CN1899985A - Treating, recovering and reutilizing method for electroplating waste liquid containing heavy metals - Google Patents
Treating, recovering and reutilizing method for electroplating waste liquid containing heavy metals Download PDFInfo
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Abstract
The present invention relates to treatment of waste electroplating solution, and is especially method of treating waste electroplating solution containing Cu, Cr, Cd, Ni and other heavy metals and recovering heavy metals. The method includes the following steps: adding water soluble great molecular weight polymer into the waste electroplating solution to form complex of heavy metal ions, ultrafiltering to obtain concentrated liquid with enriched heavy metal ions, adding sulfuric acid to the ultrafiltrate to acidify and decomplex the heavy metal ions, ulterfiltering the decomplexed solution, returning the concentrated liquid with enriched complex agent to the complexing step, treating the ultrafiltered dialysate through reverse osmosis to obtain concentrated heavy ion solution, and returning the concentrated heavy ion solution to the electroplating step.
Description
Technical field
The present invention relates to a kind of electroplating effluent treatment process, especially relate to the processing and the heavy metal recoverying and utilizing method of the electroplating effluent of heavy metals such as a kind of cupric, chromium, cadmium, nickel.
Background technology
In today of water resources growing tension, the membrane technique that is recovered as purpose with waste water recycling and material will be more extensive as a kind of novel and water technology application of the more sophisticated ultra-filtration technique of generally attention, especially technology in wastewater treatment of being subjected to various countries water treatment person efficiently.Electroplating industry is the important processing industry of China, at present based on zinc-plated, copper facing, cadmium plating, nickel plating and chromium plating, concentrates to be distributed in the industrial circles such as machine manufacturing, light industry, electronics, aerospace and instrument.According to incompletely statistics, the annual discharging of national electroplating industry contains about 400,000,000 tons of the waste water of heavy metal, causes the severe contamination of rivers,lakes and seas.Therefore, must take measures, carry out end treatment.From electroplating effluent treatment method in recent years, mainly be the environmental requirement of satisfying current increasingly stringent, make that heavy metal wastewater thereby obtains final processing in the electroplate liquid.Water-soluble polymers complexing-ultrafiltration-decomplexing method is that chemical reaction and ultra-filtration technique are carried out the coupled new technique, will obtain from now on to develop faster; Reverse osmosis method can concentrate heavy metal wastewater thereby and be used as a kind of resource, make that heavy metal becomes value product in the waste water; Water-soluble polymers complexing-ultrafiltration-decomplexing-reverse osmosis integrating process can be realized the recovery of waste water recycling and heavy metal and the cyclic regeneration of complexing agent simultaneously, thereby this method has broad application prospects.
Method comparatively commonly used during purifying electroplating wastewater is handled has chemical method, high-voltage pulse electrolytic process, ion exchange method and biological process etc.In fact, the treatment process of these heavy metal wastewater therebies all is a kind of pollution transportation, and dissolved heavy metal in the waste water is changed into precipitation or more easy-to-handle form, to the final disposal of these materials, normally carries out landfill.Therefore, heavy metal usually causes the pollution to underground water and surface water to the harm of environment long-term existence still, and the improvement of this pollution is usually needed to pay expensive more cost.In recent years, efforts at environmental protection person constantly seeks more safety and economic method is handled heavy metal wastewater thereby, reducing or eliminating the accumulation of heavy metal in environment, and satisfies the environmental requirement of increasingly stringent.
