CN102336451A - Coal chemical phenol-containing waste water dephenolization method - Google Patents

Coal chemical phenol-containing waste water dephenolization method Download PDF

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Publication number
CN102336451A
CN102336451A CN2011101635770A CN201110163577A CN102336451A CN 102336451 A CN102336451 A CN 102336451A CN 2011101635770 A CN2011101635770 A CN 2011101635770A CN 201110163577 A CN201110163577 A CN 201110163577A CN 102336451 A CN102336451 A CN 102336451A
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extraction
waste water
solvent
coal chemical
tower
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CN2011101635770A
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朱艳红
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QINGDAO JUNYANG CHEMICAL TECHNOLOGY CO LTD
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QINGDAO JUNYANG CHEMICAL TECHNOLOGY CO LTD
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Publication of CN102336451A publication Critical patent/CN102336451A/en
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Abstract

The invention discloses a coal chemical phenol-containing waste water dephenolization method, which comprises the following steps of: using tert-amyl methyl ether as a main extractant, extracting the coal chemical phenol-containing waste water and the extractant in an extraction tower or a multistage mixing clarifier to obtain a solvent phase and a raffinate phase; carrying out rectification on the solvent phase, and recovering a solvent and crude phenols; distilling the raffinate phase, and recovering a residual extraction solvent; and recycling the recovered extractant. In comparison with the prior art, the method provided by the invention has advantages of simple process flow, less equipment investment, low energy consumption of solvent recovery and high phenol recovery efficiency; in addition, petroleum hydrocarbon and tar pollutants can be simultaneously and efficiently removed. By the adoption of the method, subsequent biochemical load can be more effectively mitigated so as to guarantee standard discharge or reuse of waste water.

