CN102060355A - Method for processing heavy-metal complexed wastewater through Fenton reinforced iron-chip internal electrolysis process - Google Patents
Method for processing heavy-metal complexed wastewater through Fenton reinforced iron-chip internal electrolysis process Download PDFInfo
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- CN102060355A CN102060355A CN 201010542945 CN201010542945A CN102060355A CN 102060355 A CN102060355 A CN 102060355A CN 201010542945 CN201010542945 CN 201010542945 CN 201010542945 A CN201010542945 A CN 201010542945A CN 102060355 A CN102060355 A CN 102060355A
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Abstract
The invention discloses a method for processing heavy-metal complexed wastewater through a Fenton reinforced iron-chip internal electrolysis process. The method comprises the following steps of: filling an internal electrolysis filler into an iron-chip internal electrolysis reactor, then introducing the wastewater into the reactor after regulating the pH value of the wastewater to 1.5-3.5, adding a Na2SO4 solution, controlling dissolved oxygen to be not higher than 3.0mg/L, and controlling the flow speed of the introduced wastewater; then introducing the discharged water of the internal electrolysis reactor into a Fenton reactor, maintaining the ferrous concentration in the water to be 300-750mg/L, adding H2O2 according to the mass concentration ratio of H2O2 to Fe2+ of 2.0-7.0, and sufficiently reacting for 60-120 minutes under the condition of controlling the pH value to be 2.5-5.5; and regulating the pH value of the discharged water to 9.0-10.0, standing and settling, and separating mud from the water. According to the method disclosed by the invention, the operation is simple and convenient, the sewage biodegradability can be markedly improved, the difficulty and the organic load of subsequent processing are greatly reduced, and the cost is saved.
Description
Technical field
The present invention relates to the advanced oxidation treatment process of a kind of poisonous and harmful, difficult for biological degradation trade effluent, specifically be that a kind of Fenton is strengthened the method that electrolysis process in the iron filings is handled heavy metal complexing waste water, be applicable to that industries such as handling printed circuit board (PCB), plating, pigment, metal processing are rich in the heavy metal complexing waste water of organic complexing agent such as EDTA.
Background technology
Heavy metal complexing waste water is mainly from production industries such as plating, printed circuit board, pigment, metal processing.Common complexing agent has EDTA, quadrol, tartrate, citric acid etc., and heavy metal ion coordination such as they and copper, nickel forms highly stable soluble complexes and becomes the principal pollutant of complexing waste water.The removal difficulty of complex state heavy metal ion is big, and common neutralization precipitation method is difficult to obtain satisfied treatment effect.
According to heavy metal complexing waste water characteristic, administer heavy metal complexing waste water and can take following technological line: (1) first contact break, manage heavy metal ion such as copper, nickel are dissociated out from complex state, be removed again, as sulphide precipitation, oxidation reduction process: for example: Fenton (Fenton) and NaClO oxidation style etc.; (2) without contact break, directly complex state and free state heavy metal are removed simultaneously, as absorption method, heavy metal chelating agent method of trapping, ion exchange method etc.Yet, ion exchange method and heavy metal chelating agent method processing cost height; Sulphide precipitation, oxidation reduction process use reagent consumption big, thus also processing cost height, and the generation sludge volume is big, perhaps uses other chemical agents easily to cause secondary pollution.Therefore, the application of these methods is restricted.
The iron filings internal electrolysis is to utilize iron filings as the anode expendable material, charcoal (comprising gac, graphite, coke etc.) is as the cathode catalysis material, form galvanic cell between iron filings and charcoal particle, synergies such as the physical adsorption by electrochemical redox, iron ion flocculation, adsorption coprecipitation and iron filings packing layer, filteration realize the purifying treatment to waste water.Studies have shown that copper, the nickel plasma in the EDTA heavy metal complexing waste water can be efficiently removed in electrolysis in the independent iron filings, yet it is to COD
Cr(chemical oxygen demand (COD), chemicaloxygen demand) clearance is lower, and water outlet is organic complexing agent such as residual a large amount of EDTA still.
