CN103708648A - Method for realizing reduction-Fenton oxidation coupled treatment of azo dyeing wastewater - Google Patents
Method for realizing reduction-Fenton oxidation coupled treatment of azo dyeing wastewater Download PDFInfo
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- CN103708648A CN103708648A CN201310732911.9A CN201310732911A CN103708648A CN 103708648 A CN103708648 A CN 103708648A CN 201310732911 A CN201310732911 A CN 201310732911A CN 103708648 A CN103708648 A CN 103708648A
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- azo dye
- dye wastewater
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Abstract
The invention discloses a method for realizing reduction-Fenton oxidation coupled treatment of azo dye wastewater, belonging to the technical field of industrial wastewater treatment and recycling of environmental protection. The method comprises the following steps: adding a low dose of activated reducer into azo dye wastewater of which the pH value has been regulated to acidic, reducing azo bonds in the wastewater into hydrazine bonds which can be easily subjected to oxidative degradation at 20-100 DEG C, and performing oxidative degradation on the reduced large molecules of the dye by using a Fenton reagent; after the reaction is finished, regulating the pH value of the effluent water to neutral, and settling to further remove organic substances in the water; and adsorbing organic small molecules of the effluent water after settling through activated carbon to further ensure the water quality of the effluent water. The method overcomes the problems of the existing Fenton oxidation coupled process such as requirement for additional special devices and equipment, complex process flow, high treatment cost and the like; the process flow disclosed by the invention is simple; and the method can ensure that the chroma removal rate of azo dyeing wastewater is 100% and the COD (chemical oxygen demand) removal rate is higher than 90% within 10 hours.
Description
Technical field
The invention belongs to Industrial Wastewater Treatment and the reuse technology field of environment protection, be specifically related to contain in a kind of textile and dyeing industry a kind of reduction-advanced oxidation coupled processing method of difficult for biological degradation azo dye printing and dyeing wastewater.
Background technology
Azoic dyestuff because of its dyeing rapidly and chromatogram extensively, be easy to synthetic and raw material is cheap, can be combined by widespread production with most of synthon or natural fiber and be applied to textile and dyeing industry.According to estimates, the output of annual synthetic dyestuff is approximately 10 in the world
6t, and azoic dyestuff accounts for 70% left and right of total amount.Yet, azoic dyestuff degree of fixation low (about 60%-70%), remainder mainly, with waste water formation discharge, is dealt with improperly and will be caused serious water body environment pollution by producing a large amount of reductibility aromatic amine compounds, and harm humans is healthy.Conventional azo dye printing and dyeing wastewater treatment process comprises Physical, chemical method and biological process three classes both at home and abroad at present.Physical is with physical adsorption most study, but have that water treatment effect is undesirable, the problem such as adsorbent reactivation and processing, and conventional biological process is removed because distinctive (one or more) azo bond structure in azoic dyestuff (especially heterocycle azo dyestuff) molecule is difficult to that it is realized to degraded efficiently, percent of decolourization unstable (11.5%-93.6%), long processing period, and applicable azoic dyestuff kind is limited, on aromatic nucleus, substituting group is hydroxyl (OH), amino (NH
2), the azoic dyestuff biological degradability of amido (N ≡) is stronger, and methoxyl group (OCH
3), sulfonic group (SO
3h), methyl (CH
3), carboxyl (COOH) and nitro (NO
2) the azoic dyestuff biological degradability that replaces is poor, the azoic dyestuff that molecular weight is larger is more difficult to biological degradation.
The key of Degradation of Azo Dyes is the fracture of azo bond structure, and chemical method has treatment effect fast and stable, outstanding feature applied widely owing to realizing the fracture of specific azo bond, wherein conventional with chemical oxidization method.The oxygenant that chemical oxidization method relates to comprises Fenton reagent, O
3, NaClO, H
2o
2deng, Fenton reagent oxidation method, as a kind of high-level oxidation technology of classics, because effect aspect Persistent organic pollutants in removing waste water is comparatively remarkable, in treatment of dyeing wastewater, be widely studied and use.However, Azo dye (especially macromole) is due to difficult degradation and be mingled with other complex construction components, although single Fenton oxidation technology can be realized percent of decolourization >90%, but organic clearance lower (the about 60%-70% of COD clearance), partial organic substances can not permineralization and is converted into intermediate product, to H
2o
2the lower processing cost that causes of utilization ratio is high, and because oxygenizement is not thorough, final outflow water is brown color to brown, is difficult to make waste water to reach discharge, more difficultly reaches reuse requirement.Therefore, Fenton reagent is coupled other oxidation means processing azo dyeing waste waters becomes study hotspot now, especially UV-Fenton oxidation, electrolysis-Fenton oxidation, biology-Fenton oxidation.
