CN102531233B - 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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- CN102531233B CN102531233B CN 201110431946 CN201110431946A CN102531233B CN 102531233 B CN102531233 B CN 102531233B CN 201110431946 CN201110431946 CN 201110431946 CN 201110431946 A CN201110431946 A CN 201110431946A CN 102531233 B CN102531233 B CN 102531233B
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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, at present take zinc-plated, copper facing, cadmium plating, nickel plating and chromium plating as main, concentrates to be distributed in the industrial circles such as manufacture, light industry, electronics, aerospace and instrument.It is reported, 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 is mainly only to satisfy the environmental requirement of current increasingly stringent in recent years.
The electroplating effluent treatment method of commonly using 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 actual applications in these techniques:
1, the heavy metal concentration of electroplating wastewater is low usually, the water body treatment capacity is large, causes adding pharmaceutical quantities large, easily causes secondary pollution;
2, the Processes and apparatus floor space is large, and running cost, fixed investment are larger;
3, complex operation, processing condition are unstable, operate more difficult control;
4, the treatment process of these heavy metal wastewater therebies is all a kind of pollution transportation, the heavy metal that dissolves in waste water is changed into precipitation or more easy-to-handle form, take landfill to dispose to these materials, heavy metal is to the harm of environment long-term existence still, usually cause the pollution to underground water and surface water, need to pay larger cost and administer these pollutions.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the 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 process and the heavy metal recoverying and utilizing method, be particularly suitable for processing 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) ion-exchange is rich poly-: rich gathering be the electroplating wastewater of high density after the lower concentration electroplating wastewater that will contain heavy metal ion carries out ion exchange reaction with ion exchange resin;
2) precipitate reduction reclaims: the high-concentration electroplating wastewater that step 1 richness is poly-reduces-precipitation process, reclaims heavy metal reaction product wherein.
In the rich poly-step of ion-exchange, described ion exchange reaction comprises:
1) absorption reaction: make heavy metal ion contained in electroplating wastewater be adsorbed in ion exchange resin fully and isolate clean water, until the absorption of ion exchange resin reaches capacity;
2) elution of reactive: add elutriant to make to be adsorbed in the heavy metal ion of ion exchange resin to break away from ion exchange resin and the electroplating wastewater of output high density.
Described elutriant is strong base solution.
Described ion exchange resin is the D301 macroreticular weakly base resin, processing be the electroplating wastewater that contains heavy metal chromium, the step of processing the electroplating wastewater contain heavy metal chromium comprises:
1) described 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, standby;
2) described absorption reaction is dynamic adsorption
Slowly inject from the upper end of ion exchange unit under first 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, then exchange is measured, and exchange is measured and comprised the following steps:
A, regulate flow velocity: slowly in the ion switch, coutroi velocity is constant with deionized water;
B, exchange: will contain Cr
6+In electroplating wastewater ion switch, and collect effluent liquid, measure its Cr
6+Concentration;
C is until ion exchange resin reaches exchange equilibrium, and the concentration of effluent liquid sexavalence Cr is close to the concentration of water inlet sexavalence Cr at this moment;
3) described elution of reactive is dynamic desorption
A, injection strong base solution are collected effluent liquid, measure its Cr
6+Concentration;
B, record data are until effluent liquid Cr
6+Concentration substantially constant, calculation result.
Described ion exchange resin is Zeo-karb, processes the electroplating wastewater of nickeliferous, cadmium, copper etc.
Described precipitate reduction recycling 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 to accelerate the reduzate coagulation;
2) solid-liquid separation: throw out is separated by filtration or centrifugal mode;
3) high-temperature calcination: the material that contains described heavy metal ion is reclaimed in the throw out high-temperature calcination use as industrial raw material.
Described reductive agent is sodium sulphite, and described reduction reaction is abundant hybrid reaction under agitation condition, and in the processing condition of described high-temperature calcination, temperature is 650-750 degree centigrade.
The invention has the beneficial effects as follows:
The present invention is by the rich poly-method of ion-exchange, to contain heavy metal chromium, nickel, cadmium, the rich poly-electroplating wastewater of high density that is of the isoionic lower concentration electroplating wastewater of copper, greatly reduced 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 recycling is made in the heavy metal waste slag recycling, both avoided the plurality of heavy metal waste residue to pile up the secondary pollution that brings, increased again the added value of producing.
Adopt ion-exchange-resin process, low concentration solution absorption is had adsorption efficiency is high, running cost is low, effluent quality is good, and the advantages such as recyclable useful matter, adsorb saturated ion exchange resin through after elution of reactive, reply the unsaturation state, thereby do further to recycle, the water outlet after absorption reaches discharging standards fully, can return in production as the rinse water utilization.
