CN102910762A - Processing method of Cu(II)-EDTA (Ethylene Diamine Tetraacetic Acid) wastewater - Google Patents
Processing method of Cu(II)-EDTA (Ethylene Diamine Tetraacetic Acid) wastewater Download PDFInfo
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- CN102910762A CN102910762A CN2012104397482A CN201210439748A CN102910762A CN 102910762 A CN102910762 A CN 102910762A CN 2012104397482 A CN2012104397482 A CN 2012104397482A CN 201210439748 A CN201210439748 A CN 201210439748A CN 102910762 A CN102910762 A CN 102910762A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a processing method of Cu(II)-EDTA (Ethylene Diamine Tetraacetic Acid) wastewater, for solving the problems that the conventional wastewater processing method is high in cost and easily causes secondary pollution and has a trivial process. The processing method comprises the following steps of: measuring the concentration of COD and Cu<2+> in the Cu(II)-EDTA wastewater before processing; adjusting the pH value of Cu(II)-EDTA wastewater in a reaction tank I to 3-6, adding catalysts and an oxidant into the reaction tank I, and stirring and reacting for 0.5 hour to 3 hours, thus obtaining the reacted Cu(II)-EDTA wastewater; and standing the reacted Cu(II)-EDTA wastewater, discharging supernatant liquor of the wastewater into a reaction tank II, adding NaOH into the supernatant liquor of the wastewater to adjust the pH value of the supernatant liquor to 11-12, standing for getting sediments, and filtering, washing and calcining the sediments to obtain copper oxide, wherein sediments in the reaction tank I are recycled as the catalysts after being dried. The processing method has the advantages of degrading organic matter and recycling copper, and has environment-friendly and economic benefits.
Description
Technical field
The invention belongs to industrial effluent resource treatment technique field, particularly the treatment process of a kind of Cu (II)-EDTA waste water.
Background technology
Printed circuit board (PCB) industry, Electroplating Operations, semi-conductor industry etc. are played an important role in China's process of economic development, and its processing procedure is all closely bound up with metal treatment.Because metal plates out the quality that speed has directly affected the plating product, therefore in metal plating liquid, add organic interfacial agent and organic polymer etc., plate out efficient and then improve plating product quality to reduce metal.Have satisfactory stability just because of EDTA, metal ion is had very strong complex ability, have simultaneously the little characteristics of corrodibility, be widely used in disturbing chemical reaction or unwanted metal ion to remove in the industrial production.EDTA is applied to the electroless-plating processing procedure of printed circuit board (PCB), and with the chelated copper ion, the concentration of control copper and as the buffer reagent of plating bath is kept stable pH value.These solution use for some time rear stability variation, must discardedly upgrade; After plating, plank is extracted out in the cleaning process also can take waste liquid out of, causes the pollution of rinse water.Just because of the chemically stable characteristic of EDTA, cause and form high stable and not volatile Cu (II)-EDTA water-based inner complex behind the EDTA chelated copper ion.EDTA is to human body and nontoxicity in the general environment, and toxic heavy metal formation inner complex is dissolved in the water again in mud and the throw out but can make, and directly affects HUMAN HEALTH through food chain.In addition, Cu (II)-EDTA waste water has recovery value very much, as not processing discharging, not only threatens human health, causes environmental pollution, also can cause the wasting of resources; Cu (II)-EDTA waste water is carried out copper resource and EDTA recovery, not only can reduce the impact to environment, also can improve the economic benefit of enterprise, realize the doulbe-sides' victory of environmental protection, economic benefit.
