CN101786775A - Method for selective recovery of copper and nickel from electroplating sludge - Google Patents
Method for selective recovery of copper and nickel from electroplating sludge Download PDFInfo
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Abstract
The invention discloses a method for selective recovery of copper and nickel from electroplating sludge. The method comprises the following steps: carrying out acid leaching on the electroplating sludge; filtering leachate, leading filtrate to enter into a copper electrolytic tank from the tank bottom under the action of an infusion pump and flow at high speed in a tank body, and carrying out swirl selective electrodeposition of copper; using solution after the copper electrodeposition for hydrolysis, and further removing chromium; using the solution after the chromium removal for swirl selective electrodeposition of nickel; and returning the solution after the swirl nickel deposition to the leaching process step. The method can simultaneously recover copper, nickel, chromium and other metal resources in the electroplating sludge, thereby turning waste into wealth and realizing the recycling and the reutilization of industrial hazardous waste; and the whole process is completely carried out in a closed-loop circulation system, that is washing solution, filtrate, clear solution and the like during the production process can be completely recycled, thereby avoiding the emission, reducing the environmental pollution and the harm and realizing the unification of environmental benefits, social benefits and economic benefits.
Description
Technical field
The present invention relates to a kind of treatment process of electroplating sludge, specifically a kind of from electroplating sludge efficient selective reclaim the method for copper and mickel.
Background technology
Electroplating sludge is a kind of solid deposits that produces in the electroplating wastewater processing process, its complicated component, and toxicity is very big, is the poisonous industrial solid wastes of environmental administration's stringent regulations.Development along with modern electroplating industry, the quantity discharged of electroplating sludge is increasing, and these electroplating sludges are eliminated the hazardous and noxious substances that wherein contains if do not deal carefully with, not only cause the wasting of resources but also will produce serious destruction, be detrimental to health environment.The treatment process of electroplating sludge mainly concentrates on the harmless treatment aspect at present, comprise stacking, landfill, burn, fill out sea etc., harmful waste security landfill technology wherein is the technology of the widest, the both economical suitable processing electroplating sludge of present domestic and international application, but the security landfill method need take a large amount of land resourcess and also be merely able to disposal of wastes and can not thoroughly root out and the electroplating sludge that detoxifies in contain a large amount of heavy metal ambrose alloy chromium etc., be easy to cause secondary pollution because of dealing with improperly.And contain a large amount of heavy metals such as copper nickel chromium triangle in the electroplating sludge, be a kind of potential renewable resource,, then not only solved problem of environmental pollution if can recycle, and can obtain considerable economic, also can solve the shortage of resources problem to a certain extent.There is complex process in the method that existing electric plating sludge resource is handled, complex operation, and performance difficulty, processing cost height cause very difficult long-time running, do not have practical value.
Summary of the invention
The object of the present invention is to provide a kind of technology simple, easy to operate, implement the method for the valuable metal copper and mickel in the selective recovery electroplating sludge easy, with low cost.
Technical scheme of the present invention is: with directly acidleach after the electroplating sludge pulp, filter the back leach liquor is carried out eddy flow selectivity electro deposited copper, liquid carries out directly carrying out eddy flow selectivity electro deposited nickel behind the dechromisation behind the electro deposited copper, solution behind the eddy flow selectivity electro deposited nickel returns the leaching that the front is used for electroplating sludge, obtain electro deposited copper, electro deposited nickel and fine chrome mine at last, thereby realized the short flow process of heavy metals such as copper in the electroplating sludge, nickel, chromium, high efficiency comprehensive recovery.
