CN1670258A - Method for producing copper powder by electrodeposition - Google Patents
Method for producing copper powder by electrodeposition Download PDFInfo
- Publication number
- CN1670258A CN1670258A CN 200510007317 CN200510007317A CN1670258A CN 1670258 A CN1670258 A CN 1670258A CN 200510007317 CN200510007317 CN 200510007317 CN 200510007317 A CN200510007317 A CN 200510007317A CN 1670258 A CN1670258 A CN 1670258A
- Authority
- CN
- China
- Prior art keywords
- copper
- electrodeposition
- copper powder
- producing
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000010949 copper Substances 0.000 claims abstract description 32
- 229910052802 copper Inorganic materials 0.000 claims abstract description 32
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 15
- 229910000882 Ca alloy Inorganic materials 0.000 claims abstract description 8
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 40
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 14
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 10
- 238000005868 electrolysis reaction Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 229910001369 Brass Inorganic materials 0.000 claims description 4
- 239000010951 brass Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- PYRZPBDTPRQYKG-UHFFFAOYSA-N cyclopentene-1-carboxylic acid Chemical compound OC(=O)C1=CCCC1 PYRZPBDTPRQYKG-UHFFFAOYSA-N 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 239000001117 sulphuric acid Substances 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001124569 Lycaenidae Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000014987 copper Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Landscapes
- Electrolytic Production Of Metals (AREA)
Abstract
The invention provides a method for producing copper powder by electrodeposition which comprises using spongy copper or waste copper as raw material, preparing electrolytic solution with the copper ion concentration 7-15g/l and sulphuric acid concentration 120-150 g/l, at the temperature of 50-60 deg. C, controlling current density to 1600-2200 A/M2, using Pb-Sn-Ca alloy board as anode, using luminous electrolytic copper board as cathode for copper powder electrodeposition production.
Description
Technical field
A kind of method of producing copper powder by electrodeposition relates to a kind of production method of metal-powder, particularly adopts the method for electrodeposition, produces the method for copper powder.
Background technology
Copper powder is widely used in powder metallurgy, electrical carbon product and industries such as chemical industry catalyst, coating.The method of producing copper powder mainly contains electrolytic process, atomization, atomized copper powder oxidation reduction process etc., and all these production methods, all depending on high purity coppers such as electrolytic copper or fine copper is raw material, makes production cost high, the economic value added of product is lower.
Summary of the invention
Purpose of the present invention is exactly in order to overcome the deficiency that above-mentioned prior art exists, a kind of method that can effectively reduce production costs, improve the producing copper powder by electrodeposition of added value of product to be provided.
Method of the present invention is achieved through the following technical solutions.
A kind of method of producing copper powder by electrodeposition is characterized in that preparation process is is raw material with copper sponge or useless composition brass, with copper with sulfuric acid dissolution after, through P
204It is that 3-4, concentration are the copper-bath of 60~80g/l that pH is prepared in the extraction of extraction back, the process dilution is also added sulfuric acid, preparing copper ion concentration is that 7~15g/l, sulfuric acid concentration are the electrolytic solution of 120~150g/l, and under 50 ℃~60 ℃ temperature, control current density is 1600~2200A/m
2, adopting the Pb-Sn-Ca alloy sheets is that anode, bright electrolysis copper coin are negative electrode, carries out producing copper powder by electrodeposition.
A kind of method of producing copper powder by electrodeposition, it is characterized in that in the process of producing copper powder by electrodeposition, electrodeposition begins per hour to add the copper sulfate rich solution that copper ion concentration is 60~80g/l by 2%~3% of global cycle liquor capacity, per hour by 0.5%~1% of global cycle liquor capacity, from Lower tank, take out stripped solution, keep adding in the whole process copper-bath rich solution and take out the stripped solution equilibrium.
A kind of method of producing copper powder by electrodeposition is characterized in that in the process of producing copper powder by electrodeposition, at 10~60min regular brush dust in the time.
A kind of method of producing copper powder by electrodeposition, the processing that it is characterized in that the electrodeposition stripped solution are directly to turn back to leach liquor or the strip liquor use of the extracting system of copper sulfate as the copper material.
Method of the present invention uses the useless assorted of copper sponge and copper to expect, has enlarged the raw material sources of copper powder, has fundamentally reduced the copper powder production cost, has promoted copper powder production.Because it is raw material that this technology adopts the not high copper scrap of price, than the method for using electrolytic copper or fine copper as raw material, its production cost reduces greatly and reduces, and improves the economic benefit of copper powder greatly.