Above-mentioned Fenton oxidation coupling process is all based on promoting H
2o
2decompose and produce hydroxyl radical free radical, strengthen the oxidation capacity of system, the whole ultimate principle that improves Azo dye degradation rate and efficiency.Because this class oxidation coupling process need to provide specific energy or microorganism life condition, generally need to be equipped with specific device, treatment scheme is comparatively complicated, and processing costs is higher, practical engineering application difficulties.
Summary of the invention
For existing Fenton oxidative coupling technique, need optional equipment specific device, treatment scheme is complicated, the deficiency that processing costs is higher, the object of the present invention is to provide a kind of based on the reductive agent reduction azo bond novel method that reduction-Fenton oxidation coupling of Fenton reagent oxidation degrade azo dyestuff molecule processes that is coupled again.The method not only can realize the efficient removal of high density azo dye waste water chroma and COD, provide technical support, and technical process is simple, without extra means equipment, significantly reduces the processing costs of waste water for dyeing waste water directly discharges even further reuse.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of reduction-Fenton oxidation coupling is processed the method for azo dye wastewater, first in azo dye wastewater, add reductive agent to process, azo bond in azo dye wastewater is reduced to hydrazine key, adopt again Fenton oxidative treatment waste water, finally adjust the pH of waste water to neutral or alkaline, standing removal precipitation, obtains water outlet.
Preferred reduction-Fenton oxidation coupling is processed a method for azo dye wastewater, and concrete grammar comprises the steps:
(1) regulating pH to 1～5 of azo dye wastewater, is that 0.1-10:100 adds reductive agent according to the mass ratio of reductive agent and waste water, carries out reduction reaction, makes the azo bond in azo dye wastewater be reduced to hydrazine key;
(2) in the azo dye wastewater being reduced, add Fenton reagent, carry out oxidizing reaction, the dye molecule that oxidative degradation is reduced generates CO
2, the small molecules such as water;
(3) after reaction finishes, regulate pH to 7～9 of waste water, standing removal precipitation, obtains water outlet; Reductive agent before under alkaline environment and then react, the poly aluminum oxide of generation or other oxide compound are conducive to the organic further sedimentation of color development in waste water;
Above-mentioned azo dye wastewater is monoazo-dyes waste water, polyazo dye waste water or both composite wastes.
Above-mentioned reductive agent is the metallic aluminium powder of activated processing, and this reductive agent particle diameter is generally below 100 orders.
Above-mentioned activation treatment is for being used the zone of oxidation on diluted hydrochloric acid dissolution metallic aluminium powder surface.
In above-mentioned steps (1), use hydrochloric acid to regulate the pH of waste water.
In step (1), the reaction times of reduction reaction is 1-2h, and temperature of reaction is 20 ℃-100 ℃.
Fenton reagent in step (2) is the H that ferrous salt and volume fraction are 30%
2o
2, the dosage of ferrous salt is 0.01mmol L
-1-0.1mmol L
-1, the H of 30% volume fraction
2o
2dosage be 2mLL
-1-15mL L
-1.
In step (2), the reaction times of oxidizing reaction is 5h-8h, and temperature of reaction is 20 ℃-100 ℃.
In the water outlet of step (3), add gac, the solid-to-liquid ratio of gac and water outlet is 0.1-1:50g/ml, at 20 ℃-100 ℃, stirs 20-60min; Gac can adsorb after the organic molecule in waste water, and the COD clearance of final outflow water is greater than 90%, and chroma in waste water, turbidity removal rate reach 100%.
Compare with the Fenton oxidative coupling technique of existing azo dye wastewater, beneficial effect of the present invention is as follows:
(1) by adding the reductive agent of very low dose, under acidic conditions, azo bond is reduced, significantly improve speed and the efficiency of follow-up Fenton reagent degradation of dye molecule, improved 1 times of left and right with not adding reductive agent phase specific efficiency; And the reductive agent adding generates again flocculation agent by adjusting pH to neutrality or alkalescence, by sedimentation, further removes the organism in waste water;
(2) at short notice (10h) can realize the efficient removal of azo dye waste water chroma, COD, therefore significantly increases the daily handling ability of azo dyeing waste water;
(3) present method is applicable to the azo dye wastewater containing molecular weight is different, complex structure degree is different, comprise monoazo-dyes, polyazo dye or its mixture, can guarantee colourity and COD removal effect, chroma removal rate 100%, COD clearance is greater than 90%, stable effluent quality;
(4) present method, without being equipped with particular device, only needs the simple operationss such as stirring, sedimentation, filtration, uses simple receptacle can realize redox-solid-liquid separation-a plurality of processes such as absorption, and treatment scheme is relatively simple, and processing costs is lower.