The method of processing traditionally this type of waste water has chemical precipitation method, biological process, electrolytic process etc.Chemical precipitation method is processed, and because waste water stability is quite high, needs to use more coagulating agent, produces a large amount of heavy metal sewage sludges, not only can't really deal with problems, and also increases cost.Biological process is processed, and necessary first contact break separates cupric ion with EDTA, and EDTA needs itself can utilize biological treatment for biology can decompose.Photochemistry and electrochemical oxidation process treatment scale are little, and because of expensive expensive, thereby rig-site utilization is restricted.Fenton reagent oxidation method is utilized iron ion catalysis H
2O
2Produce hydroxyl radical free radical, be specially adapted to the organic oxide treatment of bio-refractory or general chemical oxidation hard degradation, but need to carry out under acidic conditions, process is wayward, and needs corrosion resistant apparatus, can produce Fe (OH) under the neutral and alkali condition
3Also may with color, there be larger limitation in mud, the water after the processing during practical application.For the removal of copper, commonly used have chemical precipitation method, extraction process and an electrolytic process etc.Adopt the sodium sulphite precipitation to remove copper, clearance is high, but excessive S
2-Can increase waste water COD, cause secondary pollution, pH also produces H when reducing
2S, contaminate environment.Extraction process, electrolytic process and reverse osmosis membrane are very high to the material requirement of electrode and film, drop into larger.Therefore, the treatment process of this class waste water still is improved and the space that overcomes, or seeks another treatment technology, processes effect to increase.
Summary of the invention
The objective of the invention is for the deficiencies in the prior art, the treatment process of a kind of Cu (II)-EDTA waste water is provided.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is as follows:
Step (1). measure the COD and the Cu that process front Cu (II)-EDTA waste water
2+Concentration;
Step (2). the Cu in the conditioned reaction pond one (II)-EDTA waste water ph to 3～6, add catalyzer and oxygenant, stirring reaction 0.5～3 h obtains reacted Cu (II)-EDTA waste water; Wherein add the catalyzer of 1～10g and the oxygenant of 0.1～0.3g in every liter of Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, in wastewater supernatant fluid, adds NaOH and regulate pH value to 11～12, leave standstill and get precipitation, obtain cupric oxide after filtering, wash, calcining; Throw out in the reaction tank one reuses as catalyzer after drying; Cu (II) after wherein processing-EDTA waste water COD clearance reaches 91.7～95.3%, Cu
2+Clearance reaches 90.2～92.7%.
Described catalyzer is one or more in iron carbonyl montmorillonite, rhombohedral iron ore, magnetite, flyash, red mud, the lepidocrocite; When being multiple, ratio be arbitrarily than;
Described oxygenant is one or more in Losantin, clorox, hypochlorous acid, the hydrogen peroxide; When being multiple, ratio is any ratio, and wherein oxygenant slowly adds with peristaltic pump with the solution form.
The inventive method all can be carried out under slightly acidic and neutrallty condition, and reaction conditions is gentle, and is high to organic mineralization rate, unglazed katalysis according to also carrying out under the condition to a certain degree; Catalyzer also can reuse, and has overcome Fenton oxidation style molysite and has entered in the waste water and can not recycle, the coloured shortcoming of waste water band after the processing; For the removal of cupric ion, the present invention adopts and adds alkali after the contact break and generate precipitation, and then calcining obtains the cupric oxide product, have recovery utilization rate high, drop into littlely, can not cause the advantage of secondary pollution; The present invention has advantages of to organic matter degradation and copper recoverable, to have environmental protection and economical effects.
Embodiment
The present invention is further described in conjunction with following instance, but content of the present invention is not limited only to content related among the embodiment.
Embodiment 1
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 3, add 1g flyash and 0.3g hydrogen peroxide, stirring reaction 3h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, in wastewater supernatant fluid, adds NaOH and regulate pH value to 11, leave standstill and get precipitation, obtain cupric oxide 77.8mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 1.
COD and Cu before and after table 1 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 1950 | 161.8 | 91.7％ |
| Cu 2+Concentration/mgL -1 | 97.4 | 9.5 | 90.2％ |
Embodiment 2
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 6, add 10g red mud and 0.2g clorox, stirring reaction 0.5h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 12 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 123.7mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 2.
COD and Cu before and after table 2 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 2200 | 103.4 | 95.3％ |
| Cu 2+Concentration/mgL -1 | 110 | 8.03 | 92.7％ |
Embodiment 3
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 4, add 3g magnetite and 0.2g Losantin, stirring reaction 1h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 12 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 87.8mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 3.
COD and Cu before and after table 3 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 2165 | 140.7 | 93.5％ |
| Cu 2+Concentration/mgL -1 | 108.2 | 8. 3 | 92.3％ |
Embodiment 4
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 5, add 5g iron carbonyl montmorillonite, 0.2g hydrogen peroxide, stirring reaction 2h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 11.5 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 99.8mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 4.