Description

A kind of method for extracting and dephenolizing of Coal Chemical Industry phenolic wastewater
Technical field
The present invention relates to a kind of method for extracting and dephenolizing of Coal Chemical Industry phenolic wastewater, can efficiently remove and reclaim the phenols in the Coal Chemical Industry phenolic wastewater, realize the innoxious and resource utilization of such waste water.Belong to field of waste water treatment.
Background technology
In coal carbonization inferior, drying and gasification, can produce a large amount of gasification waste waters, contain the pollutents such as phenols of high density.Phenols has the thing toxicity than Johnson & Johnson, endangers greatlyyer, and simultaneously, phenols also is an important chemical material.Thereby, remove and reclaim the aldehydes matter in the coal chemical industrial waste water efficiently, not only have environment protection significance, also have the certain economic meaning.
At present, in full scale plant, liquid-liquid extraction be use the most extensively, stability and the highest dephenolize means of maturity.For coal chemical industrial waste water, extraction agent commonly used at present has DIPE, hexone, crude benzol, middle wet goods.But these extraction agents all have its open defect; Such as DIPE to the extracting power of polyphenol a little less than; Hexone energy consumption when carrying out solvent recuperation is too high, and not only percentage extraction is low for crude benzol and middle oil, and can only adopt flow process complicated, have the stripping process of secondary pollution to reclaim solvent etc.
To sum up, be badly in need of the extracting and dephenolizing technology of the Coal Chemical Industry phenolic wastewater that a kind of cost is low, flow process is simple and extraction efficiency is high at present.
Summary of the invention
To the deficiency that prior art exists, technical problem to be solved by this invention provides a kind of method for extracting and dephenolizing of Coal Chemical Industry phenolic wastewater, so as high-level efficiency, less energy-consumption coal chemical industrial waste water is carried out extracting and dephenolizing.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is: a kind of method for extracting and dephenolizing of Coal Chemical Industry phenolic wastewater, and it comprises following content:
1, is the main body extraction agent with methyl-tert the eleventh of the twelve Earthly Branches base ether, will contains phenol coal chemical industrial waste water and extraction agent and formerly will contain phenol coal chemical industrial waste water and extraction agent and in extraction tower or multistage mixer-settlers, extract, obtain solvent phase and the surplus water of collection.
2,, reclaim solvent and crude phenols then with solvent phase rectifying; The rectification process condition is: rectifying tower theoretical stage 15-25 level, and reflux ratio 0.1-1, working pressure 0.01-0.11MPa, the cat head service temperature is 25-90 ℃, column bottom temperature is 105-210 ℃.
3, residual extraction solvent is reclaimed in the surplus water distillation of will coming together, and the processing condition of distillating recovering solvent are: tower top temperature 72-80 ℃, and column bottom temperature 95-110 ℃; Cat head steams the 1.5-5% that inventory is charging.
4, the extraction agent that step 2 and 3 is reclaimed recycles.
The method for extracting and dephenolizing of above-mentioned Coal Chemical Industry phenolic wastewater, its extraction temperature are 30-70 ℃, extraction pH3-9.5, and extraction solvent is 1 with the volume ratio that contains the phenol coal chemical industrial waste water: 20-1: 1, extraction theory progression is the 1-10 level.If PH is low excessively, then serious to equipment corrosion,, then, phenols degree of ionization in water cause percentage extraction to reduce owing to improving if pH is too high.Optimum extraction pH is 5-8.
The method for extracting and dephenolizing of above-mentioned Coal Chemical Industry phenolic wastewater when its used extraction equipment is extraction tower, pumps into waste water and extraction agent in the extraction tower from the top and the bottom of extraction tower respectively, carries out counter-current extraction, obtains solvent phase and the surplus water of collection; When used extraction equipment was mixer-settlers, waste water and extraction agent added from the first step and last step mixer-settlers respectively.
Method of the present invention compared with prior art, its technical process is simple, facility investment is few, the solvent recuperation energy consumption is low, the organic efficiency of phenol is high, and can efficiently remove petroleum hydrocarbon, tar pollutant simultaneously.Adopt the present invention can more effectively alleviate the load of follow-up biochemical section, guarantee standard wastewater discharge or reuse.
Embodiment
Below in conjunction with embodiment to further explain of the present invention.
