CN101913737A - Method for treating etherifying phenol-contained wastewater - Google Patents

Method for treating etherifying phenol-contained wastewater Download PDF

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Publication number
CN101913737A
CN101913737A CN 201010260508 CN201010260508A CN101913737A CN 101913737 A CN101913737 A CN 101913737A CN 201010260508 CN201010260508 CN 201010260508 CN 201010260508 A CN201010260508 A CN 201010260508A CN 101913737 A CN101913737 A CN 101913737A
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phenol
contained wastewater
etherifying
treating
etherifying phenol
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CN101913737B (en
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易江华
阮文林
毕亚铃
章传力
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JIANGSU EQUALCHEM CO Ltd
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JIANGSU EQUALCHEM CO Ltd
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Abstract

The invention discloses a method for treating etherifying phenol-contained wastewater. By compounding an efficient complex extracting agent-PN on the basis of high-concentration phenol-contained wastewater generated by etherification reaction carried out by adopting 2,4-dichlorophenol and 2,5-dichloronitrobenzene as raw materials on the production line of triclosan, the volatile phenol and the chemical oxygen demand of the etherifying phenol-contained wastewater are effectively reduced; meanwhile, after an extracted phenol substance in the complex extracting agent-PN can be recycled to the production line for recycling after back extracted, thereby achieving the aims of reducing the production cost and comprehensively utilizing resources.