Summary of the invention
The objective of the invention is defective, provide a kind of efficient processing to be rich in the novel method of the heavy metal complexing waste water of complexing agent such as EDTA at existing complexing waste water treatment process.Produce in " iron filings internal electrolysis " on the basis of a large amount of ferrous ions, add hydrogen peroxide and constitute Fenton reagent, at certain pH, H
2O
2/ Fe
2+Ratio and Fe
2+Under the concentration, produce hydroxyl radical free radical, realize effective degraded of complexing agents such as the abundant removal of copper, nickel and EDTA simultaneously, and improve the biodegradability of waste water greatly with strong oxidizing property.
Purpose of the present invention is achieved through the following technical solutions:
A kind of Fenton is strengthened the method for electrolysis process processing heavy metal complexing waste water in the iron filings, comprises following processing step:
(1) interior electrolysis filler is packed in the iron filings in the electrolysis reactor, then wastewater pH is adjusted to 1.5～3.5 backs and feeds in the reactors, add the Na of 0～0.06mol/L
2SO
4Solution is as ionogen, and the control dissolved oxygen is not higher than 3.0mg/L, and it is 20～60min that the flow velocity of control feeding waste water makes hydraulic detention time; Electrolysis filler comprises cast iron filing and activated carbon grain in the described iron filings, and the quality proportioning of cast iron filing and activated carbon grain was controlled at 1: 1～6: 1;
(2) again the water outlet of electrolysis reactor in above-mentioned is fed the Fenton reactor, keep that ferrous iron concentration is 300～750mg/L in the water, press H
2O
2/ Fe
2+Mass concentration ratio is 2.0～7.0 to add hydrogen peroxide, and control pH is at 2.5～5.5 times abundant reaction 60～120min;
(3) pH to 9.0～10.0, quiescent setting, mud-water separation are transferred in water outlet.
The described cast iron filing of aforesaid method is that the particulate state of particle diameter 0.5～3.0mm, thread iron plane flower and length and width are all a kind of in the cast iron bar of 1～10mm; Described active carbon granule is particulate state or the column of 1.0～5mm, and gac is accelerated cast iron filing dissolution rate and Fe as catalytic material
2+Produce, also can use coke, materials such as coal gangue or graphite replace.
Electrolysis filler was also handled through pre-activated in aforesaid method was described, its technology is: cast iron filing is that 9%～10% sodium hydroxide solution is at 80～100 ℃ of following oil removing 0.5h with the washing composition immersion and at 80～100 ℃ of oil removing 20～30min or with mass concentration, be 1%～2% salt acid soak 0.5h then with volume fraction, remove oxide on surface, with the clean after drying of flushing with clean water.
Electrolysis reactor is fixed-bed reactor or fluidized-bed reactor in the described iron filings of aforesaid method, when filler is the particulate state iron filings, takes the fluidized-bed reactor form, when filler is strip or wood shavings shape iron filings, takes the fixed-bed reactor form; The cast iron filing dosage is 20～80g/L, with gac be to load reactor in 1: 1～6: 1 by mass ratio.
According to aforesaid method, when adopting fluidized-bed reactor, with the alr mode reaction, stirring velocity 80～160min when adopting fixed-bed reactor, takes the pulse water-feeding mode to react and the intermittent aeration mode.
Compared with prior art, the outstanding feature that has of the present invention is: the 1. needed Fe of Fenton reaction process
2+All produce and provide, only need add H by electrolysis process in the iron filings of front
2O
22. the wastewater biochemical raising after the electrolysis pretreatment in iron filings has reduced the organic loading and the intractability of follow-up Fenton oxidation, reduces H
2O
2Consumption; 3. only need in waste water enters the iron charcoal disposable adjusting pH value before the electrolysis reactor; 4. in the iron filings electrolytic process with industrial waste---cast iron filing is as raw material, and microelectrolysis process consumed power not, and the treatment of wastes with processes of wastes against one another economizes on resources; In addition, the catalyst activity carbon granule can not be consumed in interior electrolytic process, therefore, only need regularly add cheap cast iron filing in this technology operational process, and running cost is low, is a kind of novel method of processing heavy metal complex waste water of efficient economy.
Embodiment
Below in conjunction with specific embodiment the present invention is done further concrete detailed description the in detail, but embodiments of the present invention are not limited thereto, the processing parameter for not indicating especially can carry out with reference to routine techniques.
