CN102797017A - Method for preparing high-purity metallic silver - Google Patents
Method for preparing high-purity metallic silver Download PDFInfo
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- CN102797017A CN102797017A CN2011101349209A CN201110134920A CN102797017A CN 102797017 A CN102797017 A CN 102797017A CN 2011101349209 A CN2011101349209 A CN 2011101349209A CN 201110134920 A CN201110134920 A CN 201110134920A CN 102797017 A CN102797017 A CN 102797017A
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Abstract
The invention relates to a method for preparing high-purity metallic silver with the purity of more than 99.9999 percent. The method comprises the following steps of: preparing electrolyte from deionized water, analytically pure concentrated nitric acid and analytically pure silver nitrate, performing electrolysis by using a metallic silver clad double-layer anode bag with the purity of 99.99 percent as an anode and using a titanium net or a silver net as a cathode, and thus obtaining the high-purity metallic silver with the purity of more than 99.9999 percent on the cathode by controlling the electrolysis conditions. The method is simple and convenient to operate, and the metallic silver is big and high in purity.
Description
Technical field
The present invention relates to the preparation method of a kind of purity, particularly a kind of method for preparing high fine silver with electrolytic refining process at the silver of the high pure metal more than 99.9999%.
Background technology
Silver is as important industrial raw material, and its purposes very extensively.High fine silver has good conductive, heat conductivility, is excellent electrical conductor and heat conductor, and is along with expanding economy, also increasingly high to the requirement of silver-colored purity.Be equipped with in the technology in many silvery, successfully prepared 99.99% purity silver.People such as Xu Lanying utilize the AgCl deposition to obtain the chemical reduction method of high-purity silver powder with ammonia-hydrazine reduction, make the total content of impurity be lower than 10ppm, reach the requirement of 99.99% silver medal basically.Publication number is the Chinese invention patent " high purity silver preparing electrolysis process " of CN1974860A, prepares silver powder with electrolysis process, but just reaches 99.99% purity.
In order to adapt to the needs of industrial development, along with the develop rapidly of microelectronic industry, seek the more preparation approaches and methods of high-purity silver, become the problem that domestic and international extremely is attracted attention.And the preparation of 99.9999% high fine silver does not also appear in the newspapers at present.This patent has obtained purity at the argent more than 99.9999% through electrolytic smelting method at the specified conditions electrolytic deposition.
Summary of the invention
The object of the invention aims to provide the method for manufacture of a kind of purity at the silver of the high pure metal more than 99.9999%, particularly relates to the preparation of carrying out high fine silver with electrolytic smelting method.
For realizing above-mentioned purpose, the present invention takes following technical scheme:
A kind of preparation method of high pure metal silver; Its step comprises: with deionized water, analytical pure concentrated nitric acid and analytical pure Silver Nitrate preparing electrolyte; Argent overcoat bilayer anode bag with 99.99% purity constitutes anode; With titanium net or silver-colored net is that negative electrode carries out electrolysis, can obtain high pure metal silver at negative electrode.
A kind of optimized technical scheme is characterized in that: the Ag that contains 150-650g/L in the said electrolytic solution
+HNO with 2-10g/L
3
A kind of optimized technical scheme is characterized in that: impurity concentration is in the said electrolytic solution: Cu < 0.05g/>L, Bi < 0.02g/>L and Pb < 0.02g/>L.
A kind of optimized technical scheme is characterized in that: the interpole gap between negative electrode and the anode is 5-20cm.
A kind of optimized technical scheme is characterized in that: during electrolysis, cathode current density is 50-500A/m
2
A kind of optimized technical scheme is characterized in that: the purity of the high pure metal silver that electrolysis obtains is more than 99.9999%, and promptly the argent with 99.99% purity is a raw material, and the purity of the high pure metal silver that electrolysis obtains is more than 99.9999%.
The advantage that this high-purity silvery is equipped with technology is:
The present invention has that technology is simple, easy to operate, product form is thick, the advantage that purity is high.Utilize this technology, it is the high fine silver of 99.9999% above purity that the stock silver of 99.99% purity is purified.
Through embodiment the present invention is further specified below.
Embodiment
Embodiment 1
With deionized water, analytical pure concentrated nitric acid and analytical pure Silver Nitrate preparation concentration of silver ions is 150g/L, and concentration of nitric acid is the electrolytic solution of 2g/L.Analyze through ICP-OES, impurity concentration is Cu < 0.05g/>L, Bi < 0.02g/>L and Pb < 0.02g/>L in the electrolytic solution.As anode, the titanium net is a negative electrode with 99.99% silver plate overcoat bilayer anode bag, and interpole gap is 5cm, is 50A/m in cathode current density
2Carry out electrolysis under the condition, scraped silver powder from negative electrode in per 24 hours, washing, vacuum-drying.