Accompanying drawing explanation
Fig. 1 is reduction-Fenton oxidation processing technique schema of azo dye wastewater;
Fig. 2 is the 494nm absorbancy-reaction times change curve containing REACTIVE Orange 122 waste water of processing through reduction-Fenton oxidation coupling.
Embodiment
Below in conjunction with accompanying drawing and further detailed explanation the present invention of specific examples, but scope not thereby limiting the invention.
Reduction-Fenton oxidation coupling of the present invention is processed the method for azo dyeing waste water, first by activated reductibility pulvis, the azo bond of Azo dye to be reduced under acidic conditions, the dye molecule being reduced by the degraded of Fenton reagent oxidation again, after should completing, adjusting water outlet pH is to neutral, by sedimentation, further except the organism in anhydrating, waste water can be further by charcoal absorption organic molecule, the useless water purification of final realization.
As shown in Figure 1, azo dye wastewater is first removed branch, fabric fibre, large granular impurity etc. through grid, by the presetting wastewater pH of hydrochloric acid to 1-5, acid waste water is heated to 20 ℃-100 ℃ through preheater, with 0.1%-10% mass ratio, adds activated reductive agent Al powder, in insulation reduction pond at 20 ℃ of-100 ℃ of lasting stirring reaction 1-2h, standing 2h carries out solid-liquid separation, supernatant liquor is transferred to oxidation pond, continues to add Fenton reagent, Fe
2+(FeCl
2) addition is 0.01mmol L
-1-0.1mmol L
-1, the H of 30% volume fraction
2o
2addition is 2mL L
-1-15mL L
-1, be placed in insulation oxidation pond and continue stirring reaction 5-8h, then waste water enters Neutralization settlement pond, adjusts pH to 7-9, standing about 4h, supernatant liquor enters activated carbon adsorption tank, and gac addition is (0.1-1): 50, churning time 20-60min.Adsorption tank effluent color dilution clearance 100%, COD clearance >90%, water outlet can directly be discharged or reuse after ion-exchange desalination.
Embodiment 1
Certain printing and dyeing mill's waste water from dyestuff is containing REACTIVE Orange 122 (C
31h
20clN
7o
16s
5.4na, molecular weight 1034), it is 847mg L that colourity reaches 1080, COD
-1.This waste water regulates pH to 2.0 with dense HCl, is heated to 50 ℃, with 0.5wt% ratio, adds activated reduction pulvis Al, continues stirring reaction 3h, after suspension liquid standing sedimentation, and solid-liquid separation.Supernatant liquor adds Fenton reagent, and wherein iron protochloride addition is 0.04mmol L
-1, H
2o
2for 4mL L
-1, keep temperature-resistant, continue stirring reaction 5h, suspension liquid, through solid-liquid separation, regulates clear liquid pH to 7.5 with 20% sodium hydroxide solution, standing 1 hour, filters.Filtrate is added charcoal absorption organic molecule 30min according to 1:50 solid-to-liquid ratio, and after solid-liquid separation, supernatant liquor colourity is that 0, COD is 95mg L
-1, delivery turbidity is 0.
Embodiment 2
The reactive red B-2BF of Beijing printing and dyeing mill waste water, colourity is that 1100, COD is 744mg L
-1.This waste water regulates pH to 1.5 with dense HCl, is heated to 80 ℃, with 1.0wt% ratio, adds activated reduction pulvis Al, continues stirring reaction 1.5h, after suspension liquid standing sedimentation, and solid-liquid separation.Supernatant liquor adds Fenton reagent, and wherein iron protochloride addition is 0.1mmol L
-1, H
2o
2for 3mL L
-1, keep temperature-resistant, continue stirring reaction 4h, suspension liquid, through solid-liquid separation, regulates clear liquid pH to 7.0 with 20% sodium hydroxide solution, standing 1 hour, filters.Filtrate is added charcoal absorption organic molecule 60min according to 0.5:50 solid-to-liquid ratio, and after solid-liquid separation, supernatant liquor colourity is that 0, COD is 67mg L
-1, delivery turbidity is 0.
