CN101343750B - Application of sulphuric acid hydrogen imidazole ion liquid in electrolytical refined copper - Google Patents
Application of sulphuric acid hydrogen imidazole ion liquid in electrolytical refined copper Download PDFInfo
- Publication number
- CN101343750B CN101343750B CN2008100588696A CN200810058869A CN101343750B CN 101343750 B CN101343750 B CN 101343750B CN 2008100588696 A CN2008100588696 A CN 2008100588696A CN 200810058869 A CN200810058869 A CN 200810058869A CN 101343750 B CN101343750 B CN 101343750B
- Authority
- CN
- China
- Prior art keywords
- copper
- imidazole ion
- hydrogen sulfate
- ion liquid
- application
- 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.)
- Expired - Fee Related
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000010949 copper Substances 0.000 title claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 title claims description 16
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 title description 6
- 239000001257 hydrogen Substances 0.000 title description 2
- 229910052739 hydrogen Inorganic materials 0.000 title description 2
- 235000011149 sulphuric acid Nutrition 0.000 title 1
- 239000001117 sulphuric acid Substances 0.000 title 1
- -1 hydrogen sulfate imidazole ion Chemical class 0.000 claims abstract description 16
- 238000007670 refining Methods 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims description 20
- 230000000996 additive effect Effects 0.000 claims description 18
- 241000370738 Chlorion Species 0.000 claims description 5
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims description 4
- 239000001828 Gelatine Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract 3
- 239000013078 crystal Substances 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract 1
- 239000002639 bone cement Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 239000008151 electrolyte solution Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 description 1
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 1
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to an application of a hydrogen sulfate imidazole ion fluid in copper electrolysis refining. The hydrogen sulfate imidazole ion fluid is used as an addition agent applied in electrorefining of copper, and the addition quantity is 25 to 50 ppm. Electrolytic copper with smooth surface and high purity can be achieved through adding a slight amount of addition agent in the copper electrolysis refining process. The ion electric conductivity of the addition agent is high, the chemical thermal stability is good, the using effect is good, convenient and reliable, and compared with the traditional addition agents such as bone glue, thiourea and chloride ion, the hydrogen sulfate imidazole ion fluid can improve the electrolytic copper surface appearance, refine the crystal grains and effectively improve the edge crystal effect.
Description
Technical field
The present invention relates to metallurgical technology field, the particularly application of hydrogen sulfate imidazole ion liquid in electrolytical refined copper.
Background technology
Copper has physics-chem characteristics such as good electrical conductivity, thermal conductivity, erosion resistance and ductility.Conductivity and heat conductivility are only second to silver, and fine copper can pull into very thin copper wire, make very thin Copper Foil.Because numerous premium propertiess, copper has a purposes widely industrial, comprises aspects such as electric utility, machinofacture, traffic, building.In copper smelt industry,, add a small amount of additive in the electrolytic solution of being everlasting in order to obtain the electrolytic copper that surfacing is smooth, purity is high.Additive can not only make cathode copper deposition careful, bright and clean, have toughness, and can reduce foreign matter content in the copper deposition.The additive of tradition electrolytical refined copper mainly comprises gelatine, thiocarbamide, chlorion etc., in use often easily decomposed by the influence of chemistry and thermostability.
Ionic liquid is a kind of green solvent with broad prospect of application, the incomparable advantages of conventional organic solvents such as chemical heat stability is high, not flammable, steam forces down because it has, ionic conductivity height, electrochemical window are wide have become one of the focus in applied research field.Hydrogen sulfate imidazole ion liquid ([BMIM] HSO
4) as a kind of novel ionic liquid, be widely used in all kinds of organic reaction catalyzer in recent years, the difficult leaching agent that leaches copper mine, gold mine, silver ore.But it be yet there are no report as Application of Additives in the metal electrodeposition.
Summary of the invention
The additive sulfuric acid hydrogen imidazole ion liquid that the purpose of this invention is to provide a kind of novel electrolytical refined copper can obtain the uniform cathode copper of refinement after adding this additive on the basis of traditional industry electrolytical refined copper, and can effectively improve the brilliant phenomenon of marginal branch.
Technical scheme of the present invention is: with hydrogen sulfate imidazole ion liquid ([BMIM] HSO
4) as the additive in the electrolytic copper refining, addition is 25-50ppm.
This additive also can use as: gelatine, chlorion or the like mixed with conventional additive.
This additive is compared with conventional additive in the industrial electrolysis refined matte, and major advantage comprises: (1) it is made easily as organic additive, cost is low, ionic conductivity is high.(2) good chemistry and thermostability, heat decomposition temperature is greater than 200 ℃.(3) result of use is good, convenient and reliable, and it is obvious to alleviate the brilliant effect effect of marginal branch.Compare the cathode copper that can not only obtain smooth densification with conventional additive, more can effectively improve the brilliant effect of marginal branch.
