CN101787547A - Method for recovering valuable metals from waste printed circuit board - Google Patents
Method for recovering valuable metals from waste printed circuit board Download PDFInfo
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- CN101787547A CN101787547A CN201010107804A CN201010107804A CN101787547A CN 101787547 A CN101787547 A CN 101787547A CN 201010107804 A CN201010107804 A CN 201010107804A CN 201010107804 A CN201010107804 A CN 201010107804A CN 101787547 A CN101787547 A CN 101787547A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a method for recovering valuable metals from a waste printed circuit board. The method comprises the following steps: sorting and crushing the printed circuit board, evenly mixing powder containing multiple metal parts with a fluxing agent, and smelting at low temperature for 1-3.5h; adding hot water into smelting products for leaching; evaporating and concentrating filtrate after filtration, and then returning evaporation mother liquor to the water leaching process step; using solution after leaching for swirl electrodeposition of metal silver, and adding 5-25% of HNO3 into filter residue for leaching; filtering the solution after electrodeposition, and adding 1-5 times of the weight of aqua regia into the filter residue for leaching; using the solution after leaching by the aqua regia for the swirl electrodeposition of gold, adding saturated NH4Cl into the solution after the electrodeposition for reaction, then filtering, using ammonium chloroplatinate for refining the filter residue, obtaining sponge platinum, adding methanoic acid into the solution after precipitation, and carrying out reaction for obtaining crude palladium powder. The method can extract copper, nickel, silver, gold, platinum, palladium and other main products and other by-products, realize the maximization of reutilization of value metal resources in the waste printed circuit board and solve the environmental pollution problem; and the adoption of the swirl electrolysis technology can realize low energy consumption, low reagent consumption, short process flow and simple operation.
Description
Technical field
The present invention relates to a kind of method that from waste printed circuit board, reclaims valuable metal.Specifically from waste printed circuit board, reclaim the method for valuable metal by the eddy flow electrolysis tech.
Background technology
It is reported that the useless electronic product of annual global output is up to 3000～4,000 ten thousand tons, and contain multiple hazardous and noxious substances such as Pb, Sn, Sb, Al, polyvinyl chloride and halogenide fire retardant in the printed circuit board (PCB) (PCB), is a kind of solid refuse of highly dangerous.Precious metals such as gold and silver, palladium, platinum also have been rich in the discarded printed circuit boards simultaneously.It is reported that 1 ton of computer part contains precious metals such as gold, 270kg plastics, 128.7kg copper, 58.8kg lead, 39.6kg tin, 36kg nickel, 19.8kg antimony and platinum, the palladium of 0.9kg.According to statistics, approximately contain 272kg plastics, 130kg copper, 41kg iron, 29kg lead, 20kg tin, 10kg antimony, 9kg silver, 18kg nickel, 0.45kg gold and precious metals such as palladium, platinum in the computer integrated circuit board that 1t arbitrarily collects, metal values such as only wherein contained gold and silver, platinum, palladium are very high.Contain 3.5kg silver, 0.34kg gold, 0.14kg palladium and 130kg copper in every 1t depleted mobile phone.The waste and old printed circuit board resource utilization has caused the close attention of global range at present.CN101270411A discloses a kind of method that reclaims the copper metal from useless circuit card, it will have the copper metal of macromolecule member material to be immersed in the swelling agent from the surface that waste printed circuit board strips down, swelling 1min～4h, controlled temperature is in room temperature to 200 ℃, and the macromolecule member material that copper metal matrix material and its is surperficial separates; Utilize the difference of specific gravity of copper metal and macromolecule member material, macromolecule member material and the classification of copper metal are reclaimed.CN101230421A discloses a kind of method of carrying gold from useless circuit card, adopt secondary pickling that useless circuit card metallic particles is carried out pre-treatment, once leach and adopt 0.25～3mol/L nitric acid, 0.5～10mol/L sulfuric acid, mixed acid solution leaches the base metal based on copper of parcel gold in the useless circuit card, by rare HNO
3Solution is to the secondary stripping of base metal, further create favorable conditions for the follow-up gold of carrying, the small amount of nitrogen oxide compound that produces in the reaction adopts water to absorb, use non-cyanogen complexing agent thiocarbamide selectivity to leach gold and silver subsequently, utilize the gold and silver in the base metal iron replacement leach liquor at last, realize that the resource of gold and silver reclaims.CN1012352719A discloses a kind of recovery technology of useless circuit card, mainly is with plastics and metal separation by fragmentation, abrasive dust, selection by winnowing, screening, electric separation.Above technology only is confined to reclaim a kind of metal or only plastics and metal is separated from useless circuit card, thoroughly do not refine separating metal, the loss rate of metal height, and the sour consumption of consumption alkali is many, easily causes secondary pollution etc.
