CN103708651A - Degradation-resistant high-chlorine alkaline waste water treatment method - Google Patents

Degradation-resistant high-chlorine alkaline waste water treatment method Download PDF

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Publication number
CN103708651A
CN103708651A CN201310755502.0A CN201310755502A CN103708651A CN 103708651 A CN103708651 A CN 103708651A CN 201310755502 A CN201310755502 A CN 201310755502A CN 103708651 A CN103708651 A CN 103708651A
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waste water
water
treatment
alkali
cod
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CN103708651B (en
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黄梅
张敏东
花俊峰
陈圣福
张斌
佘万卫
金建洪
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Zhejiang University ZJU
Zhejiang Huayou Cobalt Co Ltd
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Zhejiang University ZJU
Zhejiang Huayou Cobalt Co Ltd
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Abstract

The invention discloses a degradation-resistant high-chlorine alkaline waste water treatment method. The method comprises the steps of regulating pH value of the waste water to be more than 9, adding ferric salt and oxidizing agent for reaction, filtering, adding acid solution into filtrate, regulating pH value of the waste water to be 7-8. According to the degradation-resistant high-chlorine alkaline waste water treatment method, high ferrate is in-situ synthesized under an alkaline condition, pollutants in high-chlorine alkaline waste water are oxidized simultaneously, and COD (chemical oxygen demand) in the industrial waste water is reduced. The degradation-resistant high-chlorine alkaline waste water treatment method has simple steps, is green and environment-friendly, has low requirement on treatment equipment, low cost, and remarkable degradation effect on COD in the industrial waste water and is suitable for large-scale industrial production, and the removal rate of the COD is up to 50%.

Description

A kind for the treatment of process of high chlor-alkali used water difficult to degradate
Technical field
The present invention relates to water-treatment technology field, be specifically related to a kind for the treatment of process of high chlor-alkali used water difficult to degradate.
Background technology
Along with the high speed development of national industrial level and the raising of living standards of the people, chemical industrial product is produced and consumption is advanced by leaps and bounds, and trade effluent total amount is corresponding increase also, and due to the development of production technique, the composition of waste water also becomes more diverse.Although the policy of national strict implement energy-saving and emission-reduction, due to the complicacy of wastewater source and composition, the used water difficult to degradate of extreme condition is difficult point and the blind spot in Pollution abatement always.
High salinity wastewater is the focus of domestic and international expert's research, and it mainly comes from the industries such as metallurgy, pharmacy, printing and dyeing, foodstuffs industry, as processes such as the dissolving in metallurgical production process, acid-alkali accommodation and neutralizations; Crystallization in medicinal chemicals building-up process, filtration, washing procedure; As medium in hot pickled mustard tube production curing process in foodstuffs industry.Alkaline waste water refers in water body and contains some alkaloids, the waste water water sample that causes water body pH to be greater than 9.If these waste water, without just processing directly discharge, by corrosion pipeline and buildings, enter after water body, will change the pH value of water body, affect the self-purification of water body, destroy water body natural, ecological, cause water resources to reduce or destroy.Alkaline waste water total amount accounts for the sixth left and right of wastewater emission amount at present, is mainly derived from the black liquor of alkali paper-making, the waste water of the ash alkali unhairing waste water that boils yarn, mercerising wash water, tanning industry of printing and dyeing industry and oil, chemical industry part producing process etc.Alkaline waste water is processed the simple acid-base neutralisation method of normal employing at present, not only can consume a large amount of acid solutions, but also increase the salinity of water body, to subsequent disposal, brings difficulty; On the other hand, simple adjustment soda acid can not make organic matter degradation in water body, thereby water body COD is still higher, must use additive method to carry out combined treatment.
People have carried out the research that high salinity wastewater is processed at present, relate generally to biochemical process, Physical, chemical method etc.Application biochemical process is processed high salinity wastewater, and the high salt in water body or alkaline environment can make the metabolism of microorganism slow, and lower processing efficiency is restricted its application of processing for high salinity wastewater.And the method for utilizing halophilic bacterium to administer, because halophilic bacterium is cultivated comparatively difficulty, very easily because salinity fluctuation is dead, thereby remarkably influenced the final treatment effect of waste water.