Notification number provides a kind of cyanogen system for the patent of invention of CN1403385 and contains two round-robin methods that reclaim of heavy metal-containing electroplating effluent, it comprises the steps: that (1) retrieving arrangement exchanges: with cyanogen system and contain heavy metal-containing electroplating effluent by preliminary retrieving arrangement, its device is the ionization exchange resin, the waste water of electroplating process discharging is by behind this retrieving arrangement, resins exchange via retrieving arrangement, make the complete sorption of prussiate heavy metal substance contained in the waste water in resin and isolate clean water, this isolates clean water and delivers in the last program again, as the washing water in the electroplating process, to reach first cyclic pattern of water, and cyanogen based compound and heavy metal substance still continue to carry out in the exchange of retrieving arrangement, and whether the absorption of detecting resin with sensor has reached degree of saturation; (2) regenerator is handled: when the absorption of resin reaches when saturated, the regenerator that adds anionic nature, prussiate metallics in the state of the negatively charged ion cyanogen coating heavy metal of this prussiate breaks away from resin, make resin reply the unsaturation state, further recycle again, and the liquid that produces cyanide anion ion coated heavy metal; (3) destroy cryanide ion: the liquid of above-mentioned cyanide anion ion coated heavy metal is inserted in the electrolyzer, again with positive and negative electrode 0.5-6V voltage, 0.01-6A/dm2 current density, the state electrolysis that keeps 25-60 ℃ of temperature, destroy the cyanogen negatively charged ion that the heavy metal skin is coated, make deleterious cyanogen generate nontoxic gass such as nitrogen and carbonic acid gas, and, with the isolating heavy metal of cyanogen be that sorption is in negative potential; (4) reclaim heavy metal: with heavy metal by stripping down recovery on the negative potential.
Summary of the invention
The objective of the invention is to contain the deficiency that exists aspect the electroplating wastewater processing of heavy metal and the heavy metal recycling in processing, the reuse of heavy metal electroplating effluents such as a kind of cupric, chromium, cadmium, nickel and the recoverying and utilizing method of heavy metal are provided at existing.
Heavy metal electroplating effluents such as a kind of cupric of the present invention, chromium, cadmium, nickel are handled and the heavy metal recoverying and utilizing method, the steps include:
1) complexing: in heavy metal ion electroplating effluents such as cupric, chromium, cadmium, nickel, add complexing agent water-soluble macromolecule polymkeric substance, make itself and the effect of water-soluble macromolecule polymkeric substance form the ionic complex waste liquid;
2) ultrafiltration enrichment: the ionic complex waste liquid that will contain heavy metal ion such as copper, chromium, cadmium, nickel separates through ultrafiltration and concentration, makes the enrichment of heavy metal ion complex compound get ultrafiltration and concentration liquid, and dialyzate is as the water of productive use reuse;
3) acidifying decomplexing: in ultrafiltration and concentration liquid, add sulfuric acid, regulate pH to 1～2, make the heavy metal ion complex compound in the ultrafiltration and concentration liquid carry out decomplexing by acidifying;
4) ultrafiltration is reclaimed: the solution of decomplexing is carried out ultrafiltration get ultrafiltration dialysis liquid, complexing agent is enriched in and turns back in the concentrated solution in the complexing operation next time;
5) reverse osmosis concentration: ultrafiltration dialysis liquid is carried out reverse osmosis concentration separate, get the heavy metal ion reverse osmosis concentrated liquid, make that the concentration of heavy metal ion reaches 2800～3500mg/L in the reverse osmosis concentrated liquid, and turn back in the Electroplating Production operation and recycle, dialyzate is as the water of productive use reuse.
In the complexing step, used water dissolubility high polymer such as sodium polyacrylate are as complexing agent, and the concentration of the heavy metal ion in the electroplating effluent is 60～220mg/L, and the content of electro-coppering, chromium, nickel waste liquid and complexing agent was respectively 1: 25 by mass ratio; 1: 30; 1: 33.In the complexing treating processes, can adopt 1 part of concentration is in 1.7～2.1g/L complexing agent, while stir the NaOH solution that to add 0.1 part of concentration be 1g/L, adjusts pH to 6～7.
In the ultrafiltration enriching step, it is the polyvinylidene fluoride film of molecular weight cut-off 50000 that described ultrafiltration and concentration separates the ultra-filtration membrane of selecting for use, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, entrance pressure 3Bar goes out to press 1Bar.
In the ultrafiltration recycling step, at normal temperatures and pressures, the decomplexing liquid pump is gone into to carry out ultrafiltration in the ultrafiltration equipment.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, and entrance pressure 3Bar goes out to press 1Bar, and adding entry, to make pH be 2～3, at least 1 time feed liquid washed, and discharges the copper in the feed liquid, and ultrafiltrated turns back to complexing operation next time.