Summary of the invention
The object of the present invention is to provide a kind of method that from waste printed circuit board, reclaims valuable metal by the eddy flow electrolysis tech.To realize that technology is simple, flow process is short, energy consumption is low, environmental friendliness, can be applicable to industrialization promotion.
Technical scheme of the present invention may further comprise the steps:
(1) the printed circuit board (PCB) sorting is pulverized powder and the NaOH that contains many metal parts: NaNO
3=1: 0～1.0 fusing agent by 1: 0.1～1.0 quality than mixing after, at 350～550 ℃ of following low smelting heat 1～3.5h;
(2) smelted product cooling, levigate back by water: melting solid mass ratio is the hot water of 25～60 ℃ of addings in 1: 1～6: 1, under the stirring of 100～1000r/min, leaches 0.5～3h;
(3) filter: filtrate obtains Na after evaporation concentration
2PbO
3, Na
2SnO
3, Na
2SbO
3, NaAlO
2Mixed crystallization, and return the smeltery of refining lead or tin metallurgy and extract valuable metal; Mother liquid evaporation returns the water logging operation; Filter residue enters subsequent handling;
(4) filter residue adds 0.5～3.5mol/LH
2SO
4Solution and oxygenant leach 2～8h for 20～70 ℃ in temperature, and the solution after leaching is filtered, and filtrate enters electrolyzer from bottom land under the effect of infusion pump, carry out eddy flow selectivity electro deposited copper, and its electrodeposition condition is: electrolytic solution pH is 1.0～5.0; The electrodeposition temperature is 20～60 ℃, and current density is 200～550A/m
2, the electrodeposition time is that 0.5～4h obtains electro deposited copper; Described oxygenant is the agent of 5～15g persulfate oxidation or feeds O with the speed of 5～30g/h
3, or add 5～50mlH
2O
2, filter residue enters subsequent handling;
(5) liquid carries out eddy flow selectivity electrowinning nickel again behind the electrodeposition, and its electrodeposition condition is: the electrodeposition temperature is 20～70 ℃, and current density is 200～450A/m
2, electrolytic solution pH is 1.0～5.0, and the electrodeposition time is to obtain electro deposited nickel behind 0.5～4h, and liquid returns H behind the electrodeposition
2SO
4Leach;
The filter residues in (6) the 4th steps add 5～25%HNO according to liquid-solid ratio 5: 1～1: 1
3Solution, the control extraction temperature is 20～80 ℃; Leaching 0.5～2.5h; Leach back liquid eddy flow electrowinning silver, its electrodeposition condition is: the electrodeposition temperature is 20～60 ℃, and current density is 50～200A/m
2, electrolytic solution pH is 1.0～5, obtains electrodeposition silver behind electrodeposition 0.5～4h;
(7) after liquid filtered behind the electrodeposition, filtrate was returned nitric acid and is leached, and filter residue adds the chloroazotic acid of 1～5 times of quality, leaches 1～2.5h under the agitation condition of 20～70 ℃ of temperature, 100～1000r/min;
(8) chloroazotic acid leaches back liquid eddy flow electrodeposition gold, and its electrodeposition condition is: the electrodeposition temperature is 20～60 ℃, and current density is 50～400A/m
2, electrolytic solution pH is 1.0～5.5, obtains the electrodeposition gold behind electrodeposition 0.5～4h;
(9) add saturated NH behind the electrodeposition behind the electrodeposition gold in the liquid
4Cl reaction 2～8h after-filtration, filter residue is an ammonium chloroplatinate, obtains spongy platinum after refining; Filtrate enters subsequent handling;
(10) in post precipitation liquid in palladium: the ratio of formic acid=0.5～3 adds formic acid, reacts 0.5～2h under 50～90 ℃ of intensively stirred conditions, and pH is controlled at 6.0～9.0, obtains thick palladium powder.