Embodiment 1: the inner electrolysis fluidized bed associating of iron filings Fenton oxide treatment EDTA complex copper waste water
Being that the cast iron filing grain of 0.7mm soaks with washing composition and at 80 ℃ of following oil removing 20min with particle diameter, is that 1% salt acid soak 0.5 is good with volume fraction then, and the removal oxide on surface is standby with the clean after drying of flushing with clean water.Be added in the fluidized-bed reactor after will mixing through the activated carbon grain 20g of above-mentioned activation pretreated cast iron filing grain 20g and particle diameter 1.2mm again, then waste water regulated pH to 1.5 back and fed in the fluidized-bed, add 0.06mol/LNa
2SO
4Solution is as ionogen, mechanical stirring speed 80r/min, and it is 20min that the flow velocity that control feeds waste water makes the residence time of waterpower in interior electrolysis reactor; Again interior electrolysis water outlet is fed the Fenton reactor, ferrous ion concentration is 555mg/L in the mensuration water, add the hydrogen peroxide of 1665mg/L, regulate pH to 2.5, the control Fenton reaction times is 60min, get reacted water outlet 40ml and transfer pH to 9.0, quiescent setting is got the concentration that supernatant liquor is measured extraneous copper, COD, TOC in the waste water again.
Data analysis: waste water quality is before handling: 100mg/L Cu
2+, 364.0mg/L COD, 261.2mg/L TOC.As shown in Table 1, after the inner electrolysis fluidized bed processing of iron filings, pollutants removal rate is: copper, 96.2%; COD, 18.9%; TOC, 17.3%; After the inner electrolysis fluidized bed associating of iron filings Fenton oxide treatment, pollutants removal rate is brought up to: copper,＞99.5%; COD, 80.0%; TOC, 76.2%.
Interpretation of result: 1) compare with electrolysis in the independent iron filings, Fenton reagent is strengthened the degradation efficiency that electrolysis process in the iron filings can significantly improve EDTA, and water outlet COD and copper are removed efficient and significantly improved; 2) iron filings and activated carbon granule are realized fluidized state, have guaranteed contact fully between the two, have both improved the efficient of galvanic cell reaction between the iron charcoal, can prevent the appearance of problems such as reactor frequent jams and the easy fouling of iron filings again.
Table 1 is the effluent quality situation after the inner electrolysis fluidized bed and Fenton oxidization combination art breading of iron filings
Embodiment 2: electrolysis fixed bed associating Fenton oxidative treatment EDTA complex copper waste water in the iron filings
Is 9% soaking with sodium hydroxide and at 100 ℃ of following oil removing 0.5h with thread iron plane flower with mass concentration, is that 2% salt acid soak 0.5 is good with volume fraction then, and the removal oxide on surface is standby with the clean after drying of flushing with clean water.To load the into interior electrolysis fixed bed of iron filings through the pretreated thread iron plane flower 80g of above-mentioned activation with particle diameter 4.5mm gac 20g.Wastewater pH is adjusted to 3.5 backs to feed in the fixed-bed reactor, take pulse water-feeding mode and intermittent aeration mode, the hydraulic detention time that control water inlet flow velocity is kept waste water is 60min, the fixed bed water outlet is fed the Fenton reactor, ferrous ion concentration is 330mg/L in the mensuration water, in the Fenton reactor, add the 1320mg/L hydrogen peroxide then, regulate pH to 5.5, the control Fenton reaction times is when being 120min, get reacted water outlet 40ml and transfer pH to 10.0, quiescent setting is got the concentration that supernatant liquor is measured extraneous copper, COD, TOC in the waste water again.
Data analysis: waste water quality is before handling: 100mg/L Cu
2+, 364.0mg/L COD, 261.2mg/L TOC.As shown in Table 2, after interior electrolysis treatment, pollutants removal rate is: copper, 95.8%; COD, 21.9%; TOC, 19.9%; Behind Fenton intensive treatment 90min, pollutants removal rate is brought up to again: copper,＞99.6%; COD, 78.7%; TOC, 74.3%.
Interpretation of result: 1) compare with electrolysis in the independent iron filings, Fenton reagent is strengthened in the iron filings electrolysis process and copper, COD and TOC are removed efficient is significantly improved; 2) fixed-bed reactor adopt pulse water-feeding and intermittent aeration mode, spend fully contacting of surface, activated carbon grain for waste water and iron plane and have created favourable condition, have reduced easy loss and possibility of jamming that the iron plane flower causes because of corrosion.