The present invention adopts the extraction agent that is the main body with methyl-tert the eleventh of the twelve Earthly Branches base ether; To contain phenol coal chemical industrial waste water and extraction agent earlier extracts in extraction tower or multistage mixer-settlers; Obtain solvent phase and the surplus water of collection, then with solvent phase with the rectifying mode reclaim solvent and crude phenols, the surplus water of will coming together crosses the distillation mode and reclaims residual extraction solvent.The extraction agent that reclaims recycles.Extraction temperature is 30-70 ℃, extraction pH 3-9.5, and extraction solvent is 1 with the volume ratio that contains the phenol coal chemical industrial waste water: 20-1: 1, extraction theory progression is the 1-10 level.
Embodiment 1
One cover processing power is the coal gasification waste water treatment unit of 80 tons of/hour waste water, and total phenol content is 6200mg/L, and pH 7.0, and COD 25000mg/L. adopts the method for the invention, and extraction agent is selected methyl-tert the eleventh of the twelve Earthly Branches base ether for use, and extraction equipment is an extraction tower.Waste water and extraction agent are pumped in the extraction tower from the top and the bottom of extraction tower respectively, carry out counter-current extraction, obtain solvent phase and the surplus water of collection, extraction temperature is 50 ℃, extraction pH 5.0, and the volume ratio of extraction agent and phenolic wastewater is 1: 7, extraction progression is 4 grades.
Then with solvent phase with the rectifying mode reclaim solvent and crude phenols, the surplus water of will coming together crosses the distillation mode and reclaims residual extraction solvent.The rectification process condition is: rectifying tower theoretical stage 15-25 level, and reflux ratio 0.1-1, working pressure 0.01-0.11MPa, the cat head service temperature is 25-90 ℃, column bottom temperature is 105-210 ℃; The surplus water that will come together distills, and reclaims residual extraction solvent, and the processing condition of distillating recovering solvent are: tower top temperature 72-80 ℃, and column bottom temperature 95-110 ℃; Cat head steams the 1.5-5% that inventory is charging.
The extraction agent that reclaims recycles.
Total phenol content in the processed waste water is less than 300mg/L, and COD is less than 3500mg/L.
Embodiment 2
One cover processing power is the coal gasification waste water treatment unit of 130 tons of/hour waste water, and total phenol content is 5900mg/L, and pH 8.0; COD 22000mg/L; Adopt the method for the invention, extraction agent is selected methyl-tert the eleventh of the twelve Earthly Branches base ether for use, and extraction equipment is the placed in-line mixer-settlers of level Four.Waste water and extraction agent are added from the first step and last step mixer-settlers respectively, obtain solvent phase and the surplus water of collection, extraction temperature is 55 ℃, extraction pH 8.0, and the volume ratio of extraction agent and phenolic wastewater is 1: 8, extraction progression is 6 grades.Then with solvent phase with the rectifying mode reclaim solvent and crude phenols, the surplus water of will coming together crosses the distillation mode and reclaims residual extraction solvent, its processing condition are with embodiment 1.The extraction agent that reclaims recycles.
Total phenol content in the processed waste water is about 450mg/L, the about 4000mg/L of COD.
Embodiment 3
One cover processing power is the coal gasification waste water treatment unit of 300 tons of/hour waste water, and total phenol content is 7600mg/L, and pH 6.5, and COD 19000mg/L adopts the method for the invention, and extraction agent is selected methyl-tert the eleventh of the twelve Earthly Branches base ether for use, and extraction equipment is an extraction tower.Waste water and extraction agent are pumped in the extraction tower from the top and the bottom of extraction tower respectively, carry out counter-current extraction, obtain solvent phase and the surplus water of collection, extraction temperature is 30 ℃, extraction pH3, and the volume ratio of extraction agent and phenolic wastewater is 1: 20, extraction progression is 1 grade.Then with solvent phase with the rectifying mode reclaim solvent and crude phenols, the surplus water of will coming together crosses the distillation mode and reclaims residual extraction solvent, its processing condition are with embodiment 1.The extraction agent that reclaims recycles.
Total phenol content in the processed waste water is about 280mg/L, the about 3000mg/L of COD.
Embodiment 4
One cover processing power is the coal gasification waste water treatment unit of 130 tons of/hour waste water, and total phenol content is 5900mg/L, and pH 8.0; COD 22000mg/L; Adopt the method for the invention, extraction agent is selected methyl-tert the eleventh of the twelve Earthly Branches base ether for use, and extraction equipment is the placed in-line mixer-settlers of level Four.Waste water and extraction agent are added from the first step and last step mixer-settlers respectively, obtain solvent phase and the surplus water of collection, extraction temperature is 70 ℃, extraction pH 9.5, and the volume ratio of extraction agent and phenolic wastewater is 1: 1, extraction progression is 10 grades.Then with solvent phase with the rectifying mode reclaim solvent and crude phenols, the surplus water of will coming together crosses the distillation mode and reclaims residual extraction solvent, its processing condition are with embodiment 1.The extraction agent that reclaims recycles.
Total phenol content in the processed waste water is about 450mg/L, the about 4000mg/L of COD.