Description

Method for treating etherifying phenol-contained wastewater
Technical field
The present invention relates to a kind of processing method of industrial waste water, what be specifically related to is a kind of method for treating etherifying phenol-contained wastewater of triclosan.
Background technology
Triclosan is as the high-efficiency broad spectrum antiseptic-germicide, it all has gram-positive microorganism, negative bacterium, yeast and virus kills and restraining effect widely, be widely used in the household chemicals field such as cream frost, shampoo of disinfection hand cleanser, sanitary lotion, Antibacterial soaps, personal care, also be used for the rotproofing of the arrangement of hygiene tissue and paper pulp, polymkeric substance.Highly purified trichlorine is survived and is used for preventing the specific medicament toothpaste of stomatopathy, and itself and fluorochemical are used, and have the Synergistic slow release effect.
The main synthetic method of triclosan is with 2,4-chlorophenesic acid and 2,5-dichloro nitre benzene is that raw material carries out etherificate, reduction, diazotization, hydrolysis reaction, distillation, refining obtaining, whole production line mainly produces high-concentration waste water in the etherification reaction process, adopt non-extraction process to handle this waste water, be difficult to reach emission request.Triclosan etherification reaction equation is:
Summary of the invention
Goal of the invention: the present invention provides a kind of method for treating etherifying phenol-contained wastewater in order to solve the deficiencies in the prior art.
Technical scheme: a kind of method for treating etherifying phenol-contained wastewater may further comprise the steps:
1) is mixed with complexing extractant-PN with aviation kerosene, isobutyl ketone, n-Octanol and N,N-dimethylacetamide;
2) the pH value of the described etherifying phenol-contained wastewater of adjusting is 2-3;
3) described acidifying etherifying phenol-contained wastewater extracts with described complexing extractant-PN in the time of 30 ℃-50 ℃, stirs, and layering is regulated waste water ph to 6-9, carries out treating processess such as biochemistry then, qualified discharge, and described etherifying phenol-contained wastewater treating processes is finished;
4) stripped described complexing extractant-PN dissolves with alkali lye, the sodium phenolate that forms is dissolved in alkali lye, separates with described complexing extractant-PN, and described complexing extractant-PN proceeds extraction, described alkali lye carries out the triclosan etherification reaction, thereby realizes the resource circulation utilization.
As optimization, in above-mentioned steps 1) in, described complexing extractant-PN comprises following component by mass percent: aviation kerosene 60%-80%, diisobutyl ketone 1%-10%, N,N-dimethylacetamide 1%-10% and n-Octanol 15%-20%.
As optimization, in above-mentioned steps 2) in, the pH value that adopts hydrochloric acid to regulate described etherifying phenol-contained wastewater.
As optimization, in above-mentioned steps 3) in, described extraction churning time is 1 hour.
As optimization, in above-mentioned steps 4) in, described alkali lye is mass percent 10%-30% sodium hydroxide solution.
The present invention is about a kind of method for treating etherifying phenol-contained wastewater, be based on the triclosan production line with 2,4-chlorophenesic acid and 2,5-dichloro nitre benzene is the high-concentration phenolic wastewater that etherification reaction produced that raw material carries out, volatile phenol concentration reaches 6000mg/L, chemical oxygen demand (COD) concentration reaches 50000mg/L, the first acidifying of described etherifying phenol-contained wastewater, extract with described complexing extractant-PN again, regulate the pH value to 6-9 with described alkali lye, described etherifying phenol-contained wastewater volatile phenol concentration after the processing can reach in the 100mg/L, chemical oxygen demand (COD) concentration reaches in the 1000mg/L, described volatile phenol percentage extraction can reach 98.3%, described chemical oxygen demand (COD) percentage extraction reaches 98%, after handling through biochemistry etc. again, can qualified discharge.After being extracted into the aldehydes matter process reextraction among described complexing extractant-PN, can return the production line recycle.
Beneficial effect: the present invention compared with prior art, its remarkable advantage is: the present invention adopts composite complexing extractant-PN that triclosan etherificate waste water is carried out extraction treatment, can remove high density volatile phenol and chemical oxygen demand (COD) effectively, reclaim simultaneously excessive phenol effectively, reduce production cost, utilized resource fully.
Embodiment
The present invention is further described below in conjunction with embodiment:
Embodiment 1
Add 600kg aviation kerosene, 100kg isobutyl ketone, 100kgN in reactor, N-N,N-DIMETHYLACETAMIDE and 200kg n-Octanol stir, and package spare.100ml volatile phenol concentration being reached the etherifying phenol-contained wastewater that 6000mg/L, chemical oxygen demand (COD) concentration reach 50000mg/L in the time of 30 ℃ joins in the 250ml reaction flask, regulate pH=2-3 with hydrochloric acid, add complexing extractant-PN that 50ml prepares, after fully stirring, pour separating funnel into, standing demix.Lower floor's etherifying phenol-contained wastewater through extraction is branched away, and the mensuration volatile phenol is that 105mg/l, COD are 1142mg/l.Regulate etherifying phenol-contained wastewater pH value to 6-9, carry out treating processess such as biochemistry then, qualified discharge.The extraction agent of layering remainder in the extraction test is joined in the 250ml reaction flask, add the sodium hydroxide solution of 30ml mass percent 10%, after fully stirring, pour separating funnel into, standing demix.The concentration that lower floor's strip liquor is measured phenol is 16.1mg/ml.
Embodiment 2
Add 800kg aviation kerosene, 10kg isobutyl ketone, 10kgN in reactor, N-N,N-DIMETHYLACETAMIDE and 180kg n-Octanol stir, and package spare.100ml volatile phenol concentration being reached the etherifying phenol-contained wastewater that 6000mg/L, chemical oxygen demand (COD) concentration reach 50000mg/L in the time of 40 ℃ joins in the 250ml reaction flask, regulate pH=2-3 with hydrochloric acid, add 80ml complexing extractant-PN, after fully stirring, pour separating funnel into, standing demix.The stripped etherifying phenol-contained wastewater of lower floor is branched away, and the mensuration volatile phenol is that 95mg/l, COD are 987mg/l.Regulate etherifying phenol-contained wastewater pH value to 6-9, carry out treating processess such as biochemistry then, qualified discharge.The extraction agent of layering remainder in the extraction test is joined in the 250ml reaction flask, add the sodium hydroxide solution of 30ml mass percent 25%, after fully stirring, pour separating funnel into, standing demix.The concentration that lower floor's strip liquor is measured phenol is 19.2mg/ml.
Embodiment 3
Add 750kg aviation kerosene, 50kg isobutyl ketone, 50kgN in reactor, N-N,N-DIMETHYLACETAMIDE and 150kg n-Octanol stir, and package spare.100ml volatile phenol concentration being reached the etherifying phenol-contained wastewater that 6000mg/L, chemical oxygen demand (COD) concentration reach 50000mg/L in the time of 50 ℃ joins in the 250ml reaction flask, regulate pH=2-3 with hydrochloric acid, add 100ml complexing extractant-PN, after fully stirring, pour separating funnel into, standing demix.The stripped etherifying phenol-contained wastewater of lower floor is branched away, and the mensuration volatile phenol is that 92mg/l, COD are 989mg/l.Regulate etherifying phenol-contained wastewater pH value to 6-9, carry out treating processess such as biochemistry then, qualified discharge.The extraction agent of layering remainder in the extraction test is joined in the 250ml reaction flask, add the sodium hydroxide solution of 30ml mass percent 30%, after fully stirring, pour separating funnel into, standing demix.The concentration that lower floor's strip liquor is measured phenol is 19.1mg/ml.

