CN102531233A - Heavy-metal-containing electroplating wastewater treatment and heavy metal recycling method - Google Patents
Heavy-metal-containing electroplating wastewater treatment and heavy metal recycling method Download PDFInfo
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- CN102531233A CN102531233A CN201110431946XA CN201110431946A CN102531233A CN 102531233 A CN102531233 A CN 102531233A CN 201110431946X A CN201110431946X A CN 201110431946XA CN 201110431946 A CN201110431946 A CN 201110431946A CN 102531233 A CN102531233 A CN 102531233A
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Abstract
The invention discloses a heavy-metal-containing electroplating wastewater treatment and heavy metal recycling method, which includes the following steps: low-concentration electroplating wastewater containing heavy metal ions is led to pass through ion exchange resin, the heavy metal ions contained in the electroplating wastewater are led to be completely absorbed by the ion exchange resin, and clean water is extracted until absorption of the ion exchange resin reaches saturation; eluent is added to lead the heavy metal ions absorbed by the ion exchange resin to be separated from the the ion exchange resin so as to produce high-concentration electroplating wastewater; a reductant is then added to the high-concentration electroplating wastewater for reduction reaction to obtain water-insoluble reduction products containing heavy metal ions; a flocculant is added to accelerate coagulation of the reduction products; finally, the methods such as filtration and centrifugation are adopted to separate sediment, and heavy metal materials are recycled through high-temperature calcinations to serve as useful industrial raw materials. The heavy-metal-containing electroplating wastewater treatment and heavy metal recycling method has the advantages of being low in cost, high in efficiency, strong in universality and the like, effectively reduces secondary pollution, and is suitable for being widely used in the electroplating and electronic industries.
Description
Technical field
The present invention relates to the electroplating waste water treatment technology field, particularly a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal.
Background technology
Electroplating industry is the important processing industry of China, is main with zinc-plated, copper facing, cadmium plating, nickel plating and chromium plating at present, concentrates to be distributed in the industrial circles such as machine manufacturing, light industry, electronics, aerospace and instrument.It is reported that the waste water that the annual discharging of national electroplating industry contains heavy metal causes the severe contamination of rivers,lakes and seas more than 400,000,000 tons.And electroplating wastewater processing mainly is only to satisfy the environmental requirement of current increasingly stringent in recent years.
Electroplating effluent treatment method commonly used both at home and abroad at present mainly contains chemical method, electrolytic process, ion exchange method, membrane separation process and microbial method etc., and all there are some drawbacks in these technologies in practical application:
1, the heavy metal concentration of electroplating wastewater is low usually, the water body treatment capacity is big, and it is big to cause adding pharmaceutical quantities, is prone to cause secondary pollution;
2, the Processes and apparatus floor space is big, and running cost, fixed investment are bigger;
3, technological operation is complicated, and processing condition are unstable, the difficult control of operation;
4, the treatment process of these heavy metal wastewater therebies all is a kind of pollution transportation; Dissolved heavy metal in the waste water is changed into deposition or more easy-to-handle form; Take landfill to dispose to these materials; Heavy metal usually causes the pollution to underground water and surface water to the harm of environment long-term existence still, need pay bigger cost and administer these pollutions.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art; A kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal is provided; Be a kind of efficient, low-cost and effectively avoid the heavy metal-containing electroplating effluent of secondary pollution to handle and the heavy metal recoverying and utilizing method, be particularly suitable for handling low concentration heavy metal water.
Technical scheme of the present invention is:
A kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal is characterized in that the steps include:
1) IX richness is gathered: lower concentration electroplating wastewater and the ion exchange resin that will contain heavy metal ion carries out richly after the ion exchange reaction gathering the electroplating wastewater for high density;
2) precipitate reduction reclaims: the high-concentration electroplating wastewater that step 1 richness is gathered reduces-precipitation process, reclaims heavy metal reaction product wherein.
Gather in the step in the IX richness, said ion exchange reaction comprises:
1) absorption reaction: make heavy metal ion contained in the electroplating wastewater be adsorbed in ion exchange resin fully and isolate clean water, reach capacity until the absorption of ion exchange resin;
2) elution of reactive: add elutriant and make the heavy metal ion that is adsorbed in ion exchange resin break away from ion exchange resin and the electroplating wastewater of output high density.
Said elutriant is a strong base solution.