Claims (4)

1. the method for extracting and dephenolizing of a Coal Chemical Industry phenolic wastewater is characterized in that, it comprises following content:
A, be the main body extraction agent, will contain phenol coal chemical industrial waste water and extraction agent and formerly will contain phenol coal chemical industrial waste water and extraction agent and in extraction tower or multistage mixer-settlers, extract, obtain solvent phase and the surplus water of collection with methyl-tert the eleventh of the twelve Earthly Branches base ether;
B, then with solvent phase rectifying, reclaim solvent and crude phenols; Its rectification process condition is: rectifying tower theoretical stage 15-25 level, and reflux ratio 0.1-1, working pressure 0.01-0.11MPa, the cat head service temperature is 25-90 ℃, column bottom temperature is 105-210 ℃;
Residual extraction solvent is reclaimed in c, the surplus water distillation of will coming together; The processing condition of its distillating recovering solvent are: tower top temperature 72-80 ℃, and column bottom temperature 95-110 ℃; Cat head steams the 1.5-5% that inventory is about charging;
The extraction agent that d, step b and c reclaim recycles.
2. method for extracting and dephenolizing according to claim 1 is characterized in that, when its used extraction equipment is extraction tower, waste water and extraction agent is pumped in the extraction tower from the top and the bottom of extraction tower respectively, carries out counter-current extraction, obtains solvent phase and the surplus water of collection; When used extraction equipment was mixer-settlers, waste water and extraction agent added from the first step and last step mixer-settlers respectively.
3. method for extracting and dephenolizing according to claim 1 is characterized in that, its extraction temperature is 30-70 ℃, extraction pH 3-9.5, and extraction solvent is 1 with the volume ratio that contains the phenol coal chemical industrial waste water: 20-1: 1, the theoretical stage of extraction is the 1-10 level.
4. method for extracting and dephenolizing according to claim 3 is characterized in that, its extraction pH is 5-8.
CN2011101635770A 2011-06-17 2011-06-17 Coal chemical phenol-containing waste water dephenolization method Pending CN102336451A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102659204A (en) * 2012-05-11 2012-09-12 青岛科技大学 Method for treating waste water in coal chemical industry
CN102674609A (en) * 2012-05-11 2012-09-19 华南理工大学 Separation treatment method for waste water in coal tar machining process
CN102674608A (en) * 2012-05-11 2012-09-19 华南理工大学 Method for recycling and treating high-concentration phenol/ammonia wastewater
CN103818982A (en) * 2014-03-13 2014-05-28 中钢集团鞍山热能研究院有限公司 Centrifugal extracting wastewater dephenolization technology
CN104528862A (en) * 2014-12-25 2015-04-22 天津大学 Phenolic wastewater treatment device and method
CN104909421A (en) * 2015-06-08 2015-09-16 华南理工大学 Treatment method of high-concentration phenolic wastewater generated in lignite upgrading process
CN105461001A (en) * 2014-08-21 2016-04-06 辽宁大唐国际阜新煤制天然气有限责任公司 Method and apparatus for treating coal gasification wastewater containing high concentration phenols, and use of extractant
CN106698776A (en) * 2015-08-26 2017-05-24 盐城市瓯华化学工业有限公司 Dephenolizing method for phenol-containing wastewater
CN111039486A (en) * 2019-12-30 2020-04-21 江西兄弟医药有限公司 Method for treating o-ethoxyphenol production wastewater
CN116514209A (en) * 2023-05-23 2023-08-01 中关村至臻环保股份有限公司 Emulsion liquid film extractant for removing phenolic pollutants in wastewater and preparation method and application device thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102659204A (en) * 2012-05-11 2012-09-12 青岛科技大学 Method for treating waste water in coal chemical industry
CN102674609A (en) * 2012-05-11 2012-09-19 华南理工大学 Separation treatment method for waste water in coal tar machining process
CN102674608A (en) * 2012-05-11 2012-09-19 华南理工大学 Method for recycling and treating high-concentration phenol/ammonia wastewater
CN103818982A (en) * 2014-03-13 2014-05-28 中钢集团鞍山热能研究院有限公司 Centrifugal extracting wastewater dephenolization technology
CN105461001A (en) * 2014-08-21 2016-04-06 辽宁大唐国际阜新煤制天然气有限责任公司 Method and apparatus for treating coal gasification wastewater containing high concentration phenols, and use of extractant
CN104528862A (en) * 2014-12-25 2015-04-22 天津大学 Phenolic wastewater treatment device and method
CN104909421A (en) * 2015-06-08 2015-09-16 华南理工大学 Treatment method of high-concentration phenolic wastewater generated in lignite upgrading process
CN106698776A (en) * 2015-08-26 2017-05-24 盐城市瓯华化学工业有限公司 Dephenolizing method for phenol-containing wastewater
CN111039486A (en) * 2019-12-30 2020-04-21 江西兄弟医药有限公司 Method for treating o-ethoxyphenol production wastewater
CN116514209A (en) * 2023-05-23 2023-08-01 中关村至臻环保股份有限公司 Emulsion liquid film extractant for removing phenolic pollutants in wastewater and preparation method and application device thereof
CN116514209B (en) * 2023-05-23 2024-03-29 中关村至臻环保股份有限公司 Emulsion liquid film extractant for removing phenolic pollutants in wastewater and preparation method and application device thereof

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Application publication date: 20120201