The present invention includes following steps:
(1) acidleach: with electroplating sludge less water pulp, slowly add mineral acid then, control pH value of solution value is 0.5～3.5, is under 20～90 ℃ in temperature, leaches 0.5～5h;
(2) eddy flow selectivity electro deposited copper: leach liquor is filtered, filtrate is entered copper electrolysis cells from bottom land under the effect of infusion pump, flow at high speed in cell body is carried out eddy flow selectivity electro deposited copper, its electrodeposition condition is: the electrodeposition temperature is 20～90 ℃, and current density is 50～1000A/m
2, the electrodeposition time is 0.5～5h, circular flow is 5～40m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid hydrolysis dechromisation behind the copper electrodeposition: liquid pH value to 4.0～5.5 behind the adjusting copper electrodeposition, control reaction temperature is 20～90 ℃, hydrolysis dechromisation time 0.5～5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) eddy flow selectivity electro deposited nickel: liquid behind the dechromisation is entered electrolytic nickel cell from bottom land under the effect of infusion pump, flow at high speed in cell body is carried out eddy flow selectivity electro deposited nickel, and its electrodeposition condition is: the electrodeposition temperature is 20～90 ℃, and current density is 50～1000A/m
2, the electrodeposition time is 0.5～5h, electrolyte ph is 1.0～4.5, circular flow 5～40m
3/ KgNi obtains electro deposited nickel from negative electrode.
(6) the molten leaching operation of returning behind the eddy flow nickel electrodeposition.
The mineral acid of described acidleach is hydrochloric acid or sulfuric acid or nitric acid.
It is 1.0～1.5 that described electroplating sludge leaches reaction pH value, and temperature is 20～45 ℃, and the leaching reaction times is 30～60min.
Described eddy flow selectivity electro deposited copper best electrodeposition condition be: temperature is 20～40 ℃, and current density is 300～500A/m
2, the electrodeposition time is 2～3h, circular flow is 20～30m
3/ KgCu.
The top condition of described hydrolysis dechromisation is: the pH value is 4.5～5.1, and temperature is 45～60 ℃, and the reaction times is 50～60min.
The best electrodeposition condition of described eddy flow selectivity electro deposited nickel is: temperature is 55～60 ℃, and current density is 300～500A/m
2, the electrodeposition time is 2～3h, and the pH value is 2.5～3.0, and circular flow is 25～30m
3/ KgNi.
The product electro deposited copper quality of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The product electro deposited nickel chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium can reach 30% in the dechromisation slag, can be used as the raw material of producing chromic salts.
The present invention can reclaim metals resources such as copper in the electroplating sludge, nickel, chromium simultaneously, turns waste into wealth, and has realized the cycling and reutilization of industrial dangerous waste; Its whole technologies are carried out in a closed cycle system fully, and promptly the washing lotion of production process, filtrate, clear liquid etc. all can be recycled, and do not efflux, and have reduced pollution and harm to environment; Realized the unification of environmental benefit, society and economic benefit.
Embodiment
Embodiment 1:
It is green that the outward appearance of the electroplating sludge of choosing is, the mud shape, and water content is 83.4%.Dry its main chemical compositions analysis of back sees the following form:
| Element | ??Ni | ??Cu | ??Cr | ??Fe | ??Ca | ??Mg |
| Content (%) | ??12.74 | ??6.9 | ??14.51 | ??0.23 | ??3.34 | ??1.23 |
May further comprise the steps:
(1) gets dried electroplating sludge 1000g, use the less water pulp, slowly add sulfuric acid then, 20 ℃ of control reaction temperature, pH value of solution value 0.5, extraction time 2.5h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 20 ℃ of control electrodeposition temperature, current density 100A/m
2, electrodeposition time 5h, circular flow 40m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 4.0 hydrolysis dechromisation behind the adjusting copper electrodeposition, 90 ℃ of control reaction temperature, reaction times 0.5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 20 ℃ of control electrodeposition temperature, current density 50A/m
2, electrodeposition time 5h, pH value of solution value 1.0, circular flow 40m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 32.93% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Embodiment 2:
(1) gets the dried electroplating sludge 1000g of embodiment 1, use the less water pulp, slowly add sulfuric acid then, 60 ℃ of control reaction temperature, pH value of solution value 3.0, extraction time 0.5h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 35 ℃ of control electrodeposition temperature, current density 950A/m
2, electrodeposition time 1.5h, circular flow 5m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 5.1 hydrolysis dechromisation behind the adjusting copper electrodeposition, 25 ℃ of control reaction temperature, reaction times 5.0h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 65 ℃ of control electrodeposition temperature, current density 950A/m