COD and Cu before and after table 4 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 2450 | 181.3 | 92.6％ |
| Cu 2+Concentration/mgL -1 | 122.5 | 10 | 91.9％ |
Embodiment 5
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 6, add 8g rhombohedral iron ore, 0.1g clorox, stirring reaction 3h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 11.8 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 90.1mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 5.
COD and Cu before and after table 5 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 2200 | 118.8 | 94.6％ |
| Cu 2+Concentration/mgL -1 | 110 | 8.6 | 92.1％ |
Embodiment 6
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 5, add 6g lepidocrocite, 0.2g hypochlorous acid, stirring reaction 1h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 12 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 99.6mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 6.
COD and Cu before and after table 6 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 2450 | 176.4 | 92.8％ |
| Cu 2+Concentration/mgL -1 | 122.5 | 10.5 | 91.4％ |
Embodiment 7
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 5.5, add 2g lepidocrocite, 2g magnetite, 0.25g hydrogen peroxide, stirring reaction 2.5h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 12 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 78.3mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 7.
COD and Cu before and after table 7 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 1950 | 154 | 92.1％ |
| Cu 2+Concentration/mgL -1 | 97.4 | 9.1 | 90.6％ |
Embodiment 8
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 5, add 3g iron carbonyl montmorillonite, 1g rhombohedral iron ore, 1g flyash, 0.3g hypochlorous acid, stirring reaction 2h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 11 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 101.4mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 8.
COD and Cu before and after table 8 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 2450 | 127.4 | 94.8％ |
| Cu 2+Concentration/mgL -1 | 122.5 | 9.3 | 92.4％ |
Embodiment 9
Step (1). measure the COD and the Cu that process front 1L Cu (II)-EDTA waste water
2+Concentration;
Step (2). the 1L Cu (II) in the conditioned reaction pond one-EDTA waste water ph to 4, add 6g flyash, 0.1g clorox, 0.1g hydrogen peroxide, stirring reaction 2.5h obtains reacted Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, NaOH regulates pH value to 11 in wastewater supernatant fluid, leaves standstill and gets precipitation, obtains cupric oxide 89.1mg after filtering, wash, calcining; Throw out drying in the reaction tank one reuses as catalyzer; Result such as table 9.
COD and Cu before and after table 9 Cu (II)-EDTA wastewater treatment
2+Concentration
| ? | Before the processing | After the processing | Clearance |
| COD/ mg·L -1 | 2200 | 149.6 | 93.2％ |
| Cu 2+Concentration/mgL -1 | 110 | 9.2 | 91.6％ |
Claims (3)
1. the treatment process of a Cu (II)-EDTA waste water is characterized in that, the method may further comprise the steps:
Step (1). measure the COD and the Cu that process front Cu (II)-EDTA waste water
2+Concentration;
Step (2). the Cu in the conditioned reaction pond one (II)-EDTA waste water ph to 3～6, add catalyzer and oxygenant, stirring reaction 0.5～3 h obtains reacted Cu (II)-EDTA waste water; Wherein add the catalyzer of 1～10 g and the oxygenant of 0.1～0.3g in every liter of Cu (II)-EDTA waste water;
Step (3). after reacted Cu (II)-EDTA waste water leaves standstill, wastewater supernatant fluid is disposed to reaction tank two, in wastewater supernatant fluid, adds NaOH and regulate pH value to 11～12, leave standstill and get precipitation, obtain cupric oxide after filtering, wash, calcining; Throw out in the reaction tank one reuses as catalyzer after drying; Cu (II) after wherein processing-EDTA waste water COD clearance reaches 91.7～95.3%, Cu
2+Clearance reaches 90.2～92.7%.
2. the treatment process of a kind of Cu according to claim 1 (II)-EDTA waste water, it is characterized in that: described catalyzer is one or more in iron carbonyl montmorillonite, rhombohedral iron ore, magnetite, flyash, red mud, the lepidocrocite; When being multiple, ratio be arbitrarily than.
