CN101580317A - Nickel-containing wastewater treatment technology - Google Patents
Nickel-containing wastewater treatment technology Download PDFInfo
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- CN101580317A CN101580317A CNA2009100118498A CN200910011849A CN101580317A CN 101580317 A CN101580317 A CN 101580317A CN A2009100118498 A CNA2009100118498 A CN A2009100118498A CN 200910011849 A CN200910011849 A CN 200910011849A CN 101580317 A CN101580317 A CN 101580317A
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- nickel
- dimethylglyoxime
- containing wastewater
- filtration
- treatment technology
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Abstract
The invention discloses nickel-containing wastewater treatment technology, which comprises the following steps: using sodium hydroxide or ammonia water to adjust the pH value of nickel-containing wastewater to between 5.5 and 9.5; adding dimethylglyoxime into the nickel-containing wastewater under the stirring at normal temperature for a nickel deposition reaction, wherein the molar ratio of the dimethylglyoxime to Ni<2+> in a filtrate is 2.2:1-2.4: 1; filtering after the reaction is performed for 20 to 60 minutes; washing a filter cake by hot water with a temperature between 40 and 90 DEG C, and then obtaining a pure nickel chelate through the filtration; using hydrochloric acid, sulfuric acid or nitric acid to dissolve the nickel chelate according to product requirements; and obtaining corresponding nickel salt solution and the dimethylglyoxime after the filtration; recovering the dimethylglyoxime from an acid-dissolved filtrate; removing residual Fe<3+]> through neutralization; heating hydrolysis and filtration, and then evaporating, washing, crystallizing the filtrate and drying the crystal to obtain a product; merging the filtrates in step two and recovering the dimethylglyoxime; and using the recovered dimethylglyoxime for the nickel deposition reaction. The nickel-containing wastewater treatment technology can ensure that the nickel-containing wastewater reaches the standard after the treatment and the content of the residual Ni<2+> is less than 1mg/L, can also completely recover nickel, and has low treatment cost and less equipment investment.
Description
Technical field
The present invention relates to a kind of nickel-containing wastewater treatment technology.
Background technology
Though nickel and its esters toxicity are lower, as a kind of element with biological action, nickel can activate or suppress a series of enzyme (as arginase, carboxylase etc.) and its toxic action takes place.Animals eat nickel salt can cause stomatitis, gingivitis and acute gastroenteritis, and to the cardiac muscle and liver infringement is arranged.Experiment showed, that nickel is 7～8 mg/kg to the lethal quantity of rabbit, nickel and compound thereof have hormesis to human skin, mucous membrane and respiratory tract, can cause dermatitis and trachitis, even pneumonia takes place.Prove by experimentation on animals and crowd's observation: nickel has the effect of accumulating, and accumulates in kidney,spleen,liver at most, can bring out nasopharyngeal carcinoma and lung cancer.Nickel also has disadvantageous effect (nickel is 20ppm to the toxigenous threshold concentration of paddy rice) to plant-growth simultaneously, in addition hydrobiont is had tangible toxic action.Therefore there is strict demand in country to nickel content in the industrial wastewater discharge.
Often contain nickel in the waste water of nickel minerals exploitation smelting, light industry, machine manufacturing, nickel salt production, metal processing.Particularly the consumption nickel amount of nickel plating not only accounts for 12～15% of the whole nation total consumption nickel amount in the light industry, and the utilization ratio of nickel also lower (comprehensive utilization ratio of the cleaning production grade III Standard of electronickelling is 88%) in the Ni-Speed, so nickel-plating waste water becomes maximum nickel contamination hidden danger.At coating performance and to aspects such as complicated shape plating piece plating difficulty or ease the incomparable superiority of electronickelling is arranged owing to chemical nickel plating in the nickel plating technology, chemical nickel plating is because most of additive that uses food grade simultaneously, do not use such as toxic substances such as prussiates, than electronickelling environmental protection, so chemical nickel plating has the galvanized possibility of replacement in a lot of fields.But compare with plating, the chemical nickel-plating solution less stable uses 6～8 cycles promptly aging usually, and the aged plating bath still contains the Ni about 10g/L
2+Owing to contain a large amount of NH in the old liquid of chemical nickel plating
4 +And complex compound such as citric acid, lactic acid increased intractability again, deals with improperly and not only wastes resource but also can cause nickel contamination.