Chemical oxidization method is to adopt chemical reaction the organism in waste water to be degraded to remove the process of COD.Industrial conventional chemical oxidization method comprises advanced oxidation processes, electrochemical process, photochemical catalytic oxidation etc. at present.The advantage of method of chemical treatment is applied widely, can be used for different sorts pollutent, especially for high-concentration hardly-degradable waste water, method of chemical treatment has the unique advantage that is better than other treatment processs, as high removal efficiency or be converted into product of bio-degradable etc., because of but a kind of desirable water treatment method.
Fenton oxidation reaction is by generation, to have the class oxidation system that the hydroxyl radical free radical of strong oxidation capacity is feature in high-level oxidation technology, it has unique advantage to poor, the baroque Persistent organic pollutants of biodegradability, has vital role in Industrial Wastewater Treatment.Because Fenton oxidation reaction is to utilize ferrous ion as catalyzer, by hydrogen peroxide is converted into hydroxyl radical free radical, realize organic oxidative degradation, its optimum oxidation condition is pH=3~4, thereby it is a kind of typical acidic oxidation reaction process.For alkaline waste water, because oxidant hydrogen peroxide is unstable under alkaline condition, easily decompose, the Fenton advanced oxidation system that causes having strong oxidation characteristic cannot be directly used in the processing of alkaline waste water.General indirect treatment process pattern is first to carry out acid adjustment pre-treatment at present, then causes follow-up acid advanced oxidation reaction.But recent result of study shows, Fenton's reaction speed and efficiency under high chlorine condition are obviously suppressed, and in solution, process is relevant therewith in the existence of some yin, yang ion.While containing a large amount of chlorion as existing result of study proof by alkali environment acid adjustment introducing or initial water body itself, the stronger chlorion of hydroxyl free gene preferential oxidation reductibility generating becomes chlorine and is consumed in a large number, cause the free radical quantity of actual participation organic pollutant degradation limited, finally cause Fenton oxidation method to show poor efficiency characteristic and more difficult application when processing this type of high-chloride wastewater.
Ferrate is a kind of Green Oxidant in recent years rising, its feature structure high ferro acid group (FeO 4 2-) redox potential under acidic conditions is 2.2V, is greater than ozone and is only less than OH, thereby show strong oxidizing property, each type organic in can powerful degraded water body.Meanwhile, high ferro acid group self is reduced into the Fe (OH) existing with colloidal form in water 3, it, can be efficiently except the fine suspended substance in anhydrating as a kind of colory inorganic flocculating agent.The strong oxidation that ferrate has and the acting in conjunction of flocculation, make it aspect water body disinfection and scrubbing, not only be better than all kinds of oxygenants comprehensively, but also can avoid producing secondary pollutant, so being used as new and effective Green Oxidant, ferrate carries out primary study.
Ferrate synthesizes the three kinds of methods that mainly contain: dry method, wet method, electrolytic process.It is to have applied at present and the method for tool industrial prospect that wet method is wherein prepared ferrate, and representative salt comprises potassium ferrate and Na2Fe04.Because of Na2Fe04 solvable in saturated strong base solution, so commercial ferrate is mainly potassium ferrate.Although the purity to 95.9% of potassium ferrate in preparation process, yield generally only has 10~15%, and solid-state high ferro acid group unstable, very easily decompose.And ferrate needs first water-solublely while using, if contain solution impurity in water body, there is the interfering factorss such as illumination, high temperature, ferrate, by fast decoupled, causes oxygenant to lose efficacy.Therefore, when ferrate carries out industrial applications as strong oxidizer and good flocculation agent, be subject to the restriction of the factors such as cost, oxidation activity, output also to lack at present the example of successful Application.
Summary of the invention
The invention provides a kind for the treatment of process of high chlor-alkali used water difficult to degradate, original position synthesized high iron hydrochlorate under alkaline condition, and the pollutent in the high chlor-alkali wastewater of Simultaneous Oxidation, to reduce the COD of trade effluent.Present method step is simple, environmental protection, low, with low cost to treatment facility requirement, and remarkable to the reduction effect of COD in trade effluent, and COD clearance reaches as high as 50%, is applicable to large-scale industrial production.