In the reverse osmosis concentration step, at normal temperatures and pressures, the copper-containing solution behind the decomplexing pumps into and carries out reverse osmosis concentration in the rolling reverse osmosis equipment, and its processing condition are: pressure 30Bar, the feed liquid cycles of concentration is near 10 times.
Compared with prior art, the invention has the advantages that process stabilizing, water-soluble polymers complexing-ultrafiltration-decomplexing-reverse osmosis integrating process can be realized the recycling of heavy metal such as waste water recycling and copper, chromium, cadmium, nickel and complexing agent simultaneously, solves the copper electroplating wastewater to the harm of environment and the waste of copper resource.Concentration of heavy metal ion such as copper is 60～220mg/L in the electroplating effluent, adopt the present invention after, make concentrated solution obtain to reclaim the concentration of heavy metals such as copper, thereby the present invention has broad application prospects.For example adopt the technology of the present invention, the copper concentration of discharge water is lower than 1mg/L, and part is returned in the production rinse water as plating piece, and redundance reaches the emission standard of country and discharges.And the about 2800～3500mg/L of concentration of recovery cupric ion.
Description of drawings
Fig. 1 is the process flow sheet of the embodiment of the invention.
Embodiment
In Fig. 1, copper electroplating wastewater 1, NaOH and macromolecular complexing agent 2 add complex reactor 3 and carry out complex reaction, and the cupric complex liquid pumps into and carries out ultrafiltration and concentration among the ultrafiltration apparatus UF1, removes the ultrafiltrated and the H of impurity gained such as a large amount of water and small molecules
2SO
4Solution enters decomplexing reactor 4 decomplexings, and water purification through in and operation 5 back recycling.The decomplexing liquid pump is gone into ultrafiltration equipment UF2, and gained decomplexing copper liquid pump water rolling reverse osmosis equipment R0 carries out reverse osmosis concentration, and gained copper concentrated solution returns coating bath 6, and the gained water purification through in and operation 5 back recycling.The regenerated polymer of ultrafiltration apparatus UF2 gained returns complex reactor 3, participates in complex reaction.
1) complexing: getting copper concentration is 60mg/L copper electroplating liquid 1L, and adding concentration is the complexing agent 1L of 1.7g/L and the NaOH solution 0.1L that concentration is 1g/L, and stirring state is adjusted pH to 6～7, churning time 20min down.
2) ultrafiltration: the cupric complex liquid pumped into carries out ultrafiltration and concentration in the ultrafiltration apparatus, remove impurity such as a large amount of water and small molecules, ultrafiltrated 1L go into subsequent processing.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, and entrance pressure 3Bar goes out to press 1Bar, 2 times of cycles of concentration, under the condition of test, copper can reach 98.1% removal in the complexing ultra-filtration process, and copper concentration is lower than 1mg/L in the penetrating fluid.
3) decomplexing: with the 1L liquid of ultrafiltration gained under normal temperature and pressure conditions, with 10% (volume ratio) H
2SO
4, carry out decomplexing; Stirring state is adjusted pH to 1～2, churning time 20min down.
4) ultrafiltration: at normal temperatures and pressures, the decomplexing liquid pump is gone into to carry out ultrafiltration in the ultrafiltration equipment.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, and entrance pressure 3Bar goes out to press 1Bar, and the water that adds pH to 2～3 repeatedly washs feed liquid, discharges the copper in the feed liquid, and ultrafiltrated turns back to complexing operation next time, and the rate of recovery of copper reaches 99%.
5) reverse osmosis concentration: at normal temperatures and pressures, the copper-containing solution behind the decomplexing pumps into and carries out reverse osmosis concentration in the rolling reverse osmosis equipment, and the film of selecting for use is the polyethersulfone reverse osmosis membrane.Its processing condition are: pressure 30Bar, the area of film are 0.24m
2, the feed liquid cycles of concentration is near 10 times, and the copper concentration of returning reaches 3000mg/L, and the concentrated solution that obtains returns in the Electroplating Production operation, permeate discharge or use as the washing water of copper spare.