Claims (5)

1. method for treating etherifying phenol-contained wastewater is characterized in that: may further comprise the steps:
1) is mixed with complexing extractant-PN with aviation kerosene, isobutyl ketone, n-Octanol and N,N-dimethylacetamide;
2) the pH value of the described etherifying phenol-contained wastewater of adjusting is 2-3;
3) described acidifying etherifying phenol-contained wastewater extracts with described complexing extractant-PN in the time of 30-50 ℃, stir, and layering, waste water is regulated the pH value to 6-9, carries out treating processess such as biochemistry then, qualified discharge;
4) stripped described complexing extractant-PN dissolves with alkali lye, and the sodium phenolate of formation is dissolved in described alkali lye, separates with described complexing extractant-PN, and described complexing extractant-PN proceeds extraction, and described alkali lye carries out the triclosan etherification reaction.
2. method for treating etherifying phenol-contained wastewater according to claim 1, it is characterized in that: in above-mentioned steps 1) in, described complexing extractant-PN comprises following component by mass percent: aviation kerosene 60%-80%, diisobutyl ketone 1%-10%, N,N-dimethylacetamide 1%-10% and n-Octanol 15%-20%.
3. method for treating etherifying phenol-contained wastewater according to claim 1 is characterized in that: in above-mentioned steps 2) in, the pH value of described etherifying phenol-contained wastewater is regulated with hydrochloric acid.
4. method for treating etherifying phenol-contained wastewater according to claim 1 is characterized in that: in above-mentioned steps 3) in, the time that described extraction is stirred is 1 hour.
5. method for treating etherifying phenol-contained wastewater according to claim 1 is characterized in that: in above-mentioned steps 4) in, described alkali lye is mass percent 10%-30% sodium hydroxide solution.
CN2010102605087A 2010-08-24 2010-08-24 Method for treating etherifying phenol-contained wastewater Expired - Fee Related CN101913737B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515391A (en) * 2011-12-15 2012-06-27 中蓝连海设计研究院 Method for pre-treating wastewater from ultraviolet absorber production
CN104163524A (en) * 2014-08-27 2014-11-26 江苏天成生化制品有限公司 Method for treating phenol-containing wastewater in gas generator
CN115140868A (en) * 2022-07-26 2022-10-04 山东奥友生物科技股份有限公司 Continuous treatment process for waste alkaline water in preparation process of 2,4 '-trichloro-2' -nitrodiphenyl ether

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5330164A (en) * 1976-09-02 1978-03-22 Honshu Kagaku Kougiyou Kk Treating of waste water containing phenols
CN1045960A (en) * 1989-03-28 1990-10-10 福建师范大学 The treatment process of phenolic wastewater
CN101077799A (en) * 2006-05-26 2007-11-28 中国科学院化学研究所 Infiltration vaporization blending composite film for removing phenols from waste water
CN101597124A (en) * 2009-01-09 2009-12-09 华南理工大学 A kind of processing contains the method for phenol ammonia coal gasification waste water

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5330164A (en) * 1976-09-02 1978-03-22 Honshu Kagaku Kougiyou Kk Treating of waste water containing phenols
CN1045960A (en) * 1989-03-28 1990-10-10 福建师范大学 The treatment process of phenolic wastewater
CN101077799A (en) * 2006-05-26 2007-11-28 中国科学院化学研究所 Infiltration vaporization blending composite film for removing phenols from waste water
CN101597124A (en) * 2009-01-09 2009-12-09 华南理工大学 A kind of processing contains the method for phenol ammonia coal gasification waste water

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515391A (en) * 2011-12-15 2012-06-27 中蓝连海设计研究院 Method for pre-treating wastewater from ultraviolet absorber production
CN104163524A (en) * 2014-08-27 2014-11-26 江苏天成生化制品有限公司 Method for treating phenol-containing wastewater in gas generator
CN115140868A (en) * 2022-07-26 2022-10-04 山东奥友生物科技股份有限公司 Continuous treatment process for waste alkaline water in preparation process of 2,4 '-trichloro-2' -nitrodiphenyl ether

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