2, electrodeposition time 2h, pH value of solution value 4.5,5m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 32.5% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Embodiment 3:
(1) gets dried electroplating sludge 1000g, use the less water pulp, slowly add hydrochloric acid then, 55 ℃ of control reaction temperature, pH value of solution value 0.5, extraction time 3.0h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 90 ℃ of control electrodeposition temperature, current density 700A/m
2, electrodeposition time 3h, circular flow 35m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 4.5 hydrolysis dechromisation behind the adjusting copper electrodeposition, 50 ℃ of control reaction temperature, reaction times 1.5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 90 ℃ of control electrodeposition temperature, current density 500A/m
2, electrodeposition time 2h, pH value of solution value 2.5,15m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 30.5% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Embodiment 4:
(1) gets dried electroplating sludge 1000g, use the less water pulp, slowly add hydrochloric acid then, 75 ℃ of control reaction temperature, pH value of solution value 2.5, extraction time 3.5h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 35 ℃ of control electrodeposition temperature, current density 450A/m
2, electrodeposition time 3h, circular flow 25m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 5.3 hydrolysis dechromisation behind the adjusting copper electrodeposition, 75 ℃ of control reaction temperature, reaction times 0.5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 65 ℃ of control electrodeposition temperature, current density 450A/m
2, electrodeposition time 1.5h, pH value of solution value 2.0, circular flow 40m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 32.65% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Embodiment 5:
(1) gets dried electroplating sludge 1000g, use the less water pulp, slowly add nitric acid then, 70 ℃ of control reaction temperature, pH value of solution value 3.5, extraction time 4.5h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 65 ℃ of control electrodeposition temperature, current density 200A/m
2, electrodeposition time 1.5h, circular flow 35m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 4.8 hydrolysis dechromisation behind the adjusting copper electrodeposition, 60 ℃ of control reaction temperature, reaction times 1.5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 60 ℃ of control electrodeposition temperature, current density 350A/m
2, electrodeposition time 3h, pH value of solution value 1.5, circular flow 10m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 32.2% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Embodiment 6:
(1) gets dried electroplating sludge 1000g, use the less water pulp, slowly add nitric acid then, 30 ℃ of control reaction temperature, pH value of solution value 1.0, extraction time 4.5h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 45 ℃ of control electrodeposition temperature, current density 450A/m
2, electrodeposition time 2h, circular flow 10m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 5.0 hydrolysis dechromisation behind the adjusting copper electrodeposition, 60 ℃ of control reaction temperature, reaction times 3.5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 65 ℃ of control electrodeposition temperature, current density 250A/m
2, electrodeposition time 3h, pH value of solution value 2.0, circular flow 15m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 31.6% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Embodiment 7:
(1) gets dried electroplating sludge 1000g, use the less water pulp, slowly add sulfuric acid then, 60 ℃ of control reaction temperature, pH value of solution value 1.0, extraction time 1.5h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 45 ℃ of control electrodeposition temperature, current density 750A/m
2, electrodeposition time 2h, circular flow 15m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 4.5 hydrolysis dechromisation behind the adjusting copper electrodeposition, 70 ℃ of control reaction temperature, reaction times 2.5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 55 ℃ of control electrodeposition temperature, current density 350A/m
2, electrodeposition time 3.5h, pH value of solution value 3.0, circular flow 30m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 31.5% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Embodiment 8:
(1) gets dried electroplating sludge 1000g, use the less water pulp, slowly add sulfuric acid then, 30 ℃ of control reaction temperature, pH value of solution value 3.0, extraction time 5.0h;
(2) leach liquor is filtered filtrate eddy flow selectivity electro deposited copper, 55 ℃ of control electrodeposition temperature, current density 450A/m
2, electrodeposition time 2h, circular flow 35m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid pH value to 5.5 hydrolysis dechromisation behind the adjusting copper electrodeposition, 60 ℃ of control reaction temperature, reaction times 3.5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) filtrate eddy flow selectivity electro deposited nickel, 65 ℃ of control electrodeposition temperature, current density 650A/m
2, electrodeposition time 3h, pH value of solution value 2.5, circular flow 15m
3/ KgNi obtains electro deposited nickel from negative electrode.