Described eddy flow selects the electrodeposition condition of electrowinning copper to be: the electrodeposition temperature is 40～60 ℃, and current density is 350～500A/m
2, electrolytic solution pH is controlled at 1.0～5.0 in the electrolytic deposition process, and the electrodeposition time is 0.5～3h.
Described eddy flow selects the electrodeposition condition of electrowinning nickel to be: the electrodeposition temperature is 45～70 ℃, and current density is 200～450A/m
2, electrolytic solution pH is controlled at 1.0～4.0 in the electrolytic deposition process, and the electrodeposition time is 1～3h.
The electrodeposition condition of described eddy flow electrowinning silver is: the electrodeposition temperature is 40～80 ℃, and current density is 50～200A/m
2, electrolytic solution pH is controlled at 1.0～5.0 in the electrolytic deposition process, and the electrodeposition time is 0.5～4h.
The present invention is according to component and have the characteristics of form, can extract the byproduct of major products such as copper, nickel, silver, gold, platinum, palladium and leaded, tin, antimony, aluminium respectively; Realize the maximization of valuable metal resource regeneration in the waste printed circuit board, also solved the problem of a large amount of waste printed circuit board environmental pollutions; The purity height of major products such as resulting copper, nickel, silver, gold, platinum, palladium; It is low that the eddy flow electrolysis tech that uses also has energy consumption, reagent consumption less, the production process environmental friendliness, technical process is short, simple operation and other advantages.
Embodiment
Embodiment 1
To contain many metal-powder parts and NaOH: NaNO through the PCB that pulverizes sorting
3=1: 0 fusing agent is put into process furnace by 1: 0.4 quality after than mixing, at 420 ℃ of following low smelting heat 2.5h; In liquid-solid ratio 2: 1 (weight ratio), 25 ℃ of temperature leach 2h under the speed stirring condition with 1000r/min with hot water for smelted product cooling, levigate back; Solution after the leaching filters, and filtrate obtains Na after evaporation concentration
2PbO
3, Na
2SnO
3, Na
2SbO
3, NaAlO
2Mixed crystallization returns corresponding smeltery such as refining lead or tin metallurgy and extracts valuable metal; Mother liquid evaporation returns the water logging operation; With the 500g filter residue 1.5mol/LH
2SO
4Solution adds the agent of 10g persulfate oxidation, be 55 ℃ in temperature, leach 2h, after solution after leaching filtered, filter residue entered subsequent handling, and filtrate is utilized eddy flow electrodeposition selective deposition metallic copper, its electrodeposition condition is: the electrodeposition temperature is 20 ℃, and current density is 350A/m
2, electrolytic solution pH is 1.0, obtains electro deposited copper behind the electrodeposition 1.5h;
Liquid behind the electrodeposition that the step obtains in the utilization, eddy flow is selected electrowinning nickel, and its electrodeposition condition is: the electrodeposition temperature is 20 ℃, and current density is 250A/m
2, electrolytic solution pH is 1.0, obtains electro deposited nickel behind the electrodeposition 1.5h, liquid returns H behind the electrodeposition
2SO
4Leach;
At H
2SO
4In the filter residue after the leaching, by 1: 1 (weight ratio) 25%HNO of liquid-solid ratio
3Solution, the control extraction temperature is 30 ℃, leaches 0.5h; Leach back liquid and utilize eddy flow electrowinning silver, its electrodeposition condition is: the electrodeposition temperature is 20 ℃, and current density is 100A/m
2, electrolytic solution pH is 1.0, obtains electrodeposition silver behind the electrodeposition 0.5h; After liquid filtered behind the electrodeposition, filtrate was returned nitric acid and is leached, and filter residue adds the chloroazotic acid of 1 times of quality, stirred and temperature is controlled under 40 ℃ the condition and leaches 1h in the speed of 400r/min; Leach back liquid and utilize eddy flow electrodeposition gold, its electrodeposition condition is: the electrodeposition temperature is 20 ℃, and current density is 150A/m
2, electrolytic solution pH is 5.5, obtains the electrodeposition gold behind the electrodeposition 0.5h; Add saturated NH in the surplus liquid behind the electrodeposition gold
4Cl reaction 6h after-filtration, filtrate enters subsequent handling, and filter residue is an ammonium chloroplatinate, obtains spongy platinum after refining; In post precipitation liquid in palladium: the ratio of formic acid=0.5 adds formic acid, reacts 2h under 60 ℃ of intensively stirred conditions, and pH is controlled at 6.0, obtains thick palladium powder.The various major product rate of recovery are respectively: Cu 98.6%, Ni 97.5%, Ag 95.3%, Au 99.5%, Pt 98.9%, Pd 93.4%.