1) complexing: be that to add concentration among the chromium plating bath 1L of 200mg/L be the complexing agent 1L of 1.8g/L and the NaOH 0.1L that concentration is 1g/L toward chromium ion concentration, stirring state is adjusted pH to 6～7 down, and churning time is 20min.
2) ultrafiltration: will contain the chromium complex liquid and pump into and carry out ultrafiltration and concentration in the ultrafiltration apparatus, and remove impurity such as a large amount of water and small molecules, ultrafiltrated is gone into subsequent processing.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, and entrance pressure 3Bar goes out to press 1Bar, 1.8 times of cycles of concentration, under the condition of test, chromium can reach 98.3% removal in the complexing ultra-filtration process, and chromium concn is lower than 1mg/L in the penetrating fluid.
3) decomplexing: with ultrafiltrated under normal temperature and pressure conditions, with 10% (volume ratio) H
2SO
4, carry out decomplexing; Stirring state is adjusted pH to 1～2, churning time 20min down.
4) ultrafiltration: at normal temperatures and pressures, the decomplexing liquid pump is gone into to carry out ultrafiltration in the ultrafiltration equipment.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, and entrance pressure 3Bar goes out to press 1Bar, and the water that adds pH to 2～3 repeatedly washs feed liquid, discharges the chromium in the feed liquid, and ultrafiltrated turns back to complexing operation next time, and the rate of recovery of chromium reaches 99.1%.
5) reverse osmosis concentration: at normal temperatures and pressures, the chromium solution behind the decomplexing pumps into and carries out reverse osmosis concentration in the rolling reverse osmosis equipment, and the film of selecting for use is the polyethersulfone reverse osmosis membrane.Its processing condition are: pressure 30Bar, the area of film are 0.24m
2, the feed liquid cycles of concentration is near 10 times, and the chromium concn that returns reaches 3000mg/L, and the concentrated solution that obtains returns in the Electroplating Production operation, permeate discharge or use as the washing water of chromium spare.
1) complexing: be to add concentration 1.9g/L complexing agent 1L among the nickel plating solution 1L of 220mg/L and concentration is 1g/L NaOH 0.1L toward nickel concentration, stirring state is adjusted pH to 6～7, churning time 20min down.
2) ultrafiltration: nickeliferous complex liquid pumped into carry out ultrafiltration and concentration in the ultrafiltration apparatus, remove impurity such as a large amount of water and small molecules, ultrafiltrated is gone into subsequent processing.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, and entrance pressure 3Bar goes out to press 1Bar, 2.1 times of cycles of concentration, under the condition of test, nickel can reach 98.3% removal in the complexing ultra-filtration process, and nickel concentration is lower than 1mg/L in the penetrating fluid.
3) decomplexing: with ultrafiltrated under normal temperature and pressure conditions, with 10% volume H
2SO
4, carry out decomplexing; Stirring state is adjusted pH to 1～2, churning time 20min down.
4) ultrafiltration: at normal temperatures and pressures, the decomplexing liquid pump is gone into to carry out ultrafiltration in the ultrafiltration equipment.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000, (as the flat sheet membrane such as UF605-2, UF610 of the U.S.).The ultrafiltration technology condition is: room temperature, and entrance pressure 3Bar goes out to press 1Bar, and the water that adds pH to 2～3 repeatedly washs feed liquid, discharges the nickel in the feed liquid, and ultrafiltrated turns back to complexing operation next time, and the rate of recovery of nickel reaches 99.2%.
5) reverse osmosis concentration: at normal temperatures and pressures, the solution containing nickel behind the decomplexing pumps into and carries out reverse osmosis concentration in the rolling reverse osmosis equipment, and the film of selecting for use is the polyethersulfone reverse osmosis membrane.Its processing condition are: pressure 30Bar, the area of film are 0.24m
2, the feed liquid cycles of concentration is near 10 times, and the nickel concentration that returns reaches 3001mg/L, and the concentrated solution that obtains returns in the Electroplating Production operation, permeate discharge or use as the washing water of nickel spare.