The major impurity content of the silver powder that obtains is seen table 1:
Table 1 major impurity content is (GD-MS analyzes, the ppm of unit) relatively
| Element | Fe | Ni | Cu | Se | Au | Pd | Pb | Bi |
| Stock silver | 0.073 | 0.13 | 9.20 | 0.062 | 0.40 | 0.75 | 0.17 | 0.13 |
| Product silver powder | 0.025 | <0.1 | <0.1 | <0.1 | <0.01 | <0.1 | <0.005 | 0.007 |
Embodiment 2
With deionized water, analytical pure concentrated nitric acid and analytical pure Silver Nitrate preparation concentration of silver ions is 650g/L, and concentration of nitric acid is the electrolytic solution of 10g/L.Analyze through ICP-OES, impurity concentration is Cu < 0.05g/>L, Bi < 0.02g/>L and Pb < 0.02g/>L in the electrolytic solution.As anode, silver-colored net is a negative electrode with 99.99% silver plate overcoat bilayer anode bag, and interpole gap is 20cm, is 500A/m in cathode current density
2Carry out electrolysis under the condition, scraped silver powder from negative electrode in per 2 hours, washing, vacuum-drying.
The major impurity content of the silver powder that obtains is seen table 2:
Table 2 major impurity content is (GD-MS analyzes, the ppm of unit) relatively
| Element | Fe | Ni | Cu | Se | Au | Pd | Pb | Bi |
| Stock silver | 0.073 | 0.13 | 9.20 | 0.062 | 0.40 | 0.75 | 0.17 | 0.13 |
| Product silver powder | 0.020 | <0.05 | <0.1 | <0.1 | <0.01 | <0.1 | <0.005 | <0.005 |
Embodiment 3
With deionized water, analytical pure concentrated nitric acid and analytical pure Silver Nitrate preparation concentration of silver ions is 350g/L, and concentration of nitric acid is the electrolytic solution of 3.5g/L.Analyze through ICP-OES, impurity concentration is Cu < 0.05g/>L, Bi < 0.02g/>L and Pb < 0.02g/>L in the electrolytic solution.As anode, silver-colored net is a negative electrode with 99.99% silver plate overcoat bilayer anode bag, and interpole gap is 10cm, is 300A/m in cathode current density
2Carry out electrolysis under the condition, scraped silver powder from negative electrode in per 4 hours, washing, vacuum-drying.
The major impurity content of the silver powder that obtains is seen table 3:
Table 3 major impurity content is (GD-MS analyzes, the ppm of unit) relatively
| Element | Fe | Ni | Cu | Se | Au | Pd | Pb | Bi |
| Stock silver | 0.05 | 0.03 | 16 | 0.05 | 0.50 | 0.8 | 0.23 | 0.12 |
| Product silver powder | 0.022 | <0.05 | <0.05 | <0. 1 | <0.01 | <0.1 | <0.005 | <0.005 |
Embodiment 4
With deionized water, analytical pure concentrated nitric acid and analytical pure Silver Nitrate preparation concentration of silver ions is 150g/L, and concentration of nitric acid is the electrolytic solution of 2.5g/L.Analyze through ICP-OES, impurity concentration is Cu < 0.05g/>L, Bi < 0.02g/>L and Pb < 0.02g/>L in the electrolytic solution.As anode, the titanium net is a negative electrode with 99.99% silver plate overcoat bilayer anode bag, and interpole gap is 7cm, is 100A/m in cathode current density
2Carry out electrolysis under the condition, scraped silver powder from negative electrode in per 12 hours, washing, vacuum-drying.
The major impurity content of the silver powder that obtains is seen table 4:
Table 4 major impurity content is (GD-MS analyzes, the ppm of unit) relatively
| Element | Fe | Ni | Cu | Se | Au | Pd | Pb | Bi |
| Stock silver | 0.05 | 0.03 | 16 | 0.05 | 0.50 | 0.8 | 0.23 | 0.12 |
| Product silver powder | 0.023 | <0.1 | <0.05 | <0.05 | <0.01 | <0.1 | <0.005 | 0.005 |
Claims (6)
1. the preparation method of high pure metal silver; Its step comprises: with deionized water, analytical pure concentrated nitric acid and analytical pure Silver Nitrate preparing electrolyte; Argent overcoat bilayer anode bag with 99.99% purity constitutes anode; With titanium net or silver-colored net is that negative electrode carries out electrolysis, can obtain high pure metal silver at negative electrode.
2. the preparation method of high pure metal silver according to claim 1 is characterized in that: the Ag that contains 150-650g/L in the said electrolytic solution
+HNO with 2-10g/L
3
3. the preparation method of high pure metal silver according to claim 2, it is characterized in that: impurity concentration is in the said electrolytic solution: Cu < 0.05g/>L, Bi < 0.02g/>L and Pb < 0.02g/>L.
4. the preparation method of high pure metal silver according to claim 1, it is characterized in that: the interpole gap between described negative electrode and the anode is 5-20cm.