Embodiment
Below in conjunction with embodiment the present invention is elaborated.
Embodiment 1:
Preparation standard electrolytic liquid, concrete composition is as follows: 40g l
-1Cu
2+, 160g l
-1H
2SO
4As positive plate, the fine copper sheet is a negative electrode with the copper of pyrorefining; Add hydrogen sulfate imidazole ion liquid additive 50ppm in electrolytic solution, be heated with stirring to 65 ℃, fixed negative pole fine copper sheet reaction area is regulated cathode current density to 280A m
-2, carry out constant-current electrolysis and get final product.
Embodiment 2:
The electrolytic solution moiety is: 30g l
-1Cu
2+, 100g l
-1H
2SO
4Add hydrogen sulfate imidazole ion liquid additive 25ppm, and the change cathode current density is 250A m
-2, other conditions and operation are same as embodiment 1, carry out constant-current electrolysis.
Embodiment 3:
25ppm hydrogen sulfate imidazole ion liquid additive and 25ppm chlorion are mixed in the adding electrolytic solution, and wherein chlorion adds with the form of NaCl, and other conditions and operation are same as embodiment 1, carry out constant-current electrolysis.
The hydrogen sulfate imidazole ion liquid that above embodiment is used, if preparation can be by following carrying out (be example with 1.5mol):
1) preparation of intermediate product: n-propylcarbinyl chloride 1.5mol and N-Methylimidazole 1.5mol are mixed, with toluene 150ml is solvent, mechanical stirring under the 80-90 ℃ of argon shield, through back flow reaction 24-72h after underpressure distillation purify, 70-80 ℃ of following vacuum-drying 8-12h get final product intermediate product;
2) additive is synthetic: will be mixed with sulfuric acid 0.5mol by step 1) gained intermediate product 0.5mol, with distilled water 120ml as solvent, 100-110 ℃ of following mechanical stirring, underpressure distillation is purified behind the back flow reaction 4-6h, and 110-120 ℃ of following vacuum-drying 8-12h can make hydrogen sulfate imidazole ion liquid additive.
Claims (2)
1. the application of hydrogen sulfate imidazole ion liquid in copper electrolyzing refining is characterized in that hydrogen sulfate imidazole ion liquid [BMIM] HSO
4Be applied to electrolytic copper refining as additive, its addition is 25-50ppm.
2. the application of hydrogen sulfate imidazole ion liquid according to claim 1 in copper electrolyzing refining is characterized in that hydrogen sulfate imidazole ion liquid [BMIM] HSO
4Additive mixes use with conventional additive gelatine or chlorion equal proportion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100588696A CN101343750B (en) | 2008-08-29 | 2008-08-29 | Application of sulphuric acid hydrogen imidazole ion liquid in electrolytical refined copper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100588696A CN101343750B (en) | 2008-08-29 | 2008-08-29 | Application of sulphuric acid hydrogen imidazole ion liquid in electrolytical refined copper |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101343750A CN101343750A (en) | 2009-01-14 |
| CN101343750B true CN101343750B (en) | 2010-07-28 |
Family
ID=40245864
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100588696A Expired - Fee Related CN101343750B (en) | 2008-08-29 | 2008-08-29 | Application of sulphuric acid hydrogen imidazole ion liquid in electrolytical refined copper |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101343750B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694982B (en) * | 2015-03-05 | 2018-04-27 | 中国科学院过程工程研究所 | A kind of cyanideless electro-plating Brass Plating Solution and its application method containing ion liquid addictive |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928957B (en) * | 2010-10-04 | 2012-07-11 | 普宁市长欣五金有限公司 | Method for electrolyzing refined copper at room temperature |
| CN102418117B (en) * | 2011-11-29 | 2014-04-16 | 宁波蓝鼎电子科技有限公司 | Method for electrolytic refining in fire refining of cathode copper |
| CN104499002A (en) * | 2014-12-10 | 2015-04-08 | 上海大学 | Method for preparing copper-iron nano plated layer from low-grade sulfide ore through direct electro-deposition |
| CN106011930B (en) * | 2016-07-28 | 2018-09-25 | 河南豫光金铅股份有限公司 | A kind of continuous preparation method of cupric electrolysis refining electrolyte |
| CN107460503B (en) * | 2017-09-14 | 2019-07-02 | 西南科技大学 | The method of micro-nano copper powder is recycled from waste printed circuit board |
-
2008
- 2008-08-29 CN CN2008100588696A patent/CN101343750B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694982B (en) * | 2015-03-05 | 2018-04-27 | 中国科学院过程工程研究所 | A kind of cyanideless electro-plating Brass Plating Solution and its application method containing ion liquid addictive |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101343750A (en) | 2009-01-14 |
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| PB01 | Publication | ||
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| C14 | Grant of patent or utility model | ||
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Granted publication date: 20100728 Termination date: 20130829 |