Embodiment 2
To contain many metal-powder parts and NaOH: NaNO through the PCB that pulverizes sorting
3=1: 0.4 fusing agent is put into process furnace by 1: 0.1 quality after than mixing, at 350 ℃ of following low smelting heat 1.5h; In liquid-solid ratio 1: 1 (weight ratio), 35 ℃ of temperature leach 0.5h under the speed stirring condition with 100r/min with hot water for smelted product cooling, levigate back; Solution after the leaching filters, and filtrate obtains Na after evaporation concentration
2PbO
3, N
A2SnO
3, Na
2SbO
3, NaAlO
2Mixed crystallization returns corresponding smeltery such as refining lead or tin metallurgy and extracts valuable metal; Mother liquid evaporation returns the water logging operation; With the 500g filter residue 3.5mol/LH
2SO
4Feed O with 20g/h in the solution
3, be 20 ℃ in temperature, leach 8h, after the solution after leaching filtered, filter residue entered subsequent handling, filtrate is utilized eddy flow electrodeposition selective deposition metallic copper, its electrodeposition condition is: the electrodeposition temperature is 60 ℃, current density is 200A/m
2, electrolytic solution pH is 3.0, obtains electro deposited copper behind the electrodeposition 4h;
Liquid behind the electrodeposition that the step obtains in the utilization, eddy flow is selected electrowinning nickel, and its electrodeposition condition is: the electrodeposition temperature is 40 ℃, and current density is 200A/m
2, electrolytic solution pH is 5.0, obtains electro deposited nickel behind the electrodeposition 0.5h, liquid returns H behind the electrodeposition
2SO
4Leach;
At H
2SO
4In the filter residue after the leaching, by 5: 1 (weight ratio) 5%HNO of liquid-solid ratio
3Solution, the control extraction temperature is 30 ℃, leaches 2.5h; Leach back liquid and utilize eddy flow electrowinning silver, its electrodeposition condition is: the electrodeposition temperature is 60 ℃, and current density is 50A/m
2, electrolytic solution pH is 5.0, obtains electrodeposition silver behind the electrodeposition 4h; After liquid filtered behind the electrodeposition, filtrate was returned nitric acid and is leached, and filter residue adds the chloroazotic acid of 5 times of quality, stirred and temperature is controlled under 35 ℃ the condition and leaches 2.5h in the speed of 1000r/min; Leach back liquid and utilize eddy flow electrodeposition gold, its electrodeposition condition is: the electrodeposition temperature is 60 ℃, and current density is 50A/m
2, electrolytic solution pH is 2.5, obtains the electrodeposition gold behind the electrodeposition 1.5h; Add saturated NH in the surplus liquid behind the electrodeposition gold
4Cl reaction 2h after-filtration, filtrate enters subsequent handling, and filter residue is an ammonium chloroplatinate, obtains spongy platinum after refining; In post precipitation liquid in palladium: the ratio of formic acid=1 adds formic acid, reacts 1h under 50 ℃ of intensively stirred conditions, and pH is controlled at 7.0, obtains thick palladium powder.The various major product rate of recovery are respectively: Cu 98.6%, Ni 97.5%, Ag 95.3%, Au 99.5%, Pt 98.9%, Pd 93.4%.
