CN101880777A - Method for removing bismuth and antimony in electrolytic silver powder by utilizing clay-graphite crucible for smelting - Google Patents
Method for removing bismuth and antimony in electrolytic silver powder by utilizing clay-graphite crucible for smelting Download PDFInfo
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- CN101880777A CN101880777A CN 201010226978 CN201010226978A CN101880777A CN 101880777 A CN101880777 A CN 101880777A CN 201010226978 CN201010226978 CN 201010226978 CN 201010226978 A CN201010226978 A CN 201010226978A CN 101880777 A CN101880777 A CN 101880777A
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- silver powder
- electrolytic silver
- graphite crucible
- clay
- antimony
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Abstract
The invention relates to a method for removing bismuth and antimony in electrolytic silver powder by utilizing a clay-graphite crucible for smelting, which comprises the steps of uniformly mixing the electrolytic silver powder, saltpeter which accounts for 1-2% of the weight of the electrolytic silver powder, borax which accounts for 2-3% of the weight of the electrolytic silver powder and quartz powder which accounts for 2-3% of the electrolytic silver powder, adding into the clay-graphite crucible, and carrying out the reaction for 2-3h under the condition of 1100-1300 DEG C. The use of the method for treatment can lead the content of the bismuth and the content of the antimony in the electrolytic silver powder to be less than 0.0005%, achieve the GB/T 4135-2002.1 silver standard, and greatly prolong the service life of the crucible.
Description
(1), technical field
The present invention relates to a kind of method of utilizing the clay-graphite crucible melting to remove bismuth antimony in the electrolytic silver powder, is to be primarily aimed at a kind of pyrogenic process method of purification that electrolytic silver powder that bismuth antimony exceeds standard carries out.
(2), background technology
Existing silver refinery practice mainly comprises silver-colored electrolysis, chemical refining, solvent extraction etc.According to practice for many years, the silver of silver preparing electrolysis process production does not reach 2
#The silver label standard.And chemical refining or solvent extraction need to increase great amount of investment and too high to site requirements.
The silver that some refinery's electrorefining of silver is produced contains a small amount of bismuth, antimony and other impurity, and finished product does not reach GB/T 4135-20022
#The silver label standard is not though still reach technical requirements through electrolysis repeatedly.Not only increase production cost, and increased employee's labor capacity greatly.
(3), summary of the invention
Technical problem to be solved by this invention is, a kind of method of utilizing the clay-graphite crucible melting to remove bismuth antimony in the electrolytic silver powder is provided, by electrolytic silver powder is implemented oxidation, slag making processing in clay-graphite crucible, scalp, low-cost bismuth, antimony, the quality of the finished product silver that raising is produced effectively removed down.
In order to solve the problems of the technologies described above, the present invention has adopted following technical scheme.
A kind of method of utilizing the clay-graphite crucible melting to remove bismuth antimony in the electrolytic silver powder is characterized in that:
The first step: with electrolytic silver powder, the nitre of electrolytic silver powder weight 1～2%, the silica powder mixing of the borax of electrolytic silver powder weight 2～3% and electrolytic silver powder weight 2～3% adds in the clay-graphite crucible, reacts 2～3 hours under 1100～1300 ℃ of conditions;
Wherein, used silica powder granularity requirements Φ＜0.074mm.
Second step: discharging; Isolate scum silica frost in the discharging process.
Wherein the optimum ratio of the first step and processing condition are: with electrolytic silver powder, the nitre of electrolytic silver powder weight 1.5%, the silica powder mixing of the borax of electrolytic silver powder weight 2.5% and electrolytic silver powder weight 2.5% adds in the clay-graphite crucible, and reaction is 3 hours under 1200 ℃ of conditions.
Positively effect of the present invention is:
The present invention allocates an amount of oxygenant--nitre into according to the bismuth in the electrolytic silver powder, antimony and other foreign matter contents, and bismuth, antimony etc. is oxidized to Bi respectively
2O
3, Sb
2O
3, Sb
2O
5, CuO, PbO etc.
The present invention adds an amount of slag former---borax according to impurity component in the electrolytic silver powder and content, and all kinds of oxide impurities that high temperature oxygen is changed into react with it, generates the slag phase, thereby separates with silver, reaches the refining purpose.
The present invention also adds an amount of crucible protective material--silica powder.Because under the high temperature oxidation state; the clay-graphite crucible oxidation that intermediate frequency furnace adopted is fast especially; as not adding an amount of protective material; crucible is easy to oxidized and seepage even broken crucible accident takes place, and this is the key of this invention---not only utilize the intermediate frequency furnace high temperature oxidation stability but also solved a not sludge proof difficult problem of clay-graphite crucible.Wherein the consumption of silica powder is very important, and too high meeting causes production cost to improve, and because the silica powder infusibility also can influence smelting efficiency.Consumption is crossed the low purpose that does not then reach the protection crucible.
According to method of the present invention, same crucible uses three times, and each 3 hours, the crucible wall thickness still kept about 1/3rd.And if do not add silica powder, melting promptly occurred run-down in 2 hours.
Handle through the inventive method, bismuth, antimony content reach GB/T4135-20021 all less than 0.0005% in the electrolytic silver powder
#The standard of silver.
(4), embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment one
The first step: with electrolytic silver powder, the saltpetre of electrolytic silver powder weight 1%, the silica powder mixing of the borax of electrolytic silver powder weight 3% and electrolytic silver powder weight 2% adds in the clay-graphite crucible, and reaction is 2 hours under 1300 ℃ of conditions;
Wherein, used silica powder granularity requirements Φ＜0.074mm.