At present, the processing of nickel-containing waste water mainly contains following method:
1. neutralization precipitation method
Add alkali and regulate PH, make Ni
2+Form with nickel hydroxide precipitate is removed.This method is simple to operate, is one of at present the most frequently used method.But this method needs the wastewater to reach standard after very high PH just can make processing.Precipitation is less when using NaOH, but the cost height.Though use the lime cost low, it is more to handle the waste residue that produces, nickel reclaims difficulty, and has the hidden danger of secondary pollution.Also form nickel hydroxide colloidal precipitation in the N-process easily, cause filtration difficulty,, be difficult for precipitation, also need add the flocculation agent aids precipitation because it is less to form sedimentary particle.Waste water after the processing is alkalescence, also needs could discharge with the acid neutralization.In nickel-containing waste water, contain a large amount of NH in addition
4 +During with the stronger organism of complex ability, be difficult to make the waste water after the processing to reach the discharge of wastewater requirement.
2. sulfide precipitation
The nickel sulphide precipitation particle that sulfide precipitation forms is little, forms colloid easily.Vulcanizing agent originally has residual (S in the trade effluent in water simultaneously
2-Also there is strict demand in content country), meet acid generation hydrogen sulfide and cause environmental pollution, and adopt the sulfuration method to be difficult to Ni
2+Content is reduced to below the 1mg/L.
3. ferrite process
It mainly is to utilize sedimentary absorption property that the iron oxysome is handled waste water, so work as Ni in the waste water
2+Excessive concentration or waste water contain NH
4 +, just can't make the wastewater to reach standard after the processing during complex compound such as citric acid, and waste residue meet acid again can stripping, have the hidden danger of secondary pollution.Owing to form a large amount of precipitations, cause nickel to reclaim difficulty simultaneously.
4. solvent extration
Need more extraction progression by extraction, be difficult to Ni in the waste water simultaneously
2+Concentration is handled below the 1mg/L, and solvent extraction agent loss in extraction and regenerative process is more, causes the processing cost height.
5. absorption method
Sorbent material is used gac, humic acid, sepiolite, resin etc. always.Absorption method is usually used in handling Ni
2+The waste water that concentration is lower.This method exist saturated extent of adsorption little, be difficult for to reclaim nickel, deal with improperly and cause defectives such as secondary pollution, facility investment are big easily.
6. membrane separation technique
Comprise reverse osmosis, membrane extraction, ultrafiltration etc., because membrane sepn need reach at pending waste water under the condition of certain index could normal operation, suspended solid in the waste water, organism, colloidalmaterial etc. all have disadvantageous effect to the life-span of film, former water will adopt certain pre-treatment measure before advancing reverse osmosis membrane device, the film treating processes needs very high pressure simultaneously, the primary equipment investment is many, maintenance, working cost height.Concentrated solution also needs through harmless treatment once more in addition.
Summary of the invention
The objective of the invention is to solve the above-mentioned defective that prior art exists, provide a kind of back of nickel-containing waste water can being handled up to standard, make remaining Ni
2+Content＜1mg/L can all reclaim nickel again, the nickel-containing wastewater treatment technology that processing cost is low, facility investment is little.
Concrete technical scheme of the present invention is:
Nickel-containing waste water is regulated PH=5.5～9.5 with sodium hydroxide or ammoniacal liquor; Normal temperature stirs down and adds dimethylglyoxime and sink nickel reactant, Ni in dimethylglyoxime and the filtrate
2+Mol ratio be 2.2: 1～2.4: 1, react 20～60 minutes after-filtration, filter cake obtains purified nickel chelate more after filtration with 40～90 ℃ of hot washes; Nickel chelate dissolves with hydrochloric acid, sulfuric acid or nitric acid according to product requirement, can obtain corresponding nickel salt solution and dimethylglyoxime after the filtration; Acid lixiviation liquid after reclaiming dimethylglyoxime, again through neutralization, heating hydrolysis, remove by filter residual Fe
3+After, evaporation, washing, crystallization, drying obtain product; Merge the filtrate in second step and reclaim dimethylglyoxime; The dimethylglyoxime circulation of reclaiming is used for heavy nickel reactant.