The present invention proposes " two-step approach " new process for treating waste water, proposed first with D301 resin absorption Cr (VI), reduced the processing wastewater scale of construction and dosage, greatly reduced running cost and reduce secondary pollution.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 again the added value of producing.
The technology of the present invention highly versatile, substitute the electroplating wastewater of the heavy metal ion such as the D301 resin is nickeliferous with regard to processing, 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, technique of the present invention has that cost is low, efficient is high and the 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 present invention;
Fig. 2 is embodiment of the present invention dynamic desorption curve synoptic diagram;
Fig. 3 is embodiment of the present invention spectrophotometry Plays curve synoptic diagram.
Embodiment
Electroplating wastewater processing and the heavy metal recoverying and utilizing method that contains heavy metal of the present invention comprises the following steps:
1, ion-exchange is rich poly-: the lower concentration electroplating wastewater that will contain the heavy metal ion such as chromium, nickel, cadmium, copper by with the ion exchange reaction of ion exchange resin, the rich poly-electroplating wastewater of high density that is.Comprise specifically:
1) absorption reaction: make heavy metal substance contained in electroplating wastewater be adsorbed in ion exchange resin fully and isolate clean water, until the absorption of ion exchange resin reaches capacity;
2) elution of reactive: add elutriant to make to be adsorbed in the heavy metal substance of ion exchange resin to 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 processing the electroplating wastewater of the 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 poly-reduces-precipitation process, reclaims heavy metal substance wherein.
The precipitate reduction recycling 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 to accelerate the reduzate coagulation;
2) solid-liquid separation: throw out is separated by the method such as filtering or centrifugal;
3) high-temperature calcination: the throw out high-temperature calcination is reclaimed heavy metal substance as useful industrial raw material.Wherein reductive agent is sodium sulphite, and reduction reaction is abundant hybrid reaction under agitation condition.In the processing condition of high-temperature calcination temperature 650-750 degree centigrade.
Be described in detail as follows with the electroplating wastewater that contains heavy metal chromium and the example that is recycled as of heavy metal chromium below in conjunction with accompanying drawing:
1, material and device
(1) material: D301 macroreticular weakly base resin, polymerize aluminum chloride (PAC), polyacrylamide (PAM).
(2) analytical reagent: potassium bichromate, 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 is rich poly-with low-concentration chromate waste water: absorption has that adsorption efficiency is high, running cost is low, effluent quality is good to low concentration solution to adopt ion-exchange-resin process, and the 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, standby.
2.2, dynamic adsorption
1) dress post (being namely ion exchange unit): slowly inject from the upper end of post under pretreated wet resin is constantly stirred in processing vessel in post to about 2/3 post (in case bubble is arranged, needing refitting), keep the water surface to exceed resin 2-3cm.
2) exchange is measured:
A, adjusting flow velocity: slowly inject post with deionized water, regulating piston, coutroi velocity is constant;
B, exchange: 100 mol/L sexavalence Cr solution (being namely electroplating wastewater) are injected exchange column (being namely ion exchange unit), and press certain volume and collect effluent liquid, measure its Cr
6+Concentration;
C is until resin reaches exchange equilibrium, stops containing the injection (this moment effluent liquid sexavalence Cr concentration close to the concentration of water inlet sexavalence Cr) of the electroplating wastewater of sexavalence Cr.
2.3, dynamic desorption
1) make elutriant with 1.25 mol/L NaOH solution, press certain volume and collect effluent liquid, measure its Cr
6+Concentration, record data until the concentration of effluent liquid sexavalence Cr is substantially constant, stop adding of elutriant;
2) make elution curve, calculate its regeneration efficiency, as Fig. 2.
2.4, chemical reduction method: be Cr with the sexavalence Cr wastewater reduction that contains of high density
3+
1) add the sodium sulphite of 1.5 times of theoretical requirements in the processing vessel;
2) begin slowly to stir with magnetic stirring apparatus, increase gradually stir speed (S.S.) when sodium sulphite dissolves fully, stir 0.5h;
3) reaction complete after, splash into 1-2 and drip flocculation agent, shake up, standingly filter in a moment;
4) cross the filter residue oven dry and weigh, get the concentration that supernatant liquor detects sexavalence Cr.
2.5, high-temperature calcination prepares Cr
2O
3
Filtering separation Cr (OH)
3Precipitation 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 the blank correction typical curve to sexavalence Cr concentration, as Fig. 3:
Typical curve equation: Abs=0.348C regression coefficient: R
2=0.9997.