Said ion exchange resin is the D301 macroreticular weakly base resin, processing be the electroplating wastewater that contains heavy metal chromium, the step of handling the electroplating wastewater contain heavy metal chromium comprises:
1) said ion exchange resin carries out pre-treatment
A, fresh ion exchange resin is soaked with deionized water;
B, soak with strong acid solution;
C, extremely neutral with washed with de-ionized water;
D, soak with strong base solution again;
E, be washed till neutrality with deionized water, subsequent use;
2) said absorption reaction is a dynamic adsorption
Slowly inject from the upper end of ion exchange unit under earlier pretreated wet ion exchange resin constantly being stirred in processing vessel; In case bubble is arranged, need refitting, keep the water surface to exceed ion exchange resin 2-3cm; Exchange is measured then, and exchange is measured and comprised the following steps:
A, adjusting flow velocity: slowly inject ion exchange unit with deionized water, the control constant flow rate;
B, exchange: will contain Cr
6+Electroplating wastewater injects ion exchange unit, and collects effluent, measures its Cr
6+Concentration;
C, reach exchange equilibrium until ion exchange resin, this moment, the concentration of effluent sexavalence Cr approached the into concentration of water sexavalence Cr;
3) said elution of reactive is a dynamic desorption
A, injection strong base solution are collected effluent, measure its Cr
6+Concentration;
B, record data are up to effluent Cr
6+Concentration constant basically, calculation result.
Said ion exchange resin is Zeo-karb, handles the electroplating wastewater of nickeliferous, cadmium, copper etc.
Said precipitate reduction recovering step comprises:
1) precipitate reduction: add reductive agent to described high-concentration electroplating wastewater and carry out reduction reaction, obtain the water-fast reduzate that contains heavy metal ion, add flocculation agent and accelerate the reduzate coagulation;
2) solid-liquid separation: throw out is separated through filtration or centrifugal mode;
3) high-temperature calcination: the material that contains said heavy metal ion is reclaimed in the throw out high-temperature calcination use as industrial raw material.
Said reductive agent is a sodium sulphite, and said reduction reaction is the thorough mixing reaction under agitation condition, and temperature is 650-750 degree centigrade in the processing condition of said high-temperature calcination.
The invention has the beneficial effects as follows:
The method that the present invention gathers through the IX richness will contain heavy metal chromium, nickel, cadmium, the isoionic lower concentration electroplating wastewater of copper richness and gather the electroplating wastewater for high density, significantly reduce the waste water scale of construction; Waste water with high density carries out the precipitate reduction recycling again, has reduced dosage, has reduced running cost; Improve processing efficiency; Industrial raw material is made in the heavy metal waste slag recycling utilized again, both avoided the plurality of heavy metal waste residue to pile up the secondary pollution that brings, increased the added value of producing again.
Adopt ion-exchange-resin process; To low concentration solution absorption have the adsorption efficiency height, running cost is low, effluent quality good, and advantage such as recyclable useful matter is after adsorb saturated ion exchange resin and passing through elution of reactive; Reply the unsaturation state; Thereby do further to recycle, the water outlet after the absorption reaches discharging standards fully, can return in the production as the rinse water utilization.
The present invention proposes " two-step approach " new process for treating waste water, proposed first, reduced the spent process water scale of construction and dosage, reduced running cost and reduce secondary pollution greatly with D301 resin absorption Cr (VI).Expensive, the low efficiency problem of traditional chemical reduction method processing waste water containing chrome have been solved.The resource technology that adopts heavy metal to recycle had both been avoided the long-pending secondary pollution that brings of a large amount of chromium slag mucks, had increased the added value of producing again.
The present invention's technology highly versatile; Substitute the electroplating wastewater of heavy metal ion such as the D301 resin is nickeliferous with regard to handling, cadmium, copper with Zeo-karb, adopt the remove rate of these heavy metal ion of ion exchange resin treatment of the present invention in waste water all up to 99.99%.
To sum up, technology of the present invention has that cost is low, efficient is high and advantage such as highly versatile, effectively reduces secondary pollution, is adapted at electroplating, the electron trade widespread use.
Description of drawings
Fig. 1 is the process flow sheet of the embodiment of the invention;
Fig. 2 is an embodiment of the invention dynamic desorption curve synoptic diagram;
Fig. 3 is a typical curve synoptic diagram in the embodiment of the invention spectrophotometry.