Embodiment 3
Certain printing and dyeing mill's Reactive Blue 222 waste water, colourity is that 980, COD is 714mg L
-1.This waste water regulates pH to 3.0 with dense HCl, is heated to 100 ℃, with 5.0wt% ratio, adds activated reduction pulvis Al, continues stirring reaction 1h, after suspension liquid standing sedimentation, and solid-liquid separation.Supernatant liquor adds Fenton reagent, and wherein iron protochloride addition is 0.08mmol L
-1, H
2o
2for 3mL L
-1, keep temperature-resistant, continue stirring reaction 8h, suspension liquid, through solid-liquid separation, regulates clear liquid pH to 8.0 with 20% sodium hydroxide solution, standing 1 hour, filters.Now effluent color dilution has been 0, therefore does not need to carry out charcoal absorption.Water outlet COD is 57mg L
-1, delivery turbidity is 0.
And as a comparison, adopt merely Fenton oxidation, do not pass through aluminum reduction, and maintenance iron protochloride addition is 0.08mmol L
-1, H
2o
2for 3mL L
-1, water outlet color is light brown, COD is 203mgL
-1, colourity is 30, turbidity is 0.
As shown in Figure 2, adding after reductive agent has been substantially 0 at 494nm at 4h light absorption value, and for not adding at least 8h of reductive agent needs, hence one can see that, adds the processing efficiency of the waste water that reductive agent accelerates greatly.
Embodiment 4-comparative example
The present embodiment is contrast experiment.Waste water Wei Mou used printing and dyeing mill Reactive Blue 222 waste water, colourity is that 980, COD is 714mg L
-1(with embodiment 3 be same source).This waste water regulates pH to 3.0 with dense HCl, adds H
2o
2, and H
2o
2add-on be 4mL L
-1.Reaction system stirs 24 hours in 70 ℃.Effluent color dilution is 940; COD is 675mg L
-1, the variation of colourity and COD is all very little.
In waste water, add activated aluminium powder, addition is waste water 3%, and all the other conditions remain unchanged.Stir after 5 hours, filter.Regulate filtrate pH to 7.5, after standing 1h, filter.Effluent color dilution 14, COD122mg L
-1.
This comparative example further illustrates Reactive blue waste water after aluminum reduction, more easily by Fenton reagent place, is oxidized, and has also embodied the present invention in effect and the superiority of processing azo dye wastewater.
Embodiment 5
Reactive Blue 222 wastewater source is with embodiment 3, and chroma in waste water is that 980, COD is 714mg L
-1.This waste water regulates pH to 1.0 with dense HCl, and controlling temperature of reactor is 20 ℃, with 5.0wt% ratio, adds activated reduction pulvis Al, continues stirring reaction 2h, after suspension liquid standing sedimentation, and solid-liquid separation.Supernatant liquor adds Fenton reagent, and wherein ferrous sulfate addition is 0.01mmol L
-1, H
2o
2for 15mL L
-1, continuing stirring reaction 8h, suspension liquid, through solid-liquid separation, regulates clear liquid pH to 9.0 with 20% sodium hydroxide solution, standing 1 hour, to filter, filtrate is added charcoal absorption, and gac addition is 0.1:50(gac: waste water, g/mL), constantly under agitation condition, adsorb 20min, filter.Effluent color dilution is that 0, COD is 37mgL
-1, turbidity is 0.
Embodiment 6
Reactive red B-2BF wastewater source is with embodiment 2, and colourity is that 1100, COD is 744mg L
-1.This waste water regulates pH to 5 with dense HCl, is heated to 100 ℃, with 2.0wt% ratio, adds activated reduction pulvis Al, continues stirring reaction 2h, after suspension liquid standing sedimentation, and solid-liquid separation.Supernatant liquor adds Fenton reagent, and wherein iron protochloride addition is 0.1mmol L
-1, H
2o
2for 2mL L
-1, continuing stirring reaction 4h, suspension liquid, through solid-liquid separation, regulates clear liquid pH to 9.0 with 20% sodium hydroxide solution, standing 1 hour, filters.Filtrate is added charcoal absorption organic molecule 60min according to 1:50 solid-to-liquid ratio, and after solid-liquid separation, supernatant liquor colourity is that 0, COD is 87mg L
-1, delivery turbidity is 0.
