content of 56.82% enter the extraction tower to separate the dephenolized oil raffinate phase and the extraction phase rich in phenolic substances. The number is 3 levels, the volume ratio of ammonia solution to tower top oil is 6:1, extraction at normal temperature and pressure, the extraction yield is 72.67%; the obtained extraction phase rich in phenolic substances is separated into the stripping tower to obtain the stripping phase And ammonia-containing aqueous solution, the number of back extraction stages is 5, the back extraction agent nonylphenol, its volume ratio to the extraction phase rich in phenolic substances is 6:1, normal temperature and pressure back extraction, the back extraction yield is 82.58% ; The back extraction phase rich in phenolic substances enters the rectification tower for separation to obtain ammonia, water, stripp...

Embodiment 3

[0049] The ammonia solution with a concentration of 10% and the overhead oil with a distillation range of 70-180°C and a total phenol content of 57.07% enter the extraction tower to separate the dephenolized oil raffinate phase and the extraction phase rich in phenolic substances. Extraction grade The number is 4 grades, the volume ratio of ammonia solution to tower top oil is 6:1, and the extraction is carried out under normal temperature and pressure, and the extraction yield is 86.86%. And ammonia-containing aqueous solution, the number of extraction stages is 7, the stripping agent nonylphenol, its volume ratio to the extraction phase rich in phenolic substances is 4:1, stripping at normal temperature and pressure, and the stripping yield is 93.84%; The back-extraction phase rich in phenolic substances enters the rectification tower to separate ammonia, water, stripping agent and crude phenol. The number of rectification stages is 10, and the vacuum is 0.07MPa. The temperat...

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Abstract

The invention provides a method for extracting phenolic substances from phenol-containing raw oil. The method comprises the following steps: 1, extracting: carrying out multistage countercurrent extraction on the phenol-containing raw oil with an aqueous solution of ammonia or an organic amine as an extractant to obtain an extract phase A and a raffinate phase B; 2, back-extracting: carrying out multistage countercurrent back-extraction on the extract phase A with nonylphenol or a high-boiling phenol, having a molecular weight greater than that of trimethylphenol, in coal tar as a back-extractant to obtain an aqueous phase C containing the extractant and a back-extraction phase D rich in phenolic substances; 3, regenerating the extractant: adding the back-extraction phase D rich in phenolic substances into an extractant recovery tower, carrying out rectification separation to obtain a water-containing extractant E at the tower top and a tower bottom liquid which is crude phenol oil F,mixing the water-containing extractant E with the aqueous phase C containing the extractant, and then returning the obtained mixture to step 1 for recycling; and 4, refining and regenerating the back-extractant: carrying out multi-time distillation separation on the coarse phenol oil F to obtain a back-extractant G and the phenolic substances, and returning the back-extractant G to step 2 for recycling.

Description

technical field [0001] The invention relates to the field of coal chemical industry, in particular to a method for extracting phenolic substances from phenolic raw material oil. Background technique [0002] Raw oils contain abundant types and considerable quantities of phenolic substances. The content and composition of phenolic substances produced by different chemical processes are quite different, but low-boiling phenols, phenols, naphthols and alkylnaphthols are the main components. part. According to the different properties of phenolic substances, various methods of extracting phenolic compounds from raw oil have been explored, mainly including chemical method, selective solvent method, supercritical extraction method and pressure crystallization method. Among them, chemical methods are widely used. Patents CN104845662A, CN102731262A, US4256568A, and US4595489A all involve chemical methods, but chemical methods all need to use acids and alkalis, which have a strong c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/72C07C39/04C07C39/07
Inventor 艾秋红黄晓平罗和安黄荣辉
Owner XIANGTAN UNIV
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