Embodiment 3
To contain many metal-powder parts and NaOH: NaNO through the PCB that pulverizes sorting
3=1: 1.0 fusing agent is put into process furnace by 1: 0.8 quality after than mixing, at 550 ℃ of following low smelting heat 1h; In liquid-solid ratio 4: 1 (weight ratio), 45 ℃ of temperature leach 3h under the speed stirring condition with 400r/min with hot water for smelted product cooling, levigate back; Solution after the leaching filters, and filtrate obtains Na after evaporation concentration
2PbO
3, Na
2SnO
3, Na
2SbO
3, NaAlO
2Mixed crystallization returns corresponding smeltery such as refining lead or tin metallurgy and extracts valuable metal; Mother liquid evaporation returns the water logging operation; With the 500g filter residue 0.5mol/LH
2SO
4Add 40mlH in the solution
2O
2, be 35 ℃ in temperature, leach 4h, after the solution after leaching filtered, filter residue entered subsequent handling, filtrate is utilized eddy flow electrodeposition selective deposition metallic copper, its electrodeposition condition is: the electrodeposition temperature is 40 ℃, current density is 450A/m
2, electrolytic solution pH is 5.0, obtains electro deposited copper behind the electrodeposition 0.5h;
Liquid behind the electrodeposition that the step obtains in the utilization, eddy flow is selected electrowinning nickel, and its electrodeposition condition is: the electrodeposition temperature is 55 ℃, and current density is 350A/m
2, electrolytic solution pH is 2.0, obtains electro deposited nickel behind the electrodeposition 4h, liquid returns H behind the electrodeposition
2SO
4Leach;
At H
2SO
4In the filter residue after the leaching, by 4: 1 (weight ratio) 10%HNO of liquid-solid ratio
3Solution, the control extraction temperature is 50 ℃, leaches 2h; Leach back liquid and utilize eddy flow electrowinning silver, its electrodeposition condition is: the electrodeposition temperature is 30 ℃, and current density is 150A/m
2, electrolytic solution pH is 2.0, obtains electrodeposition silver behind the electrodeposition 1h; After liquid filtered behind the electrodeposition, filtrate was returned nitric acid and is leached, and filter residue adds the chloroazotic acid of 2 times of quality, stirred and temperature is controlled under 20 ℃ the condition and leaches 1.5h in the speed of 100r/min; Leach back liquid and utilize eddy flow electrodeposition gold, its electrodeposition condition is: the electrodeposition temperature is 30 ℃, and current density is 300A/m
2, electrolytic solution pH is 1.0, obtains the electrodeposition gold behind the electrodeposition 3h; Add saturated NH in the surplus liquid behind the electrodeposition gold
4Cl reaction 5h after-filtration, filtrate enters subsequent handling, and filter residue is an ammonium chloroplatinate, obtains spongy platinum after refining; In post precipitation liquid in palladium: the ratio of formic acid=2 adds formic acid, reacts 0.5h under 80 ℃ of intensively stirred conditions, and pH is controlled at 8.0, obtains thick palladium powder.The various major product rate of recovery are respectively: Cu 98.6%, Ni 97.5%, Ag 95.3%, Au 99.5%, Pt 98.9%, Pd 93.4%.