Above-mentioned nickel-containing wastewater treatment technology, preferred PH=6.5～7.5 when regulating with sodium hydroxide or ammoniacal liquor.
Above-mentioned nickel-containing wastewater treatment technology, preferred ammoniacal liquor, thus reduce processing cost, fast reaction speed.
Above-mentioned nickel-containing wastewater treatment technology, the hot water temperature is preferred 80～90 ℃ during filter cake washing.
Above-mentioned nickel-containing wastewater treatment technology adopts countercurrent washing during filter cake washing.
Advantage of the present invention is:
Adopt above art breading nickel-containing waste water, remaining Ni
2+Content＜1mg/L except that the waste water after handling meets the demands, also can all be reclaimed institute in the waste water is nickeliferous, and is obtained qualified nickel salt product.Reaction conditions is normal temperature, normal pressure, and equipment is not had particular requirement, and dimethylglyoxime is also recyclable simultaneously recycles, so processing cost is very low.And it is neutral that the waste water after handling is, and need not neutralize just can reach emission request.
Embodiment
Embodiment 1
Wastewater sample is the old liquid of chemical nickel plating, initial p H=4.5, composition following (g/L): Ni
2+2～6, Fe
3+0.01～0.02, Cu
2+0.2～0.6, NH
4 +70～80, contain the orthophosphite of 150～200g/L in addition, the citrate of 25～50g/L, and organism such as lactic acid.
Regulate PH=5.5 with ammoniacal liquor under the stirring at normal temperature situation, add dimethylglyoxime again and sink nickel reactant, Ni in dimethylglyoxime and the filtrate
2+Mol ratio be 2.2: 1, react 60 minutes after-filtration; Filter cake with 40～45 ℃ of hot water countercurrent washings 2 to 3 times after, obtaining purified nickel chelate through filtering again; Nickel chelate is added in 40% sulfuric acid under stirring state, separate out dimethylglyoxime, obtain nickel sulfate solution and dimethylglyoxime after the filtration; Again pickling liquor is handled, adopted activated carbon adsorption to reclaim dimethylglyoxime, through neutralization, heating hydrolysis, remove by filter residual Fe
3+After, evaporation, concentrate, crystallization, drying obtain the single nickel salt product, reach through check single nickel salt product major technique and electroplate with single nickel salt standard-required (HG/T2824-1997) requirement.Merge the filtrate in second step and adopt activated carbon adsorption to reclaim dimethylglyoxime.Merge the dimethylglyoxime circulation of reclaiming and be used for heavy nickel operation.
Embodiment 2
Wastewater sample is the old liquid of chemical nickel plating, initial p H=4.5, composition following (g/L): Ni
2+2～6, Fe
3+0.01～0.02, Cu
2+0.2～0.6, NH
4 +70～80, contain the orthophosphite of 150～200g/L in addition, the citrate of 25～50g/L, and organism such as lactic acid.
Regulate PH=9.5 with ammoniacal liquor under the stirring at normal temperature situation, add dimethylglyoxime again and sink nickel reactant, Ni in dimethylglyoxime and the filtrate
2+Mol ratio be 2.4: 1, react 20 minutes after-filtration; Filter cake with 85～90 ℃ of hot water countercurrent washings 2 to 3 times after, obtaining purified nickel chelate through filtering again; Nickel chelate is added in 10% sulfuric acid under stirring state, separate out dimethylglyoxime, obtain nickel sulfate solution and dimethylglyoxime after the filtration; Again pickling liquor is handled, adopted activated carbon adsorption to reclaim dimethylglyoxime, through neutralization, heating hydrolysis, remove by filter residual Fe
3+After, evaporation, concentrate, crystallization, drying obtain the single nickel salt product, reach through check single nickel salt product major technique and electroplate with single nickel salt standard-required (HG/T2824-1997) requirement.Merge the filtrate in second step and adopt activated carbon adsorption to reclaim dimethylglyoxime.Merge the dimethylglyoxime circulation of reclaiming and be used for heavy nickel reactant.