The treatment process that the invention discloses a kind of high chlor-alkali used water difficult to degradate, comprises the following steps:
Regulate the pH>9 of waste water, then add molysite and oxygenant to react, after filtering, in filtrate, add acid solution, regulate pH to 7~8 of waste water.
The present invention is directed to the treatment process that high chlor-alkali used water difficult to degradate has proposed alkaline ferrate oxidation, strong oxidizing property by the highly active Fe oxyradical that produces in ferric acid oxidizing reaction or high price iron intermediate etc., realizes the effective removal to difficult degradation component in high chlor-alkali wastewater.
As preferably, the chloride ion content of described high chlor-alkali wastewater is 2000~20000mg/L.
As preferably, by adding alkali lye to regulate wastewater pH >=10, described alkaline solution is sodium hydroxide solution or potassium hydroxide solution, and concentration is 5~10M.By adding alkaline solution to change the pH value of solution, make solution in highly basic state, object is to provide necessary reaction conditions for follow-up ferric acid oxidizing reaction.
As preferably, described oxygenant is clorox, sodium chlorate or chlorine.In described several oxygenants, commercially available clorox is solution form, and the content of conventional effective chlorine density sign clorox in solution, as 5.2% or 10% etc.; Commercially available sodium chlorate is solid, does not generally directly feed intake, but be made into 10% or more after the solution of high concentration, feed intake again during for sewage disposal; Chlorine is generally reinforced with gas form.
As preferably, described molysite is ferrous sulfate, Iron nitrate, iron trichloride, iron nitrate or ferric sulfate etc., and in waste water solution, the concentration of molysite is 0.5~10mM, and the mol ratio of molysite and oxygenant is 1:5~30.Further preferably, in described waste water solution, the concentration of molysite is 2~10mM, and the mol ratio of molysite and oxygenant is 1:10~20.Because the diversity of oxygenant existence form, simultaneous oxidation efficiency is also that to take the molar weight of actual participation oxidizing reaction be benchmark, so the only simple pure substance amount metering with adding of each oxygenant consumption.
As preferably, 1~7h is carried out in described reaction at 20~50 ℃; Further preferably, 5~7h is carried out in described reaction at 50 ℃.
As preferably, described acid solution is sulfuric acid, hydrochloric acid or salpeter solution, and concentration is 5~10M, and adding acid solution to regulate pH value is 7~8, facilitates follow-up direct discharge.
With respect to prior art, the present invention has following useful technique effect:
(1) situ of the present invention generates ferrate, has avoided conventional oxidation style to prepare in ferrate, the predicament that preparation condition is harsh, yield is low, price is high; And generated in-situ ferrate by synchronous for being oxidized the pollutent of high chlor-alkali wastewater, this also solved have hyperoxia voltinism ferrate poor stability, store difficult problem;
(2) the present invention utilizes advanced oxidation technology to carry out the processing of indegradable industrial effluent under alkaline hypersaline environment, by at high salinity water body situ synthesized high iron hydrochlorate, cause the generation of highly active Fe oxyradical or high price iron intermediate to carry out the oxide treatment of hard-degraded substance, realize the efficient target of removing to trade effluent COD under high salinity condition;
(3) original position ferrate oxidation system has overcome water body neutral and alkali environment and the impact of high salt condition on traditional advanced oxidation processes processing waste water, can be in the alkalescence of its more difficult application high salt extreme environment efficiently remove the COD of waste water, widened the efficient range of application of processing of trade effluent; The method not only can be in the Industrial Wastewater Treatment such as daily trade effluent, Food Industry Wastewater, more can be used for the sea water preprocessing aspect that contains a large amount of negatively charged ion, to alleviating growing environmental pollution pressure and daily productive life problem of water consumption at present, be significant.
Embodiment
Below in conjunction with embodiment, describe the present invention in detail, but the present invention is not limited to this.
Embodiment 1
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 10000mg/L, the pH=10 that adds a certain amount of sodium hydrate regulator solution, in solution, slowly add the chlorine bleach liquor of 1ml5.2% available chlorine and fully stir again, measuring 0.2ml0.5MFe (NO 3) 3dropwise add in reaction solution, at 30 ℃, react 4 hours.Standing, filtration, get the H that supernatant liquor adds 5mol/L 2sO 4, the pH=7 of regulator solution, water sampling carries out COD mensuration, known water sample COD=296mg/L, after reaction, the clearance of COD is 30.8%.