Adopt method of the present invention, reduced copper anode preparation in the electrolytic process production process, hung, the replacing of copper anode scrap, the operations such as second casting of anode scrap have reduced labour intensity to a great extent.
The electrodeposition stripped solution that method of the present invention is taken out from the electric effusion recycle system, owing to contain the cupric ion of low concentration, more highly acid concentration, can directly turn back to of leach liquor or the strip liquor use of the extracting system of copper sulfate as the copper material, therefore greatly improve the rate of recovery of metal, reduced contaminated wastewater.
Adopt method of the present invention, the electrodeposition method copper powder is washed the extraction part that cupric in the powder process, acidiferous waste liquid can turn back to copper solutions, uses as the leach liquor or the strip liquor of copper material, has therefore greatly improved the rate of recovery of metal, has reduced contaminated wastewater.
Embodiment
A kind of method of producing copper powder by electrodeposition, with the copper sponge that produces in nickel anode electrolysis and the copper anode electrolysis production process or useless composition brass with sulfuric acid dissolution after, preparing pH through extraction is that 3-4, concentration are the copper-bath of 60~80g/l, the process dilution is also added sulfuric acid, preparing copper ion concentration is that 7~15g/l, sulfuric acid concentration are the electrolytic solution of 120~150g/l, under 50 ℃~60 ℃ temperature, control current density is 1600~2200A/m
2, adopting the Pb-Sn-Ca alloy sheets is that anode, bright electrolysis copper coin are negative electrode, carries out producing copper powder by electrodeposition.In the process of producing copper powder by electrodeposition, electrodeposition begins per hour to add the copper sulfate rich solution that copper ion concentration is 60~80g/l by 2%~3% of global cycle liquor capacity, per hour by 0.5%~1% of global cycle liquor capacity, from Lower tank, take out stripped solution, keep adding in the whole process copper-bath rich solution and take out the stripped solution equilibrium at 10~60min regular brush dust in the time.The processing of electrodeposition stripped solution is directly to turn back to leach liquor or the strip liquor use of the extracting system of copper sulfate as the copper material.
Below in conjunction with example method of the present invention is further described.
Operation steps
1, the preparation of electrolyzer
Anode adopts the Pb-Sn-Ca alloy sheets, and negative electrode adopts bright electrolysis copper coin, according to the size of electrolyzer, makes the useful area size the same substantially, and installs ready.
2, the preparation of electrolytic solution
Through the copper-bath after the extraction, concentration through diluting and adding sulfuric acid, makes copper ion concentration be controlled at 2~15g/l greatly about 60~80g/l, sulfuric acid concentration is controlled at 120~150g/l, and be heated to 50~60 ℃, get in the electrolyzer with pump, and be full of whole electrolyzer, and header tank filled, start silicon rectifier, the useful area calculating electric current according to all negative plates makes cathode current density be controlled at 1600~2200A/m
2, carry out the production of electrodeposition copper powder;
3, solution equilibria
Electrodeposition begins, per hour add the rich solution of copper ion concentration at 60~80g/l by 2%~3% of global cycle liquor capacity, per hour by 0.5%~1% of global cycle liquor capacity, from Lower tank, take out stripped solution, to keep adding rich solution in the whole process and take out stripped solution even, can not neglect fast neglecting slowly, generally use magnetic flow meter control.
4, brush dust
The globule size of copper powder as required, regular brush dust in 10~60min scope, the time is short more, and copper powder is thin more.
5, the processing of electrodeposition stripped solution
The electrodeposition stripped solution that from the electric effusion recycle system, takes out, owing to contain the cupric ion of low concentration, more highly acid concentration can directly turn back to leach liquor or the strip liquor use of the extracting system of copper sulfate as the copper material, therefore greatly improve the rate of recovery of metal, reduced contaminated wastewater.