Embodiment
Electroplating wastewater processing and the heavy metal recoverying and utilizing method that contains heavy metal according to the invention comprises the following steps:
1, IX richness is gathered: the lower concentration electroplating wastewater that will contain heavy metal ion such as chromium, nickel, cadmium, copper through with the ion exchange reaction of ion exchange resin, richness is gathered the electroplating wastewater for high density.Comprise specifically:
1) absorption reaction: make heavy metal substance contained in the electroplating wastewater be adsorbed in ion exchange resin fully and isolate clean water, reach capacity until the absorption of ion exchange resin;
2) elution of reactive: add elutriant and make the heavy metal substance that is adsorbed in ion exchange resin break away from ion exchange resin and the electroplating wastewater of output high density.Wherein elutriant is strong base solution such as NaOH solution; When processing contains the electroplating wastewater of heavy metal chromium; Ion exchange resin is the D301 macroreticular weakly base resin, when handling the electroplating wastewater of heavy metal ion such as nickeliferous, cadmium, copper, substitutes the D301 resin with Zeo-karb and just gets final product.
2, precipitate reduction reclaims: the high-concentration electroplating wastewater that step 1 richness is gathered reduces-precipitation process, reclaims heavy metal substance wherein.
The precipitate reduction recovering step comprises:
1) precipitate reduction: add reductive agent to described high-concentration electroplating wastewater and carry out reduction reaction, get the water-fast reduzate that contains heavy metal substance, add flocculation agent and accelerate the reduzate coagulation;
2) solid-liquid separation: throw out is separated through method such as filtering or centrifugal;
3) high-temperature calcination: the throw out high-temperature calcination is reclaimed heavy metal substance as the useful industrial raw material.Wherein reductive agent is a sodium sulphite, and reduction reaction is the thorough mixing reaction under agitation condition.In the processing condition of high-temperature calcination temperature 650-750 degree centigrade.
Introduce as follows in detail with the example that is recycled as of the electroplating wastewater that contains heavy metal chromium and heavy metal chromium below in conjunction with accompanying drawing:
1, material and device
(1) material: D301 macroreticular weakly base resin, Poly aluminum Chloride (PAC) (PAC), SEPIGEL 305 (PAM).
(2) analytical reagent: SRM 935a, 1:1 sulfuric acid, 1:1 phosphoric acid, 1% diphenylcarbazide.
(3) instrument: electronic balance (200g/0.01g), ultraviolet-visible pectrophotometer, PH meter, magnetic stirrer, ion exchange unit one cover.
2, process
Spent ion exchange resin gathers the low-concentration chromate waste water richness: absorption has the adsorption efficiency height to low concentration solution, running cost is low, effluent quality good to adopt ion-exchange-resin process, and advantage such as recyclable useful matter.
Ion exchange process is expressed with following two equations:
(1) absorption reaction:
(2) elution of reactive:
（2）
2.1, the pre-treatment of resin
A, fresh resin was soaked 24 hours with deionized water;
B, with 0.5 mol/L HCI solution soaking 0.5h;
C, extremely neutral with washed with de-ionized water;
D, use 0.5 mol/L NaOH solution soaking 0.5h again;
E, be washed till neutrality with deionized water, subsequent use.
2.2, dynamic adsorption
1) dress post (promptly being ion exchange unit): pretreated wet resin constantly stirred in processing vessel slowly inject from the upper end of post down in the post to about 2/3 post (in case bubble is arranged, needing refitting), the maintenance water surface exceeds resin 2-3cm.
2) exchange is measured:
A, adjusting flow velocity: slowly inject post with deionized water, regulating piston, control constant flow rate;
B, exchange: 100 mol/L sexavalence Cr solution (promptly being electroplating wastewater) are injected exchange column (promptly being ion exchange unit), and press certain volume and collect effluent, measure its Cr
6+Concentration;
C, reach exchange equilibrium, stop to contain the injection (this moment, the concentration of effluent sexavalence Cr approached the into concentration of water sexavalence Cr) of the electroplating wastewater of sexavalence Cr until resin.
2.3, dynamic desorption
1) makes elutriant with 1.25 mol/L NaOH solution, press certain volume and collect effluent, measure its Cr
6+Concentration, record data, constant basically up to the concentration of effluent sexavalence Cr, stop the adding of elutriant;
2) make elution curve, calculate its regeneration efficiency, like Fig. 2.
2.4, chemical reduction method: the sexavalence Cr waste water that contains of high density is reduced to Cr
3+
1) in processing vessel, adds the sodium sulphite of 1.5 times of theoretical requirements;
2) begin slowly to stir with magnetic stirring apparatus, treat to increase gradually when sodium sulphite dissolves fully stir speed (S.S.), stir 0.5h;
3) after reaction finishes, splash into 1-2 and drip flocculation agent, shake up, leave standstill moments later and filter;
4) cross the filter residue oven dry and weigh, get the concentration that supernatant detects sexavalence Cr.