Embodiment 4
To contain many metal-powder parts and NaOH: NaNO through the PCB that pulverizes sorting
3=1: 0.5 fusing agent is put into process furnace by 1: 0.1 quality after than mixing, at 500 ℃ of following low smelting heat 3.5h; In liquid-solid ratio 6: 1 (weight ratio), 60 ℃ of temperature leach 3h under the speed stirring condition with 800r/min with hot water for smelted product cooling, levigate back; Solution after the leaching filters, and filtrate obtains Na after evaporation concentration
2PbO
3, Na
2SnO
3, Na
2SbO
3, NaAlO
2Mixed crystallization returns corresponding smeltery such as refining lead or tin metallurgy and extracts valuable metal; Mother liquid evaporation returns the water logging operation; With the 500g filter residue 2.5mol/LH
2SO
4Add the agent of 5g persulfate oxidation in the solution, be 70 ℃, leach 6h in temperature, after solution after leaching filtered, filter residue entered subsequent handling, and filtrate is utilized eddy flow electrodeposition selective deposition metallic copper, its electrodeposition condition is: the electrodeposition temperature is 50 ℃, and current density is 550A/m
2, electrolytic solution pH is 2.0, obtains electro deposited copper behind the electrodeposition 2.5h;
Liquid behind the electrodeposition that the step obtains in the utilization, eddy flow is selected electrowinning nickel, and its electrodeposition condition is: the electrodeposition temperature is 70 ℃, and current density is 450A/m
2, electrolytic solution pH is 3.0, obtains electro deposited nickel behind the electrodeposition 3h, liquid returns H behind the electrodeposition
2SO
4Leach;
At H
2SO
4In the filter residue after the leaching, by 3: 1 (weight ratio) 15%HNO of liquid-solid ratio
3Solution, the control extraction temperature is 70 ℃, leaches 1h; Leach back liquid and utilize eddy flow electrowinning silver, its electrodeposition condition is: the electrodeposition temperature is 50 ℃, and current density is 200A/m
2, electrolytic solution pH is 4.0, obtains electrodeposition silver behind the electrodeposition 3h; After liquid filtered behind the electrodeposition, filtrate was returned nitric acid and is leached, and filter residue adds the chloroazotic acid of 4 times of quality, stirred and temperature is controlled under 30 ℃ the condition and leaches 2h in the speed of 800r/min; Leach back liquid and utilize eddy flow electrodeposition gold, its electrodeposition condition is: the electrodeposition temperature is 50 ℃, and current density is 400A/m
2, electrolytic solution pH is 4.5, obtains the electrodeposition gold behind the electrodeposition 4h; Add saturated NH in the surplus liquid behind the electrodeposition gold
4Cl reaction 8h after-filtration, filtrate enters subsequent handling, and filter residue is an ammonium chloroplatinate, obtains spongy platinum after refining; In post precipitation liquid in palladium: the ratio of formic acid=3 adds formic acid, reacts 1.5h under 90 ℃ of intensively stirred conditions, and pH is controlled at 9.0, obtains thick palladium powder.The various major product rate of recovery are respectively: Cu 98.6%, Ni 97.5%, Ag 95.3%, Au 99.5%, Pt 98.9%, Pd 93.4%.
Claims (5)
1. a method that reclaims valuable metal from waste printed circuit board is characterized in that, may further comprise the steps:
(1) the printed circuit board (PCB) sorting is pulverized powder and the NaOH that contains many metal parts: NaNO
3=1: 0～1.0 fusing agent by 1: 0.1～1.0 quality than mixing after, at 350～550 ℃ of following low smelting heat 1～3.5h;
(2) smelted product cooling, levigate back by water: melting solid mass ratio is the hot water of 25～60 ℃ of addings in 1: 1～6: 1, under the stirring of 100～1000r/min, leaches 0.5～3h;
(3) filter, filtrate obtains Na after evaporation concentration
2PbO
3, Na
2SnO
3, Na
2SbO
3, NaAlO
2Mixed crystallization, and return the smeltery of refining lead or tin metallurgy and extract valuable metal; Mother liquid evaporation returns the water logging operation; Filter residue enters subsequent handling;
(4) eddy flow selectivity electro deposited copper: filter residue adds 0.5～3.5mol/LH
2SO
4Solution and oxygenant leach 2～8h for 20～70 ℃ in temperature, and the solution after leaching is filtered, and filtrate enters electrolyzer from bottom land under the effect of infusion pump, carry out eddy flow selectivity electro deposited copper, and its electrodeposition condition is: electrolytic solution pH is 1.0～5.0; The electrodeposition temperature is 20～60 ℃, and current density is 200～550A/m