Embodiment 1
With copper sponge with sulfuric acid dissolution after, prepare through extraction that pH is 3, concentration is the copper-bath of 60g/l, also add sulfuric acid through dilution, preparing copper ion concentration is that 12g/l, sulfuric acid concentration are the electrolytic solution of 120g/l, under 50 ℃ of temperature, control current density is 2000A/m
2, adopting the Pb-Sn-Ca alloy sheets is that anode, bright electrolysis copper coin are negative electrode, carries out producing copper powder by electrodeposition.In the process of producing copper powder by electrodeposition, electrodeposition begins per hour to add the copper sulfate rich solution that copper ion concentration is 60g/l by 2% of global cycle liquor capacity, per hour by 0.5% of global cycle liquor capacity, from Lower tank, take out stripped solution, keep adding in the whole process copper-bath rich solution and take out the stripped solution equilibrium at 10min regular brush dust in the time.The processing of electrodeposition stripped solution is directly to turn back to leach liquor or the strip liquor use of the extracting system of copper sulfate as the copper material, and the Chemical Composition of the copper powder of production is as follows:
????Cu+Ag ????/% | ????Fe/% | ????Pb/% | ????As/% | ????Sb/% | ??O/% | ??Bi/% | ??Ni/% | ??Sn/% | ??Zn/% | ??Cr/% | Nitric acid is insoluble/% | ??S/% |
????99.80 | ????0.0024 | ????0.012 | ????0.001 | ????0.0024 | ??0.11 | ??0.0008 | ??0.0024 | ??0.001 | ??0.002 | ??0.0064 | ????0.01 | ??0.0021 |
All less than-200 orders.Loose specific weight: 1.02g/cm
3
Embodiment 2
To give up composition brass with sulfuric acid dissolution after, prepare through extraction that pH is 4, concentration is the copper-bath of 80g/l, also add sulfuric acid through dilution, preparing copper ion concentration is that 15g/l, sulfuric acid concentration are the electrolytic solution of 150g/l, under 60 ℃ of temperature, control current density is 1600A/m
2, adopting the Pb-Sn-Ca alloy sheets is that anode, bright electrolysis copper coin are negative electrode, carries out producing copper powder by electrodeposition.In the process of producing copper powder by electrodeposition, electrodeposition begins per hour to add the copper sulfate rich solution that copper ion concentration is 60~80g/l by 3% of global cycle liquor capacity, per hour by 1% of global cycle liquor capacity, from Lower tank, take out stripped solution, keep adding in the whole process copper-bath rich solution and take out the stripped solution equilibrium, at 60min regular brush dust in the time.The processing of electrodeposition stripped solution is directly to turn back to leach liquor or the strip liquor use of the extracting system of copper sulfate as the copper material, and the copper powder Chemical Composition of production is as follows:
??Cu+Ag ??/% | ??Fe/% | ??Pb/% | ??As/% | ??Sb/% | ????O/% | ??Bi/% | ??Ni/% | ??Sn/% | ??Zn/% | ??Cr/% | Nitric acid is insoluble/% | ??S/% |
??99.81 | ??0.0024 | ??0.012 | ??0.001 | ??0.0024 | ????0.12 | ??0.0008 | ??0.0024 | ??0.001 | ??0.002 | ??0.0064 | ????0.01 | ??0.0021 |
All less than-200 orders.Loose specific weight: 1.17g/cm
3
Embodiment 3
With copper with sulfuric acid dissolution after, prepare through extraction that pH is 3.5, concentration is the copper-bath of 70g/l, also add sulfuric acid through dilution, preparing copper ion concentration is that 7g/l, sulfuric acid concentration are the electrolytic solution of 135g/l, under 55 ℃ of temperature, control current density is 2200A/m
2, adopting the Pb-Sn-Ca alloy sheets is that anode, bright electrolysis copper coin are negative electrode, carries out producing copper powder by electrodeposition.In the process of producing copper powder by electrodeposition, electrodeposition begins per hour to add the copper sulfate rich solution that copper ion concentration is 70g/l by 2.5% of global cycle liquor capacity, per hour by 0.75% of global cycle liquor capacity, from Lower tank, take out stripped solution, keep adding in the whole process copper-bath rich solution and take out the stripped solution equilibrium, at 30min regular brush dust in the time.The processing of electrodeposition stripped solution is directly to turn back to leach liquor or the strip liquor use of the extracting system of copper sulfate as the copper material, and the Chemical Composition of the copper powder of production is as follows:
??Cu+Ag/ ??% | ??Fe/% | ??Pb/% | ??As/% | ??Sb/% | ????O/% | ??Bi/% | ??Ni/% | ??Sn/% | ??Zn/% | ??Cr/% | Nitric acid is insoluble/% | ??S/% |
??99.80 | ??0.0021 | ??0.010 | ??0.001 | ??0.0018 | ????0.13 | ??0.0006 | ??0.0015 | ??0.001 | ??0.0013 | ??0.0049 | ??0.01 | ??0.0018 |
All less than-200 orders.Loose specific weight: 0.95g/cm
3
Claims (4)
1. the method for a producing copper powder by electrodeposition is characterized in that preparation process is is raw material with copper sponge or useless composition brass, with copper with sulfuric acid dissolution after, through P
204It is that 3-4, concentration are the copper-bath of 60~80g/l that pH is prepared in the extraction of extraction back, the process dilution is also added sulfuric acid, preparing copper ion concentration is that 7~15g/l, sulfuric acid concentration are the electrolytic solution of 120~150g/l, and under ℃ temperature of 50C~60, control current density is 1600~2200A/m
2, to adopt the Pb-Sn-Ca alloy sheets be that anode, bright electrolysis copper coin are negative electrode, carries out producing copper powder by electrodeposition.