Table 2 effluent quality situation after electrolysis fixed bed and the Fenton oxidization combination art breading in iron filings
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. a Fenton is strengthened the method that the interior electrolysis process of iron filings is handled heavy metal complexing waste water, it is characterized in that, comprises following processing step:
(1) interior electrolysis filler is packed in the iron filings in the electrolysis reactor, then wastewater pH is adjusted to 1.5～3.5 backs and feeds in the reactors, add the Na of 0～0.06mol/L
2SO
4Solution is as ionogen, and the control dissolved oxygen is not higher than 3.0mg/L, and it is 20～60min that the flow velocity of control feeding waste water makes hydraulic detention time; Electrolysis filler comprises cast iron filing and activated carbon grain in the described iron filings, and the quality proportioning of cast iron filing and activated carbon grain was controlled at 1: 1～6: 1;
(2) again the water outlet of electrolysis reactor in above-mentioned is fed the Fenton reactor, keep that ferrous iron concentration is 300～750mg/L in the water, press H
2O
2/ Fe
2+Mass concentration ratio is 2.0～7.0 to add hydrogen peroxide, and control PH is at 2.5～5.5 times abundant reaction 60～120min;
(3) pH to 9.0～10.0, quiescent setting, mud-water separation are transferred in the water outlet of Fenton reactor.
2. method according to claim 1 is characterized in that, described cast iron filing is that the particulate state of particle diameter 0.5～3.0mm, thread iron plane flower and length and width are all a kind of in the cast iron bar of 1～10mm.
3. method according to claim 1 is characterized in that, described active carbon granule is particulate state or the column of 1.0～5.0mm.
4. method according to claim 1, it is characterized in that, electrolysis filler is also handled through pre-activated in described, its technology is: cast iron filing is that 9%～10% sodium hydroxide solution is at 80～100 ℃ of following oil removing 0.5h with the washing composition immersion and at 80～100 ℃ of oil removing 20～30min or with mass concentration, be 1%～2% salt acid soak 0.5h then with volume fraction, remove oxide on surface, with the clean after drying of flushing with clean water.
5. method according to claim 2 is characterized in that, electrolysis reactor is fixed-bed reactor or fluidized-bed reactor in the described iron filings, when filler is the particulate state iron filings, take the fluidized-bed reactor form, when filler is strip or wood shavings shape iron filings, take the fixed-bed reactor form; The cast iron filing dosage is 20～80g/L, with gac be to load in 1: 1～6: 1 by mass ratio.
6. method according to claim 5 is characterized in that, when adopting fluidized-bed reactor, with the alr mode reaction, stirring velocity 80～160min when adopting fixed-bed reactor, takes the pulse water-feeding mode to react and the intermittent aeration mode.
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| CN102249393A (en) * | 2011-06-08 | 2011-11-23 | 武汉凯迪水务有限公司 | Circulating fluidized bed advanced treatment equipment for industrial wastewater |
| CN102351349A (en) * | 2011-09-15 | 2012-02-15 | 广东工业大学 | Treatment method for high-stability complexing heavy metal waste water |
| CN102603103A (en) * | 2012-04-10 | 2012-07-25 | 东莞市珠江海咸水淡化研究所 | Complex heavy-metal waste water emergency quick treatment method |
| CN102774935A (en) * | 2012-08-24 | 2012-11-14 | 四川大学 | Method for treating hardly-degraded wastewater by ferric and cupric bimetallic particles |
| CN103011376A (en) * | 2012-12-13 | 2013-04-03 | 同济大学 | Method for oxidatively degrading chlorophenol substances by using EDTA (ethylene diamine tetraacetic acid)-reinforced bimetal aluminum-iron system |
| CN103043855A (en) * | 2012-12-17 | 2013-04-17 | 南京工业大学 | Treatment method for wastewater of low density polyethylene grafted maleic anhydride |
| CN103086569A (en) * | 2013-01-08 | 2013-05-08 | 华南理工大学 | Method for detoxifying, emission-reducing and deeply treating wastewater of electronic electroplating industry |