Embodiment 2
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 10000mg/L, the pH=14 that adds a certain amount of sodium hydrate regulator solution, in solution, slowly add the chlorine bleach liquor of 1ml5.2% available chlorine and fully stir again, measuring 0.2ml0.5MFe (NO 3) 3dropwise add in reaction solution, at 30 ℃, react 4 hours.Standing, filtration, get the H that supernatant liquor adds 5mol/L 2sO 4, the pH=7 of regulator solution, water sampling carries out COD mensuration, known water sample COD=246mg/L, after reaction, the clearance of COD is 42.5%.
Embodiment 3
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 2000mg/L, the pH=10 that adds a certain amount of sodium hydrate regulator solution, in solution, slowly add the chlorine bleach liquor of 1ml5.2% available chlorine and fully stir again, measuring 0.2ml0.5MFe (NO 3) 3dropwise add in reaction solution, at 30 ℃, react 7 hours.Standing, filtration, get the H that supernatant liquor adds 5mol/L 2sO 4, the pH=7 of regulator solution, water sampling carries out COD mensuration, known water sample COD=258mg/L, after reaction, the clearance of COD is 39.7%.
Embodiment 4
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 2000mg/L, the pH=10 that adds a certain amount of sodium hydrate regulator solution, in solution, slowly add the chlorine bleach liquor of 0.5ml5.2% available chlorine and fully stir again, measuring 0.1ml0.5MFe (NO 3) 2dropwise add in reaction solution, at 30 ℃, react 4 hours.Standing, filtration, get the H that supernatant liquor adds 5mol/L 2sO 4, the pH=8 of regulator solution, water sampling carries out COD mensuration, known water sample COD=300mg/L, after reaction, the clearance of COD is 29.9%.
Embodiment 5
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 2000mg/L, the pH=10 that adds a certain amount of sodium hydrate regulator solution, to slowly to add 2.8ml massfraction in solution be 10% sodium chlorate solution and fully stir, measure 1.5ml0.1MFe (NO again 3) 2dropwise add in reaction solution, at 50 ℃, react 7 hours.Standing, filtration, get the H that supernatant liquor adds 5mol/L 2sO 4, the pH=7 of regulator solution, water sampling carries out COD mensuration, known water sample COD=226mg/L, after reaction, the clearance of COD is 47.2%.
Embodiment 6
Accurately measure the cobalt ore beneficiation wastewater (initial COD=868mg/L) of 100ml chloride ion-containing 10000mg/L, the pH=10 that adds a certain amount of sodium hydrate regulator solution, to slowly to add 1.9ml massfraction in solution be 10% chlorine bleach liquor and fully stir, measure 1.2ml0.4M FeSO again 4dropwise add in reaction solution, at 20 ℃, react 7 hours.Standing, filtration, get the H that supernatant liquor adds 10mol/L 2sO 4, the pH=7 of regulator solution, water sampling carries out COD mensuration, known water sample COD=641mg/L, after reaction, the clearance of COD is 26.2%.
Embodiment 7
Accurately measure the cobalt ore beneficiation wastewater (initial COD=868mg/L) of 100ml chloride ion-containing 10000mg/L, the pH=10 that adds a certain amount of sodium hydrate regulator solution, to slowly to add 7.0ml massfraction in solution be 10% sodium chlorate solution and fully stir, measure 1.1ml0.2MFe again 2(SO 4) 3dropwise add in reaction solution, at 50 ℃, react 7 hours.Standing, filtration, get the HNO that supernatant liquor adds 10mol/L 3, the pH=7 of regulator solution, water sampling carries out COD mensuration, known water sample COD=441mg/L, after reaction, the clearance of COD is 49.6%.
Embodiment 8
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 2000mg/L, add the pH=10 of a certain amount of sodium hydrate regulator solution, then pass into 0.2g chlorine and fully stir in solution, measure 0.2ml0.5M FeSO 4dropwise add in reaction solution, at 30 ℃, react 4 hours.Standing, filtration, get the HCl that supernatant liquor adds 10mol/L, the pH=8 of regulator solution, and water sampling carries out COD mensuration, known water sample COD=324mg/L, after reaction, the clearance of COD is 24.2%.