2. the method for a kind of producing copper powder by electrodeposition according to claim 1, it is characterized in that in the process of producing copper powder by electrodeposition, electrodeposition begins per hour to add the copper sulfate rich solution that copper ion concentration is 60~80g/l by 2%~3% of global cycle liquor capacity, per hour by 0.5%~1% of global cycle liquor capacity, from Lower tank, take out stripped solution, keep adding in the whole process copper-bath rich solution and take out the stripped solution equilibrium.
3. the method for a kind of producing copper powder by electrodeposition according to claim 1 is characterized in that in the process of producing copper powder by electrodeposition, at 10~60min regular brush dust in the time.
4. the method for a kind of producing copper powder by electrodeposition according to claim 1, the processing that it is characterized in that the electrodeposition stripped solution are directly to turn back to the extracting system of copper sulfate to use as the leach liquor or the strip liquor of copper material.
Priority Applications (1)
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CNB2005100073179A CN100344795C (en) | 2005-02-06 | 2005-02-06 | Method for producing copper powder by electrodeposition |
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CNB2005100073179A CN100344795C (en) | 2005-02-06 | 2005-02-06 | Method for producing copper powder by electrodeposition |
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CN100344795C CN100344795C (en) | 2007-10-24 |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101942565A (en) * | 2010-09-03 | 2011-01-12 | 罗光臣 | Regeneration and recovery method for waste red copper |
CN102828205A (en) * | 2011-08-26 | 2012-12-19 | 兰州交通大学 | Novel metal electro-deposition refining technology |
CN103866352A (en) * | 2012-12-17 | 2014-06-18 | 重庆华浩冶炼有限公司 | Producing method of electrolytic copper powder |
CN102560534B (en) * | 2006-03-01 | 2014-12-31 | Jx日矿日石金属株式会社 | Process for electrolytic refining of copper |
CN110144604A (en) * | 2019-06-17 | 2019-08-20 | 阳谷祥光铜业有限公司 | A kind of preparation process of electrodeposition copper powder |
CN111593373A (en) * | 2020-07-13 | 2020-08-28 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
CN112499598A (en) * | 2020-11-12 | 2021-03-16 | 阳谷祥光铜业有限公司 | Method for extracting tellurium from copper anode slime press leaching solution |
Families Citing this family (1)
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CN106854768B (en) * | 2016-11-21 | 2019-03-26 | 西北矿冶研究院 | electrodeposition preparation method of superfine copper powder |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0353092A (en) * | 1989-07-19 | 1991-03-07 | Nippon Mining Co Ltd | Production of copper fine powder |
US5820653A (en) * | 1993-04-19 | 1998-10-13 | Electrocopper Products Limited | Process for making shaped copper articles |
JP3696525B2 (en) * | 2001-05-02 | 2005-09-21 | 福田金属箔粉工業株式会社 | Copper fine powder manufacturing method |
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2005
- 2005-02-06 CN CNB2005100073179A patent/CN100344795C/en not_active Expired - Fee Related
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102560534B (en) * | 2006-03-01 | 2014-12-31 | Jx日矿日石金属株式会社 | Process for electrolytic refining of copper |
CN101942565A (en) * | 2010-09-03 | 2011-01-12 | 罗光臣 | Regeneration and recovery method for waste red copper |
CN101942565B (en) * | 2010-09-03 | 2012-09-05 | 罗光臣 | Regeneration and recovery method for waste red copper |
CN102828205A (en) * | 2011-08-26 | 2012-12-19 | 兰州交通大学 | Novel metal electro-deposition refining technology |
CN103866352A (en) * | 2012-12-17 | 2014-06-18 | 重庆华浩冶炼有限公司 | Producing method of electrolytic copper powder |
CN110144604A (en) * | 2019-06-17 | 2019-08-20 | 阳谷祥光铜业有限公司 | A kind of preparation process of electrodeposition copper powder |
CN111593373A (en) * | 2020-07-13 | 2020-08-28 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
CN111593373B (en) * | 2020-07-13 | 2022-06-17 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
CN112499598A (en) * | 2020-11-12 | 2021-03-16 | 阳谷祥光铜业有限公司 | Method for extracting tellurium from copper anode slime press leaching solution |
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