Claims (10)
1. a reduction-Fenton oxidation coupling is processed the method for azo dye wastewater, it is characterized in that, first in azo dye wastewater, add reductive agent to process, make the azo bond in azo dye wastewater be reduced to hydrazine key, adopt again Fenton oxidative treatment waste water, finally adjust the pH of waste water to neutral or alkaline, standing removal precipitation, obtains water outlet.
2. reduction-Fenton oxidation coupling according to claim 1 is processed the method for azo dye wastewater, it is characterized in that, concrete grammar comprises the steps:
(1) regulating pH to 1～5 of azo dye wastewater, is that 0.1-10:100 adds reductive agent according to the mass ratio of reductive agent and waste water, carries out reduction reaction, makes the azo bond in azo dye wastewater be reduced to hydrazine key;
(2) in the azo dye wastewater being reduced, add Fenton reagent, carry out oxidizing reaction;
(3) after reaction finishes, regulate pH to 7～9 of waste water, standing removal precipitation, obtains water outlet.
3. reduction-Fenton oxidation coupling according to claim 1 and 2 is processed the method for azo dye wastewater, it is characterized in that, described azo dye wastewater is monoazo-dyes waste water, polyazo dye waste water or both composite wastes.
4. reduction-Fenton oxidation coupling according to claim 1 and 2 is processed the method for azo dye wastewater, it is characterized in that the metallic aluminium powder that described reductive agent is activated processing.
5. reduction-Fenton oxidation coupling according to claim 4 is processed the method for azo dye wastewater, and described activation treatment is for being used the zone of oxidation on diluted hydrochloric acid dissolution metallic aluminium powder surface.
6. reduction-Fenton oxidation coupling according to claim 2 is processed the method for azo dye wastewater, it is characterized in that, uses hydrochloric acid to regulate the pH of waste water in described step (1).
7. reduction-Fenton oxidation coupling according to claim 2 is processed the method for azo dye wastewater, it is characterized in that, the reaction times of the described reduction reaction of step (1) is 1-2h, and temperature of reaction is 20 ℃-100 ℃.
8. reduction-Fenton oxidation coupling according to claim 2 is processed the method for azo dye wastewater, it is characterized in that, Fenton reagent described in step (2) is the H that ferrous salt and volume fraction are 30%
2o
2, the dosage of ferrous salt is 0.01mmol L
-1-0.1mmol L
-1, the H of 30% volume fraction
2o
2dosage be 2mL L
-1-15mL L
-1.
9. reduction-Fenton oxidation coupling according to claim 2 is processed the method for azo dye wastewater, it is characterized in that, the reaction times of oxidizing reaction described in step (2) is 5h-8h, and temperature of reaction is 20 ℃-100 ℃.
10. reduction-Fenton oxidation coupling according to claim 2 is processed the method for azo dye wastewater, it is characterized in that, in the described water outlet of step (3), add gac, the solid-to-liquid ratio of gac and water outlet is 0.1-1:50g/ml, at 20 ℃-100 ℃, stirs 20-60min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107777842A (en) * | 2017-11-20 | 2018-03-09 | 大连理工大学 | A kind of method of clean and effective mineralising azo dyes |
| CN112939304A (en) * | 2021-03-26 | 2021-06-11 | 沈阳大学 | Method for treating halogenated organic matter wastewater by virtue of high-grade reduction-oxidation coupling system based on magnesium-method flue gas desulfurization slag |
| CN114426349A (en) * | 2020-09-18 | 2022-05-03 | 中国石油化工股份有限公司 | Pretreatment method of ammoximation wastewater |
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| CN103145275A (en) * | 2013-03-15 | 2013-06-12 | 中北大学 | Method and device for treating wastewater by intensified micro-electrolysis-Fenton oxidation method |
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| CN103145275A (en) * | 2013-03-15 | 2013-06-12 | 中北大学 | Method and device for treating wastewater by intensified micro-electrolysis-Fenton oxidation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107777842A (en) * | 2017-11-20 | 2018-03-09 | 大连理工大学 | A kind of method of clean and effective mineralising azo dyes |
| CN107777842B (en) * | 2017-11-20 | 2021-06-08 | 大连理工大学 | Method for cleanly and efficiently mineralizing azo dye |
| CN114426349A (en) * | 2020-09-18 | 2022-05-03 | 中国石油化工股份有限公司 | Pretreatment method of ammoximation wastewater |
| CN112939304A (en) * | 2021-03-26 | 2021-06-11 | 沈阳大学 | Method for treating halogenated organic matter wastewater by virtue of high-grade reduction-oxidation coupling system based on magnesium-method flue gas desulfurization slag |
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