The quality product of eddy flow selectivity electro deposited copper reaches the requirement of Cu-CATH-2 trade mark standard cathode copper among the GB/T467-1997; The chemical ingredients of eddy flow selectivity electro deposited nickel reaches the requirement of Ni9990 trade mark electro deposited nickel among the GB/T6516-1997; The content of chromium is 32.5% in the dechromisation slag, can be used as the raw material of producing chromic salts.
Claims (7)
1. the method for a selective recovery copper and mickel from electroplating sludge is characterized in that: may further comprise the steps:
(1) acidleach: with electroplating sludge less water pulp, slowly add mineral acid then, control pH value of solution value is 0.5～3.5, is under 20～90 ℃ in temperature, leaches 0.5～5h;
(2) eddy flow selectivity electro deposited copper: leach liquor is filtered, filtrate is entered copper electrolysis cells from bottom land under the effect of infusion pump, flow at high speed in cell body is carried out eddy flow selectivity electro deposited copper, its electrodeposition condition is: the electrodeposition temperature is 20～90 ℃, and current density is 50～1000A/m
2, the electrodeposition time is 0.5～5h, circular flow is 5～40m
3/ KgCu obtains electro deposited copper from negative electrode;
(3) liquid hydrolysis dechromisation behind the copper electrodeposition: liquid pH value to 4.0～5.5 behind the adjusting copper electrodeposition, control reaction temperature is 20～90 ℃, hydrolysis dechromisation time 0.5～5h;
(4) filter, the residue washing drying, the merging of washing lotion and filtrate change next procedure over to;
(5) eddy flow selectivity electro deposited nickel: liquid behind the dechromisation is entered electrolytic nickel cell from bottom land under the effect of infusion pump, flow at high speed in cell body is carried out eddy flow selectivity electro deposited nickel, and its electrodeposition condition is: the electrodeposition temperature is 20～90 ℃, and current density is 50～1000A/m
2, the electrodeposition time is 0.5～5h, electrolyte ph is 1.0～4.5, circular flow 5～40m
3/ KgNi obtains electro deposited nickel from negative electrode;
(6) the molten leaching operation of returning behind the eddy flow nickel electrodeposition.
2. according to claim 1 from electroplating sludge the method for selective recovery copper and mickel, it is characterized in that described mineral acid is hydrochloric acid or sulfuric acid or nitric acid.
3. according to claim 1 from electroplating sludge the method for selective recovery copper and mickel, it is characterized in that it is 1.0～1.5 that described electroplating sludge leaches reaction pH value, temperature is 20～45 ℃, the leaching reaction times is 30～60min.
4. according to claim 1 from electroplating sludge efficient selective reclaim the method for copper and mickel, it is 1.0～1.5 that described electroplating sludge leaches reaction pH value, temperature is 20～45 ℃, the leaching reaction times is 30～60min.
5. according to claim 1 from electroplating sludge the method for selective recovery copper and mickel, it is characterized in that, described eddy flow selectivity electro deposited copper the electrodeposition condition be: temperature is 20～40 ℃, and current density is 300～500A/m
2, the electrodeposition time is 2～3h, circular flow is 20～30m
3/ KgCu.
6. according to claim 1 from electroplating sludge the method for selective recovery copper and mickel, it is characterized in that the condition of described hydrolysis dechromisation is: the pH value is 4.5～5.1, temperature is 45～60 ℃, the reaction times is 50～60min.
7. according to claim 1 from electroplating sludge the method for selective recovery copper and mickel, it is characterized in that the electrodeposition condition of described eddy flow selectivity electro deposited nickel is: temperature is 55～60 ℃, current density is 300～500A/m
2, the electrodeposition time is 2～3h, and the pH value is 2.5～3.0, and circular flow is 25～30m
3/ KgNi.
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