5. the preparation method of high pure metal silver according to claim 1, it is characterized in that: during electrolysis, cathode current density is 50-500A/m
2
6. the preparation method of high pure metal silver according to claim 1 is characterized in that: the purity of the high pure metal silver that electrolysis obtains is more than 99.9999%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526232A (en) * | 2013-09-26 | 2014-01-22 | 山东国大黄金股份有限公司 | Method for removing impurities contained in high-impurity crude silver |
| CN104105355A (en) * | 2013-04-12 | 2014-10-15 | 北大方正集团有限公司 | Method for improving corrosion resistance of Goldfinger, method for manufacturing PCB and PCB |
| CN104264189A (en) * | 2014-10-16 | 2015-01-07 | 云南驰宏锌锗股份有限公司 | Method for silver refining and continuous electrolysis |
| CN105274567A (en) * | 2014-05-27 | 2016-01-27 | 中色金银贸易中心有限公司 | Production process of high purity silver by high frequency electrolysis |
| CN105297074A (en) * | 2015-12-02 | 2016-02-03 | 国药集团化学试剂有限公司 | Preparation method of high-pure silver |
| CN109023434A (en) * | 2018-09-06 | 2018-12-18 | 深圳金莱利黄金珠宝有限公司 | A kind of preparation method, its purifying plant and its product of high pure metal silver |
| CN110387563A (en) * | 2019-07-26 | 2019-10-29 | 紫金矿业集团黄金冶炼有限公司 | A kind of industrial production process of 5N high purity silver |
| CN113186567A (en) * | 2021-04-21 | 2021-07-30 | 深圳金莱利黄金珠宝有限公司 | Silver purification method and silver product |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63213688A (en) * | 1988-01-29 | 1988-09-06 | Nippon Mining Co Ltd | Electrolysis method for producing high purity gold |
| JPH09256083A (en) * | 1996-03-15 | 1997-09-30 | Dowa Mining Co Ltd | Method for manufacturing high purity silver and equipment therefor |
| JP2000038692A (en) * | 1998-07-22 | 2000-02-08 | Kamioka Kogyo Kk | Production of high purity silver |
| US6522918B1 (en) * | 2000-02-09 | 2003-02-18 | William E. Crisp | Electrolytic device |
| CN1974860A (en) * | 2006-11-10 | 2007-06-06 | 湖南省鑫达银业有限公司 | High purity silver preparing electrolysis process |
| CN101667566A (en) * | 2009-09-20 | 2010-03-10 | 宁波康强电子股份有限公司 | Gold-coated-sliver base bonding silk thread and manufacture method thereof |
-
2011
- 2011-05-24 CN CN201110134920.9A patent/CN102797017B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63213688A (en) * | 1988-01-29 | 1988-09-06 | Nippon Mining Co Ltd | Electrolysis method for producing high purity gold |
| JPH09256083A (en) * | 1996-03-15 | 1997-09-30 | Dowa Mining Co Ltd | Method for manufacturing high purity silver and equipment therefor |
| JP2000038692A (en) * | 1998-07-22 | 2000-02-08 | Kamioka Kogyo Kk | Production of high purity silver |
| US6522918B1 (en) * | 2000-02-09 | 2003-02-18 | William E. Crisp | Electrolytic device |
| CN1974860A (en) * | 2006-11-10 | 2007-06-06 | 湖南省鑫达银业有限公司 | High purity silver preparing electrolysis process |
| CN101667566A (en) * | 2009-09-20 | 2010-03-10 | 宁波康强电子股份有限公司 | Gold-coated-sliver base bonding silk thread and manufacture method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 杨国才编著: "《闪速炼铜工艺于控制》", 31 December 2010, 中南大学出版社 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104105355A (en) * | 2013-04-12 | 2014-10-15 | 北大方正集团有限公司 | Method for improving corrosion resistance of Goldfinger, method for manufacturing PCB and PCB |
| CN103526232A (en) * | 2013-09-26 | 2014-01-22 | 山东国大黄金股份有限公司 | Method for removing impurities contained in high-impurity crude silver |
| CN103526232B (en) * | 2013-09-26 | 2016-04-20 | 山东国大黄金股份有限公司 | The removal methods of impurity in a kind of high impurity crude silver |
| CN105274567A (en) * | 2014-05-27 | 2016-01-27 | 中色金银贸易中心有限公司 | Production process of high purity silver by high frequency electrolysis |
| CN105274567B (en) * | 2014-05-27 | 2018-07-10 | 方超 | The production technology of high-frequency electrolysis high-purity silver |
| CN104264189A (en) * | 2014-10-16 | 2015-01-07 | 云南驰宏锌锗股份有限公司 | Method for silver refining and continuous electrolysis |
| CN105297074A (en) * | 2015-12-02 | 2016-02-03 | 国药集团化学试剂有限公司 | Preparation method of high-pure silver |
| CN109023434A (en) * | 2018-09-06 | 2018-12-18 | 深圳金莱利黄金珠宝有限公司 | A kind of preparation method, its purifying plant and its product of high pure metal silver |
| CN110387563A (en) * | 2019-07-26 | 2019-10-29 | 紫金矿业集团黄金冶炼有限公司 | A kind of industrial production process of 5N high purity silver |
| CN113186567A (en) * | 2021-04-21 | 2021-07-30 | 深圳金莱利黄金珠宝有限公司 | Silver purification method and silver product |
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| CN102797017B (en) | 2016-02-24 |
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