| CN104086033A (en) * | 2014-08-05 | 2014-10-08 | 段希福 | Treatment method of copper-containing industrial wastewater |
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| CN105540752A (en) * | 2015-12-22 | 2016-05-04 | 重庆大学 | Method for treating aniline substances in dye wastewater |
| CN105712464A (en) * | 2016-04-27 | 2016-06-29 | 河北协同环保科技股份有限公司 | Fenton-like technique and reactor for treating biochemical effluent |
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| CN106517478A (en) * | 2016-10-18 | 2017-03-22 | 同济大学 | Method for improving reduction removal of pollutants with zero-valent iron |
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| CN108975463A (en) * | 2018-09-07 | 2018-12-11 | 宜兴市滨元环保设备有限公司 | A kind of Fenton's reaction tower of improvement |
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| CN110028193A (en) * | 2019-03-20 | 2019-07-19 | 北京万邦达环保技术股份有限公司 | Waste water reclaiming system |
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| CN102351349A (en) * | 2011-09-15 | 2012-02-15 | 广东工业大学 | Treatment method for high-stability complexing heavy metal waste water |
| CN102603103A (en) * | 2012-04-10 | 2012-07-25 | 东莞市珠江海咸水淡化研究所 | Complex heavy-metal waste water emergency quick treatment method |
| CN102774935A (en) * | 2012-08-24 | 2012-11-14 | 四川大学 | Method for treating hardly-degraded wastewater by ferric and cupric bimetallic particles |
| CN103011376A (en) * | 2012-12-13 | 2013-04-03 | 同济大学 | Method for oxidatively degrading chlorophenol substances by using EDTA (ethylene diamine tetraacetic acid)-reinforced bimetal aluminum-iron system |
| CN103043855A (en) * | 2012-12-17 | 2013-04-17 | 南京工业大学 | Treatment method for wastewater of low density polyethylene grafted maleic anhydride |
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| CN103086569B (en) * | 2013-01-08 | 2014-09-10 | 华南理工大学 | Method for detoxifying, emission-reducing and deeply treating wastewater of electronic electroplating industry |
| CN104086033A (en) * | 2014-08-05 | 2014-10-08 | 段希福 | Treatment method of copper-containing industrial wastewater |
| CN104086033B (en) * | 2014-08-05 | 2015-11-25 | 顾祥茂 | A kind for the treatment of process of copper-bearing industrial wastewater |
| CN104512975B (en) * | 2014-12-20 | 2017-02-08 | 郭聪 | Electroplating comprehensive wastewater treatment process |
| CN105347580A (en) * | 2015-11-10 | 2016-02-24 | 中国石油天然气股份有限公司 | Method suitable for polymer flooding produced water processing standard-meeting discharging |
| CN105347580B (en) * | 2015-11-10 | 2018-06-01 | 中国石油天然气股份有限公司 | A kind of method of suitable polymer flooding water processing standard discharge |
| CN105540752A (en) * | 2015-12-22 | 2016-05-04 | 重庆大学 | Method for treating aniline substances in dye wastewater |
| CN105712464A (en) * | 2016-04-27 | 2016-06-29 | 河北协同环保科技股份有限公司 | Fenton-like technique and reactor for treating biochemical effluent |
| CN105712464B (en) * | 2016-04-27 | 2018-07-24 | 河北协同水处理技术有限公司 | Class Fenton technology and reactor for handling bio-chemical effluent |
| CN106517478A (en) * | 2016-10-18 | 2017-03-22 | 同济大学 | Method for improving reduction removal of pollutants with zero-valent iron |
| CN106517478B (en) * | 2016-10-18 | 2019-11-29 | 同济大学 | A method of improving Zero-valent Iron reduction removal pollutant |
| CN107473364A (en) * | 2017-08-01 | 2017-12-15 | 大连海事大学 | A kind of Fenton fluid bed catalytic type filler and preparation method thereof |
| CN108975463A (en) * | 2018-09-07 | 2018-12-11 | 宜兴市滨元环保设备有限公司 | A kind of Fenton's reaction tower of improvement |
| CN109574359A (en) * | 2018-12-30 | 2019-04-05 | 江门市崖门新财富环保工业有限公司 | A kind of process for reclaiming of nickel-containing waste water Treated sewage reusing and nickel |
| CN110028193A (en) * | 2019-03-20 | 2019-07-19 | 北京万邦达环保技术股份有限公司 | Waste water reclaiming system |
| CN110028193B (en) * | 2019-03-20 | 2022-05-06 | 北京万邦达环保技术股份有限公司 | Waste water recycling system |
| CN113666545A (en) * | 2021-07-22 | 2021-11-19 | 中国大唐集团科学技术研究院有限公司中南电力试验研究院 | Treatment method for pickling organic waste liquid by using EDTA as cleaning medium |
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Application publication date: 20110518 |