Claims (9)
1. an electroplating effluent that contains heavy metal is handled and the heavy metal recoverying and utilizing method, it is characterized in that the steps include:
1) complexing: in heavy metal ion electroplating effluents such as cupric, chromium, cadmium, nickel, add complexing agent water-soluble macromolecule polymkeric substance, make itself and the effect of water-soluble macromolecule polymkeric substance form the ionic complex waste liquid;
2) ultrafiltration enrichment: the ionic complex waste liquid that will contain heavy metal ion such as copper, chromium, cadmium, nickel separates through ultrafiltration and concentration, makes the enrichment of heavy metal ion complex compound get ultrafiltration and concentration liquid, and dialyzate is as the water of productive use reuse;
3) acidifying decomplexing: in ultrafiltration and concentration liquid, add sulfuric acid, regulate pH to 1～2, make the heavy metal ion complex compound in the ultrafiltration and concentration liquid carry out decomplexing by acidifying;
4) ultrafiltration is reclaimed: the solution of decomplexing is carried out ultrafiltration get ultrafiltration dialysis liquid, complexing agent is enriched in and turns back in the concentrated solution in the complexing operation next time;
5) reverse osmosis concentration: ultrafiltration dialysis liquid is carried out reverse osmosis concentration separate, get the heavy metal ion reverse osmosis concentrated liquid, make that the concentration of heavy metal ion reaches 2800～3500mg/L in the reverse osmosis concentrated liquid, and turn back in the Electroplating Production operation and recycle, dialyzate is as the water of productive use reuse.
2. a kind of electroplating effluent that contains heavy metal as claimed in claim 1 is handled and the heavy metal recoverying and utilizing method, it is characterized in that described water-soluble macromolecule polymkeric substance is a sodium polyacrylate.
3. a kind of electroplating effluent that contains heavy metal as claimed in claim 1 is handled and the heavy metal recoverying and utilizing method, it is characterized in that the content of described electro-coppering, chromium, nickel waste liquid and complexing agent was respectively 1: 25 by mass ratio; 1: 30; 1: 33.
4. a kind of electroplating effluent that contains heavy metal as claimed in claim 1 is handled and the heavy metal recoverying and utilizing method, it is characterized in that in the complexing treating processes, 1 part of concentration is in 1.7～2.1g/L complexing agent, while stirring the NaOH solution that to add 0.1 part of concentration be 1g/L, adjust pH to 6～7.
5. a kind of electroplating effluent that contains heavy metal as claimed in claim 1 is handled and the heavy metal recoverying and utilizing method, it is characterized in that in the ultrafiltration enriching step it is the polyvinylidene fluoride film of molecular weight cut-off 50000 that described ultrafiltration and concentration separates the ultra-filtration membrane of selecting for use.
6. handle and the heavy metal recoverying and utilizing method as claim 1 or 6 described a kind of electroplating effluents that contain heavy metal, it is characterized in that in the ultrafiltration enriching step, the ultrafiltration technology condition is: room temperature, entrance pressure 3Bar goes out to press 1Bar.
7. a kind of electroplating effluent that contains heavy metal as claimed in claim 1 is handled and the heavy metal recoverying and utilizing method, it is characterized in that in the ultrafiltration recycling step ultra-filtration membrane that described ultrafiltration is adopted is the polyvinylidene fluoride film of molecular weight cut-off 50000.
8. handle and the heavy metal recoverying and utilizing method as claim 1 or 8 described a kind of electroplating effluents that contain heavy metal, it is characterized in that in the ultrafiltration recycling step, the ultrafiltration technology condition is: room temperature, entrance pressure 3Bar, go out to press 1Bar, the water at least 1 time that adds pH to 2～3 washs feed liquid, discharges the heavy metal ion in the feed liquid, and ultrafiltrated turns back to complexing operation next time.
9. a kind of electroplating effluent that contains heavy metal as claimed in claim 1 is handled and the heavy metal recoverying and utilizing method, it is characterized in that in the reverse osmosis concentration step, at normal temperatures and pressures, the heavy metal solution that contains behind the decomplexing pumps into and carries out reverse osmosis concentration in the rolling reverse osmosis equipment, its processing condition are: pressure 30Bar, feed liquid cycles of concentration are 10 times.
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