3. the treatment process of a kind of Cu according to claim 1 (II)-EDTA waste water, it is characterized in that: described oxygenant is one or more in Losantin, clorox, hypochlorous acid, the hydrogen peroxide; When being multiple, ratio is any ratio, and wherein oxygenant slowly adds with peristaltic pump with the solution form.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103566959A (en) * | 2013-03-27 | 2014-02-12 | 北京林业大学 | Preparation of heat-treatment red mud catalyst and application thereof in water treatment technologies |
| CN104556470A (en) * | 2013-10-29 | 2015-04-29 | 南京源泉环保科技股份有限公司 | Method for removing EDTA (Ethylene Diamine Tetraacetic Acid) in waste water |
| CN105502739A (en) * | 2015-12-14 | 2016-04-20 | 南京大学 | Method for synchronous complex breaking and heavy metal removal based on self-strengthening ozone |
| CN107262154A (en) * | 2017-08-14 | 2017-10-20 | 苏州大学 | A kind of catalyst and method for carrying out embryonic stem-like cells in neutral conditions |
| CN109592821A (en) * | 2019-01-23 | 2019-04-09 | 广州大学 | A kind of method of EDTA- thallium complex in removal waste water |
| CN110182884A (en) * | 2019-05-27 | 2019-08-30 | 清华大学 | Electroplating sludge is catalyzed contact break-adsorption treatment electroplating wastewater method and contact break-absorption bifunctional material |
| CN110240248A (en) * | 2019-05-17 | 2019-09-17 | 河南师范大学 | A method of waste water being complexed using iron filings reaction bed processing Compound Heavy Metals-EDTA |
| CN110627250A (en) * | 2019-08-15 | 2019-12-31 | 广东工业大学 | Advanced oxidation-alkali regulation precipitation combined method for treating EDTA-Cu wastewater |
| CN111777628A (en) * | 2020-07-13 | 2020-10-16 | 江西省科学院应用化学研究所 | Catalytic wet oxidation catalyst for treating glyphosate wastewater, and synthesis method and application thereof |
| CN111977877A (en) * | 2020-08-10 | 2020-11-24 | 江苏泉之源环境技术有限公司 | Zero-emission process for quickly removing EDTA in wastewater |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103566959A (en) * | 2013-03-27 | 2014-02-12 | 北京林业大学 | Preparation of heat-treatment red mud catalyst and application thereof in water treatment technologies |
| CN104556470A (en) * | 2013-10-29 | 2015-04-29 | 南京源泉环保科技股份有限公司 | Method for removing EDTA (Ethylene Diamine Tetraacetic Acid) in waste water |
| CN105502739A (en) * | 2015-12-14 | 2016-04-20 | 南京大学 | Method for synchronous complex breaking and heavy metal removal based on self-strengthening ozone |
| CN105502739B (en) * | 2015-12-14 | 2020-01-10 | 南京大学 | Method for breaking complexing and synchronously removing heavy metal by self-reinforced ozone |
| CN107262154A (en) * | 2017-08-14 | 2017-10-20 | 苏州大学 | A kind of catalyst and method for carrying out embryonic stem-like cells in neutral conditions |
| CN109592821A (en) * | 2019-01-23 | 2019-04-09 | 广州大学 | A kind of method of EDTA- thallium complex in removal waste water |
| CN110240248A (en) * | 2019-05-17 | 2019-09-17 | 河南师范大学 | A method of waste water being complexed using iron filings reaction bed processing Compound Heavy Metals-EDTA |
| CN110182884A (en) * | 2019-05-27 | 2019-08-30 | 清华大学 | Electroplating sludge is catalyzed contact break-adsorption treatment electroplating wastewater method and contact break-absorption bifunctional material |
| CN110627250A (en) * | 2019-08-15 | 2019-12-31 | 广东工业大学 | Advanced oxidation-alkali regulation precipitation combined method for treating EDTA-Cu wastewater |
| CN111777628A (en) * | 2020-07-13 | 2020-10-16 | 江西省科学院应用化学研究所 | Catalytic wet oxidation catalyst for treating glyphosate wastewater, and synthesis method and application thereof |
| CN111777628B (en) * | 2020-07-13 | 2023-04-18 | 江西省科学院应用化学研究所 | Catalytic wet oxidation catalyst for treating glyphosate wastewater, and synthesis method and application thereof |
| CN111977877A (en) * | 2020-08-10 | 2020-11-24 | 江苏泉之源环境技术有限公司 | Zero-emission process for quickly removing EDTA in wastewater |
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Application publication date: 20130206 |