2.5, high-temperature calcination prepares Cr
2O
3
Filtering separation Cr (OH)
3Deposition with throw out 700 ℃ of calcinings in muffle furnace, gets Cr
2O
3
2.6, analytical procedure
Standard method: diphenyl carbazide spectrophotometry;
Draw through the absorbancy of blank correction typical curve sexavalence Cr concentration, like Fig. 3:
Typical curve equation: Abs=0.348C regression coefficient: R
2=0.9997.
Can know that through above-mentioned treating processes the present invention has following effect:
1) with the flow of D301 resin with 20ml/min, continuous adsorption concentration is the chromate waste water 7.5h of 100mg/L, can not detect sexavalence Cr in the water outlet, and sexavalence Cr clearance reaches discharging standards fully up to 99.99%;
2) with the saturated D301 resin of 5% NaOH wash-out absorption, exchange column water outlet sexavalence Cr concentration is up to 6918.74mg/L, and eluting rate is 96.37%.
3) use Na
2S9H
2O adds with 2 times of theoretical values, and the sexavalence Cr waste water that contains of 3073.21 mg/L is reduced to Cr
3+, reduction ratio is 99.67%.
4) reclaim Cr through high-temperature calcination
2O
3As industrial raw material.
Claims (10)
1. an electroplating wastewater processing and a heavy metal recoverying and utilizing method that contains heavy metal is characterized in that the steps include:
1) IX richness is gathered: lower concentration electroplating wastewater and the ion exchange resin that will contain heavy metal ion carries out richly after the ion exchange reaction gathering the electroplating wastewater for high density;
2) precipitate reduction reclaims: the high-concentration electroplating wastewater that step 1 richness is gathered reduces-precipitation process, reclaims heavy metal reaction product wherein.
2. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 1 is characterized in that gathering in the step in the IX richness, and said ion exchange reaction comprises:
1) absorption reaction: make heavy metal ion contained in the electroplating wastewater be adsorbed in ion exchange resin fully and isolate clean water, reach capacity until the absorption of ion exchange resin;
2) elution of reactive: add elutriant and make the heavy metal ion that is adsorbed in ion exchange resin break away from ion exchange resin and the electroplating wastewater of output high density.
3. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 2, it is characterized in that: said elutriant is a strong base solution.
4. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 3, it is characterized in that: said ion exchange resin is the D301 macroreticular weakly base resin, processing be the electroplating wastewater that contains heavy metal chromium.
5. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 4 is characterized in that:
1) said ion exchange resin carries out pre-treatment
A, fresh ion exchange resin is soaked with deionized water;
B, soak with strong acid solution;
C, extremely neutral with washed with de-ionized water;
D, soak with strong base solution again;
E, be washed till neutrality with deionized water, subsequent use;
2) said absorption reaction is a dynamic adsorption
Slowly inject from the upper end of ion exchange unit under earlier pretreated wet ion exchange resin constantly being stirred in processing vessel; In case bubble is arranged, need refitting, keep the water surface to exceed ion exchange resin 2-3cm; Exchange is measured then, and exchange is measured and comprised the following steps:
A, adjusting flow velocity: slowly inject ion exchange unit with deionized water, the control constant flow rate;
B, exchange: will contain Cr
6+Electroplating wastewater injects ion exchange unit, and collects effluent, measures its Cr
6+Concentration;
C, reach exchange equilibrium until ion exchange resin, this moment, the concentration of effluent sexavalence Cr approached the into concentration of water sexavalence Cr;
3) said elution of reactive is a dynamic desorption
A, injection strong base solution are collected effluent, measure its Cr
6+Concentration;
B, record data are up to effluent Cr
6+Concentration constant basically, calculation result.
6. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 2, it is characterized in that: said ion exchange resin is Zeo-karb, handles the electroplating wastewater of nickeliferous, cadmium, copper etc.
7. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 1 is characterized in that said precipitate reduction recovering step comprises:
1) precipitate reduction: add reductive agent to described high-concentration electroplating wastewater and carry out reduction reaction, obtain the water-fast reduzate that contains heavy metal ion, add flocculation agent and accelerate the reduzate coagulation;
2) solid-liquid separation: throw out is separated through filtration or centrifugal mode;
3) high-temperature calcination: the material that contains said heavy metal ion is reclaimed in the throw out high-temperature calcination use as industrial raw material.
8. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 7, it is characterized in that: said reductive agent is a sodium sulphite.
9. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 7 is characterized in that: said reduction reaction is the thorough mixing reaction under agitation condition.
10. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 7, it is characterized in that: temperature is 650-750 degree centigrade in the processing condition of said high-temperature calcination.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086545A (en) * | 2013-02-28 | 2013-05-08 | 曾嵘斌 | Method and device for removing and recovering heavy metal in waste water through regenerated active carbon |
| CN103991935A (en) * | 2014-06-10 | 2014-08-20 | 四川农业大学 | Method for efficiently removing copper ions from electroplating wastewater |
| CN105481147A (en) * | 2016-01-19 | 2016-04-13 | 青岛大学 | Synchronous decoloration and nitrogen recovery method and equipment for high-concentration printing waste liquids |
| CN106622402A (en) * | 2016-12-19 | 2017-05-10 | 马鞍山中创环保科技有限公司 | Ion exchange fiber for electroplating wastewater treatment and electroplating wastewater treatment method |
| CN106757150A (en) * | 2016-11-16 | 2017-05-31 | 天津碧水源膜材料有限公司 | A kind of method that copper in contained waste liquid is reclaimed using absorption and electro-deposition group technology |
| CN107487812A (en) * | 2017-09-02 | 2017-12-19 | 长沙埃比林环保科技有限公司 | A kind of Treating Electroplate Wastewater Containing Nickel exchanges membrane processing method |
| WO2018177221A1 (en) * | 2017-03-27 | 2018-10-04 | 福建欣宇卫浴科技股份有限公司 | Treatment system for wastewater containing chromium |
| WO2018177222A1 (en) * | 2017-03-27 | 2018-10-04 | 福建欣宇卫浴科技股份有限公司 | System and process for treating for wastewater containing chromium |
| CN112811695A (en) * | 2021-01-12 | 2021-05-18 | 洛阳国联新材料研究院有限公司 | Electroplating wastewater zero-liquid discharge system and process |
| CN112960837A (en) * | 2021-03-25 | 2021-06-15 | 洛阳国联新材料研究院有限公司 | Electroplating wastewater zero-liquid discharge system and process |
| CN115595451A (en) * | 2022-09-23 | 2023-01-13 | 安徽皖东树脂科技有限公司（Cn） | Method for recovering gold from gold-plating wastewater |
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| CN103086545A (en) * | 2013-02-28 | 2013-05-08 | 曾嵘斌 | Method and device for removing and recovering heavy metal in waste water through regenerated active carbon |
| CN103991935A (en) * | 2014-06-10 | 2014-08-20 | 四川农业大学 | Method for efficiently removing copper ions from electroplating wastewater |
| CN103991935B (en) * | 2014-06-10 | 2015-10-21 | 四川农业大学 | A kind of method removing Copper in Electroplating Waste Water ion |
| CN105481147A (en) * | 2016-01-19 | 2016-04-13 | 青岛大学 | Synchronous decoloration and nitrogen recovery method and equipment for high-concentration printing waste liquids |
| CN106757150A (en) * | 2016-11-16 | 2017-05-31 | 天津碧水源膜材料有限公司 | A kind of method that copper in contained waste liquid is reclaimed using absorption and electro-deposition group technology |
| CN106622402A (en) * | 2016-12-19 | 2017-05-10 | 马鞍山中创环保科技有限公司 | Ion exchange fiber for electroplating wastewater treatment and electroplating wastewater treatment method |
| WO2018177221A1 (en) * | 2017-03-27 | 2018-10-04 | 福建欣宇卫浴科技股份有限公司 | Treatment system for wastewater containing chromium |
| WO2018177222A1 (en) * | 2017-03-27 | 2018-10-04 | 福建欣宇卫浴科技股份有限公司 | System and process for treating for wastewater containing chromium |
| CN107487812A (en) * | 2017-09-02 | 2017-12-19 | 长沙埃比林环保科技有限公司 | A kind of Treating Electroplate Wastewater Containing Nickel exchanges membrane processing method |
| CN112811695A (en) * | 2021-01-12 | 2021-05-18 | 洛阳国联新材料研究院有限公司 | Electroplating wastewater zero-liquid discharge system and process |
| CN112960837A (en) * | 2021-03-25 | 2021-06-15 | 洛阳国联新材料研究院有限公司 | Electroplating wastewater zero-liquid discharge system and process |
| CN115595451A (en) * | 2022-09-23 | 2023-01-13 | 安徽皖东树脂科技有限公司（Cn） | Method for recovering gold from gold-plating wastewater |
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| CN102531233B (en) | 2013-11-06 |
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