2, the electrodeposition time is that 0.5～4h obtains electro deposited copper; Filter residue enters subsequent handling;
(5) liquid carries out eddy flow selectivity electrowinning nickel again behind the electrodeposition, and its electrodeposition condition is: the electrodeposition temperature is 20～70 ℃, and current density is 200～450A/m
2, electrolytic solution pH is 1.0～5.0, and the electrodeposition time is to obtain electro deposited nickel behind 0.5～4h, and liquid returns H behind the electrodeposition
2SO
4Leach;
(6) filter residue adds 5～25%HNO according to liquid-solid ratio 5: 1～1: 1
3Solution, the control extraction temperature is 20～80 ℃; Leaching 0.5～2.5h; Leach back liquid eddy flow electrowinning silver, its electrodeposition condition is: the electrodeposition temperature is 20～60 ℃, and current density is 50～200A/m
2, electrolytic solution pH is 1.0～5, obtains electrodeposition silver behind electrodeposition 0.5～4h;
(7) after liquid filtered behind the electrodeposition, filtrate was returned nitric acid and is leached, and filter residue adds the chloroazotic acid of 1～5 times of quality, leaches 1～2.5h under the agitation condition of 20～70 ℃ of temperature, 100～1000r/min;
(8) chloroazotic acid leaches back liquid eddy flow electrodeposition gold, and its electrodeposition condition is: the electrodeposition temperature is 20～60 ℃, and current density is 50～400A/m
2, electrolytic solution pH is 1.0～5.5, obtains the electrodeposition gold behind electrodeposition 0.5～4h;
(9) add saturated NH behind the electrodeposition behind the electrodeposition gold in the liquid
4Cl reaction 2～8h after-filtration, filter residue is an ammonium chloroplatinate, obtains spongy platinum after refining; Filtrate enters subsequent handling;
(10) in post precipitation liquid in palladium: the ratio of formic acid=0.5～3 adds formic acid, reacts 0.5～2h under 50～90 ℃ of intensively stirred conditions, and pH is controlled at 6.0～9.0, obtains thick palladium powder.
2. a kind of method that reclaims valuable metal from waste printed circuit board according to claim 1 is characterized in that, adds 0.5～3.5mol/LH at filter residue described in the 4th step
2SO
4Oxygenant in solution and the oxygenant is 5～15g persulphate or feeds O with the speed of 5～30g/h
3, or add 5～50mlH
2O
2
3. a kind of method that reclaims valuable metal from waste printed circuit board according to claim 1 is characterized in that described eddy flow selects the electrodeposition condition of electrowinning copper to be: the electrodeposition temperature is 40～60 ℃, and current density is 350～500A/m
2, electrolytic solution pH is controlled at 1.0～5.0 in the electrolytic deposition process, and the electrodeposition time is 0.5～3h.
4. a kind of method that reclaims valuable metal from waste printed circuit board according to claim 1 is characterized in that described eddy flow selects the electrodeposition condition of electrowinning nickel to be: the electrodeposition temperature is 45～70 ℃, and current density is 200～450A/m
2, electrolytic solution pH is controlled at 1.0～4.0 in the electrolytic deposition process, and the electrodeposition time is 1～3h.
5. a kind of method that from waste printed circuit board, reclaims valuable metal according to claim 1, it is characterized in that the electrodeposition condition of described eddy flow electrowinning silver is: the electrodeposition temperature is 40～80 ℃, current density is 50～200A/m
2, electrolytic solution pH is controlled at 1.0～5.0 in the electrolytic deposition process, and the electrodeposition time is 0.5～4h.
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|---|---|---|---|
| CN2010101078043A CN101787547B (en) | 2010-02-09 | 2010-02-09 | Method for recovering valuable metals from waste printed circuit board |
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Cited By (31)
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Effective date of registration: 20210813 Address after: Shaoshan high tech Industrial Development Zone, Xiangtan City, Hunan Province (at the junction of Hongqi Road and Lianhua Road) Patentee after: HUNAN JIANGYE ELECTRICAL AND MECHANICAL TECHNOLOGY Co.,Ltd. Address before: 410083 Hunan province Changsha Lushan Road No. 154 Patentee before: CENTRAL SOUTH University |