Embodiment 9
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 20000mg/L, the pH=10 that adds a certain amount of potassium hydroxide regulator solution, to slowly to add 10ml massfraction in solution be 10% sodium chlorate solution and fully stir, measure 1ml1.0MFeCl again 3dropwise add in reaction solution, at 50 ℃, react 5 hours.Standing, filtration, get the HCl that supernatant liquor adds 10mol/L, the pH=8 of regulator solution, and water sampling carries out COD mensuration, known water sample COD=237mg/L, after reaction, the clearance of COD is 44.6%.
Embodiment 10
Accurately measure the cobalt ore beneficiation wastewater (initial COD=428mg/L) of 100ml chloride ion-containing 10000mg/L, the pH=10 that adds a certain amount of sodium hydrate regulator solution, in solution, slowly add the chlorine bleach liquor of 2ml5.2% available chlorine and fully stir again, at 30 ℃, reacting 4 hours.Standing, filtration, get the H that supernatant liquor adds 5mol/L 2sO 4, the pH=7 of regulator solution, water sampling carries out COD mensuration, known water sample COD=335mg/L, after reaction, the clearance of COD is 21.7%.

Claims (9)

1. a treatment process for high chlor-alkali used water difficult to degradate, is characterized in that, comprises the following steps: the pH>9 that regulates waste water, add again molysite and oxygenant to react, after filtering, in filtrate, add acid solution, regulate pH to 7~8 of waste water.
2. the treatment process of high chlor-alkali used water difficult to degradate as claimed in claim 1, is characterized in that, in described waste water, chloride ion content is 2000~20000mg/L.
3. the treatment process of high chlor-alkali used water difficult to degradate as claimed in claim 2, is characterized in that, described oxygenant is clorox, sodium chlorate or chlorine.
4. the treatment process of high chlor-alkali used water difficult to degradate as claimed in claim 3, it is characterized in that, described molysite is ferrous sulfate, Iron nitrate, iron trichloride, iron nitrate or ferric sulfate, and in described waste water, the concentration of molysite is 0.5~10mM, and the mol ratio of molysite and oxygenant is 1:5~30.
5. the treatment process of high chlor-alkali used water difficult to degradate as claimed in claim 4, is characterized in that, in described waste water, the concentration of molysite is 2~10mM, and the mol ratio of molysite and oxygenant is 1:10~20.
6. the treatment process of the high chlor-alkali used water difficult to degradate as described in claim as arbitrary in claim 1~5, is characterized in that, 1~7h is carried out in described reaction at 20~50 ℃.
7. the treatment process of high chlor-alkali used water difficult to degradate as claimed in claim 6, is characterized in that, 5~7h is carried out in described reaction at 50 ℃.
8. the treatment process of high chlor-alkali used water difficult to degradate as claimed in claim 1, is characterized in that, by adding alkali lye to regulate wastewater pH >=10, described alkaline solution is sodium hydroxide solution or potassium hydroxide solution.
9. the treatment process of high chlor-alkali used water difficult to degradate as claimed in claim 1, is characterized in that, described acid solution is sulfuric acid, hydrochloric acid or salpeter solution.
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CN106673253A (en) * 2016-12-14 2017-05-17 安徽华塑股份有限公司 Treatment method for chlorine alkali industrial wastewater catalytic oxidation
CN107055850A (en) * 2016-11-25 2017-08-18 南宁市黑晶信息技术有限公司 A kind of flocculant sewage water treatment method
CN108147582A (en) * 2017-12-29 2018-06-12 攀枝花钢企欣宇化工有限公司 Chlor-alkali resin regeneration is given up water purification method
CN108408846A (en) * 2018-04-13 2018-08-17 深圳市深投环保科技有限公司 Wastewater electrochemical deep treatment method
CN110342678A (en) * 2019-07-04 2019-10-18 西安石油大学 A kind of method of controllable OH free radical Synergistic degradation processing sewage containing polysaccharide polymer

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