Embodiment 3
Wastewater sample is the old liquid of chemical nickel plating, initial p H=4.5, composition following (g/L): Ni
2+2～6, Fe
3+0.01～0.02, Cu
2+0.2～0.6, NH
4 +70～80, contain the orthophosphite of 150～200g/L in addition, the citrate of 25～50g/L, and organism such as lactic acid.
Regulate PH=7.0 with ammoniacal liquor under the stirring at normal temperature situation, add dimethylglyoxime again and sink nickel reactant, Ni in dimethylglyoxime and the filtrate
2+Mol ratio be 2.3: 1, react 30 minutes after-filtration; Filter cake with 80～90 ℃ of hot water countercurrent washings 2 to 3 times after, obtaining purified nickel chelate through filtering again; Nickel chelate is added in 25% sulfuric acid under stirring state, separate out dimethylglyoxime, obtain nickel sulfate solution and dimethylglyoxime after the filtration; Again pickling liquor is handled, adopted activated carbon adsorption to reclaim dimethylglyoxime, through neutralization, heating hydrolysis, remove by filter residual Fe
3+After, evaporation, concentrate, crystallization, drying obtain the single nickel salt product, reach through check single nickel salt product major technique and electroplate with single nickel salt standard-required (HG/T2824-1997) requirement.Merge the filtrate in second step and adopt activated carbon adsorption to reclaim dimethylglyoxime.Merge the dimethylglyoxime circulation of reclaiming and be used for heavy nickel reactant.
Embodiment 4
Wastewater sample is the old liquid of chemical nickel plating, initial p H=4.5, composition following (g/L): Ni
2+2～6, Fe
3+0.01～0.02, Cu
2+0.2～0.6, NH
4 +70～80, contain the orthophosphite of 150～200g/L in addition, the citrate of 25～50g/L, and organism such as lactic acid.
Regulate PH=7.5 with ammoniacal liquor under the stirring at normal temperature situation, add dimethylglyoxime again and sink nickel reactant, Ni in dimethylglyoxime and the filtrate
2+Mol ratio be 2.3: 1, react 35 minutes after-filtration; Filter cake with 70～75 ℃ of hot water countercurrent washings 2 to 3 times after, obtaining purified nickel chelate through filtering again; Nickel chelate is added in 30% sulfuric acid under stirring state, separate out dimethylglyoxime, obtain nickel sulfate solution and dimethylglyoxime after the filtration; Again pickling liquor is handled, adopted activated carbon adsorption to reclaim dimethylglyoxime, through neutralization, heating hydrolysis, remove by filter residual Fe
3+After, evaporation, concentrate, crystallization, drying obtain the single nickel salt product, reach through check single nickel salt product major technique and electroplate with single nickel salt standard-required (HG/T2824-1997) requirement.Merge the filtrate in second step and adopt activated carbon adsorption to reclaim dimethylglyoxime.Merge the dimethylglyoxime remittance circulation of reclaiming and be used for heavy nickel reactant.
Embodiment 5
Wastewater sample is the old liquid of chemical nickel plating, initial p H=4.5, composition following (g/L): Ni
2+2～6, Fe
3+0.01～0.02, Cu
2+0.2～0.6, NH
4 +70～80, contain the orthophosphite of 150～200g/L in addition, the citrate of 25～50g/L, and organism such as lactic acid.