By above-mentioned treating processes as can be known, 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, and in water outlet, inspection does not measure sexavalence Cr, and sexavalence Cr clearance reaches discharging standards fully up to 99.99%;
2) with the 5% saturated D301 resin of 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, is Cr with the sexavalence Cr wastewater reduction that contains of 3073.21 mg/L
3+, reduction ratio is 99.67%.
4) reclaim Cr by high-temperature calcination
2O
3As industrial raw material.
Claims (4)
1. electroplating wastewater processing and a heavy metal recoverying and utilizing method that contains heavy metal, is characterized in that the steps include:
The first step, ion-exchange are rich poly-: rich gathering be the electroplating wastewater of high density after the lower concentration electroplating wastewater that will contain heavy metal ion carries out ion exchange reaction with ion exchange resin;
Described ion exchange reaction comprises:
1. absorption reaction: make heavy metal ion contained in electroplating wastewater be adsorbed in ion exchange resin fully and isolate clean water, until the absorption of ion exchange resin reaches capacity;
Wherein, to carry out pre-treatment step as follows for described ion exchange resin:
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, standby;
Described absorption reaction is dynamic adsorption, and adsorption step is as follows:
Slowly inject from the upper end of ion exchange unit under first 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, then exchange is measured, and exchange is measured and comprised the following steps:
A, regulate flow velocity: slowly in the ion switch, coutroi velocity is constant with deionized water;
B, exchange: will contain Cr
6+In electroplating wastewater ion switch, and collect effluent liquid, measure its Cr
6+Concentration;
C is until ion exchange resin reaches exchange equilibrium, and the concentration of effluent liquid sexavalence Cr is close to the concentration of water inlet sexavalence Cr at this moment;
2. elution of reactive: add elutriant to make to be adsorbed in the heavy metal ion of ion exchange resin to break away from ion exchange resin and the electroplating wastewater of output high density;
Described elution of reactive is dynamic desorption, and elution step is as follows:
A, injection strong base solution are collected effluent liquid, measure its Cr
6+Concentration;
B, record data are until effluent liquid Cr
6+Concentration substantially constant, calculation result;
Second step, precipitate reduction reclaim: the rich poly-high-concentration electroplating wastewater of institute in the first step reduced-precipitation process, and recovery heavy metal reaction product wherein;
Described precipitate reduction recycling 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 to accelerate the reduzate coagulation;
2. solid-liquid separation: by filtering or centrifugal mode is separated throw out;
3. high-temperature calcination: the material that contains described heavy metal ion is reclaimed in the throw out high-temperature calcination use as industrial raw material;
Described elutriant is 1.25mol/L NaOH solution; Described ion exchange resin is the D301 macroreticular weakly base resin, processing be the electroplating wastewater that contains heavy metal chromium; Described reductive agent is sodium sulphite.
2. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 1, it is characterized in that: described ion exchange resin is Zeo-karb, processes the electroplating wastewater of nickeliferous, cadmium or copper.
3. 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: described reduction reaction abundant hybrid reaction under agitation condition.
4. a kind of electroplating wastewater processing and heavy metal recoverying and utilizing method that contains heavy metal according to claim 1, it is characterized in that: in the processing condition of described high-temperature calcination, temperature is 650-750 degree centigrade.
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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 |
| 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 |
| CN105481147B (en) * | 2016-01-19 | 2018-05-08 | 青岛大学 | A kind of high concentration stamp waste liquid synchronously decolourizes and nitrogen recovery method and equipment |
| 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 |
| CN106830489A (en) * | 2017-03-27 | 2017-06-13 | 福建欣宇卫浴科技股份有限公司 | System for processing chrome-containing wastewater |
| CN106800352A (en) * | 2017-03-27 | 2017-06-06 | 福建欣宇卫浴科技股份有限公司 | System for processing chrome-containing wastewater |
| 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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| JPS52135877A (en) * | 1976-05-10 | 1977-11-14 | Osaka Sanso Kougiyou Kk | Method of regenerating bed containing chromium |
| CN1096009A (en) * | 1993-05-31 | 1994-12-07 | 孙玉芬 | Compound for treatment of electroplating wastes |
| CN1093180C (en) * | 1996-12-30 | 2002-10-23 | 中国环境科学研究院 | One-step process of resin regeneration and chromium reduction for reclaiming chromium from electroplating waste water |
| CN1219705C (en) * | 2001-09-03 | 2005-09-21 | 陈正书 | Double-recovering circulation method for cyanic electroplating effluent and heavy metal-containing electroplating effluent |
| CN101830600B (en) * | 2010-03-23 | 2012-02-22 | 天津大学 | Method for treating comprehensive electroplating wastewater |
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