Regulate PH=6.5 with ammoniacal liquor under the stirring at normal temperature situation, add dimethylglyoxime again and sink nickel reactant, Ni in dimethylglyoxime and the filtrate
2+Mol ratio be 2.3: 1, react 35 minutes after-filtration; Filter cake with 75～80 ℃ of hot water countercurrent washings 2 to 3 times after, obtaining purified nickel chelate through filtering again; Nickel chelate is added in 20% sulfuric acid under stirring state, separate out dimethylglyoxime, obtain nickel sulfate solution and dimethylglyoxime after the filtration; Again pickling liquor is handled, adopted activated carbon adsorption to reclaim dimethylglyoxime, through neutralization, heating hydrolysis, remove by filter residual Fe
3+After, evaporation, concentrate, crystallization, drying obtain the single nickel salt product, reach through check single nickel salt product major technique and electroplate with single nickel salt standard-required (HG/T2824-1997) requirement.Merge the filtrate in second step and adopt activated carbon adsorption to reclaim dimethylglyoxime.Merge the dimethylglyoxime circulation of reclaiming and be used for heavy nickel reactant.
Embodiment 6
Adopt the ammoniacal liquor among sodium hydroxide alternate embodiment 1～embodiment 6, processing condition are constant.
Claims (5)
1, a kind of nickel-containing wastewater treatment technology is characterized in that:
1.1 nickel-containing waste water is regulated PH=5.5～9.5 with sodium hydroxide or ammoniacal liquor;
1.2 normal temperature stirs down and adds dimethylglyoxime and sink nickel reactant, Ni in dimethylglyoxime and the filtrate
2+Mol ratio be 2.2: 1～2.4: 1, react 20～60 minutes after-filtration, filter cake obtains purified nickel chelate more after filtration with 40～90 ℃ of hot washes;
1.3 nickel chelate according to product requirement, dissolves with hydrochloric acid, sulfuric acid or nitric acid, can obtain corresponding nickel salt solution and dimethylglyoxime after the filtration;
1.4 sour lixiviation liquid after reclaiming dimethylglyoxime, again through neutralization, heating hydrolysis, remove by filter residual Fe
3+After, evaporation, washing, crystallization, drying obtain product;
1.5 merge the filtrate in second step and reclaim dimethylglyoxime; The dimethylglyoxime circulation of reclaiming is used for heavy nickel reactant.
2, nickel-containing wastewater treatment technology according to claim 1 is characterized in that: preferred PH=6.5～7.5 when regulating with sodium hydroxide or ammoniacal liquor.
3, nickel-containing wastewater treatment technology according to claim 1 is characterized in that: preferred ammoniacal liquor.
4, nickel-containing wastewater treatment technology according to claim 1 is characterized in that: the hot water temperature is preferred 80～90 ℃ during filter cake washing.
5, nickel-containing wastewater treatment technology according to claim 1 is characterized in that: adopt countercurrent washing during filter cake washing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100118498A CN101580317A (en) | 2009-06-01 | 2009-06-01 | Nickel-containing wastewater treatment technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100118498A CN101580317A (en) | 2009-06-01 | 2009-06-01 | Nickel-containing wastewater treatment technology |
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|---|---|
| CN101580317A true CN101580317A (en) | 2009-11-18 |
Family
ID=41362656
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|---|---|---|---|
| CNA2009100118498A Pending CN101580317A (en) | 2009-06-01 | 2009-06-01 | Nickel-containing wastewater treatment technology |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101892389A (en) * | 2010-07-14 | 2010-11-24 | 王昊杨 | Method for preparing nano metallic nickel in spent electroless nickel plating solution |
| CN101923049A (en) * | 2010-03-10 | 2010-12-22 | 田农 | Quick detection of nickel plating waste water in production before discharge |
| WO2011027094A1 (en) * | 2009-09-02 | 2011-03-10 | Hill, Marcus John | Nickel recovery from waste material with oxime complexants |
| CN102120659A (en) * | 2011-01-31 | 2011-07-13 | 无锡市霄鹰环境科技有限公司 | Method for removing nickel in chemical nickel-plating wastewater |
| CN104291498A (en) * | 2014-11-03 | 2015-01-21 | 昆山市千灯三废净化有限公司 | Processing method and corresponding processing system for chemical nickel plating waste liquid containing nitric acids |
| CN111129634A (en) * | 2019-12-06 | 2020-05-08 | 深圳清华大学研究院 | Method for separating and recovering anode material of failed ternary lithium ion battery |
| CN111646557A (en) * | 2020-02-27 | 2020-09-11 | 清上(苏州)环境科技有限公司 | Heavy metal nickel recapture agent and preparation method and application thereof |
| CN114031103A (en) * | 2021-11-22 | 2022-02-11 | 湖南工程学院 | Method for preparing spherical barium sulfate from chemical nickel plating waste liquid |
| CN115427356A (en) * | 2020-02-28 | 2022-12-02 | 东友精细化工有限公司 | Method for preparing precursor material for positive active material and positive active material for lithium secondary battery, and positive active material for lithium secondary battery prepared thereby |
| EP4112556A4 (en) * | 2020-02-28 | 2023-09-06 | Dongwoo Fine-Chem Co., Ltd. | Methods for manufacturing positive electrode active material precursor material and positive electrode active material for secondary lithium battery, and positive electrode active material for secondary lithium battery manufactured thereby |
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2009
- 2009-06-01 CN CNA2009100118498A patent/CN101580317A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011027094A1 (en) * | 2009-09-02 | 2011-03-10 | Hill, Marcus John | Nickel recovery from waste material with oxime complexants |
| CN101923049A (en) * | 2010-03-10 | 2010-12-22 | 田农 | Quick detection of nickel plating waste water in production before discharge |
| CN101892389A (en) * | 2010-07-14 | 2010-11-24 | 王昊杨 | Method for preparing nano metallic nickel in spent electroless nickel plating solution |
| CN102120659A (en) * | 2011-01-31 | 2011-07-13 | 无锡市霄鹰环境科技有限公司 | Method for removing nickel in chemical nickel-plating wastewater |
| CN104291498A (en) * | 2014-11-03 | 2015-01-21 | 昆山市千灯三废净化有限公司 | Processing method and corresponding processing system for chemical nickel plating waste liquid containing nitric acids |
| CN104291498B (en) * | 2014-11-03 | 2016-04-06 | 昆山市千灯三废净化有限公司 | A kind for the treatment of process of chemical nickel plating waste solution containing nitric acid and the treatment system of correspondence |
| CN111129634A (en) * | 2019-12-06 | 2020-05-08 | 深圳清华大学研究院 | Method for separating and recovering anode material of failed ternary lithium ion battery |
| CN111129634B (en) * | 2019-12-06 | 2021-03-30 | 深圳清华大学研究院 | Method for separating and recovering anode material of failed ternary lithium ion battery |
| CN111646557A (en) * | 2020-02-27 | 2020-09-11 | 清上(苏州)环境科技有限公司 | Heavy metal nickel recapture agent and preparation method and application thereof |
| CN115427356A (en) * | 2020-02-28 | 2022-12-02 | 东友精细化工有限公司 | Method for preparing precursor material for positive active material and positive active material for lithium secondary battery, and positive active material for lithium secondary battery prepared thereby |
| EP4112556A4 (en) * | 2020-02-28 | 2023-09-06 | Dongwoo Fine-Chem Co., Ltd. | Methods for manufacturing positive electrode active material precursor material and positive electrode active material for secondary lithium battery, and positive electrode active material for secondary lithium battery manufactured thereby |
| EP4112557A4 (en) * | 2020-02-28 | 2023-09-06 | Dongwoo Fine-Chem Co., Ltd. | Methods for preparing cathode active material precursor material and cathode active material for lithium secondary battery, and cathode active material for lithium secondary battery prepared according to same |
| CN114031103A (en) * | 2021-11-22 | 2022-02-11 | 湖南工程学院 | Method for preparing spherical barium sulfate from chemical nickel plating waste liquid |
| CN114031103B (en) * | 2021-11-22 | 2023-12-05 | 湖南工程学院 | Method for preparing spherical barium sulfate from chemical nickel plating waste liquid |
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