Second goes on foot: the electrolytic silver powder after reaction is finished is poured the cast iron mould into, is cooled to high-purity silver ingot.Isolate scum silica frost in the discharging process.
Use inductive coupling plasma emission spectrograph ICP to detect, finished product bismuth, antimony content all are lower than and detect lower limit 0.0005%.
Embodiment two
The first step: with electrolytic silver powder, the SODIUMNITRATE of electrolytic silver powder weight 2%, the silica powder mixing of the borax of electrolytic silver powder weight 2% and electrolytic silver powder weight 3% adds in the clay-graphite crucible, and reaction is 3 hours under 1100 ℃ of conditions;
Wherein, used silica powder granularity requirements Φ＜0.074mm.
Second step: discharging, isolate scum silica frost in the discharging process.
Use inductive coupling plasma emission spectrograph ICP to detect, finished product bismuth, antimony content all are lower than and detect lower limit 0.0005%.
Embodiment three
The first step: with electrolytic silver powder, the saltpetre of electrolytic silver powder weight 1.5%, the silica powder mixing of the borax of electrolytic silver powder weight 2.5% and electrolytic silver powder weight 2.5% adds in the clay-graphite crucible, and reaction is 3 hours under 1200 ℃ of conditions;
Wherein, used silica powder granularity requirements Φ＜0.074mm.
Second goes on foot: the electrolytic silver powder after reaction is finished is poured the cast iron mould into, is cooled to high-purity silver ingot.Isolate scum silica frost in the discharging process.
Use inductive coupling plasma emission spectrograph ICP to detect, finished product bismuth, antimony content all are lower than and detect lower limit 0.0005%.
Comparative Examples one
With electrolytic silver powder, the saltpetre of electrolytic silver powder weight 0.5%, the borax mixing of electrolytic silver powder weight 2.5% adds in the clay-graphite crucible, and reaction is 2 hours under 1200 ℃ of conditions; Other technology is with embodiment two.
Use inductive coupling plasma emission spectrograph ICP to detect finished product bi content 0.027%.
Comparative Examples two
With electrolytic silver powder, the saltpetre of electrolytic silver powder weight 1%, the borax mixing of electrolytic silver powder weight 2.5% adds in the clay-graphite crucible, and reaction is 3 hours under 1200 ℃ of conditions; Other technology is with embodiment two.
Use inductive coupling plasma emission spectrograph ICP to detect finished product bi content 0.0006%.
Claims (2)
1. method of utilizing the clay-graphite crucible melting to remove bismuth antimony in the electrolytic silver powder is characterized in that:
The first step: with electrolytic silver powder, the nitre of electrolytic silver powder weight 1～2%, the silica powder mixing of the borax of electrolytic silver powder weight 2～3% and electrolytic silver powder weight 2～3% adds in the clay-graphite crucible, reacts 2～3 hours under 1100～1300 ℃ of conditions;
Wherein, used silica powder granularity requirements Φ＜0.074mm.
Second step: discharging; Isolate scum silica frost in the discharging process.
2. the method for utilizing the clay-graphite crucible melting to remove bismuth antimony in the electrolytic silver powder as claimed in claim 1, it is characterized in that: the first step wherein: with electrolytic silver powder, the nitre of electrolytic silver powder weight 1.5%, the silica powder mixing of the borax of electrolytic silver powder weight 2.5% and electrolytic silver powder weight 2.5%, add in the clay-graphite crucible, reaction is 3 hours under 1200 ℃ of conditions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102269781A CN101880777B (en) | 2010-07-15 | 2010-07-15 | Method for removing bismuth and antimony in electrolytic silver powder by utilizing clay-graphite crucible for smelting |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102269781A CN101880777B (en) | 2010-07-15 | 2010-07-15 | Method for removing bismuth and antimony in electrolytic silver powder by utilizing clay-graphite crucible for smelting |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101880777A true CN101880777A (en) | 2010-11-10 |
| CN101880777B CN101880777B (en) | 2012-02-22 |
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| CN2010102269781A Expired - Fee Related CN101880777B (en) | 2010-07-15 | 2010-07-15 | Method for removing bismuth and antimony in electrolytic silver powder by utilizing clay-graphite crucible for smelting |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1339619A (en) * | 2000-08-23 | 2002-03-13 | 内蒙古乾坤金银精炼股份有限公司 | Method for removing bismuth and antiomny from silver electrolyte |
| CN1396962A (en) * | 2000-01-28 | 2003-02-12 | 尤密考公司 | Process for refining silver bullion with gold separation |
| CN101054627A (en) * | 2006-04-11 | 2007-10-17 | 肇庆市大鸿明贵金属有限公司 | Method of refining noble lead or dore silver |
-
2010
- 2010-07-15 CN CN2010102269781A patent/CN101880777B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1396962A (en) * | 2000-01-28 | 2003-02-12 | 尤密考公司 | Process for refining silver bullion with gold separation |
| US20030154821A1 (en) * | 2000-01-28 | 2003-08-21 | Dirk Vanhoutte | Process for refining silver bullion with gold separation |
| CN1339619A (en) * | 2000-08-23 | 2002-03-13 | 内蒙古乾坤金银精炼股份有限公司 | Method for removing bismuth and antiomny from silver electrolyte |
| CN101054627A (en) * | 2006-04-11 | 2007-10-17 | 肇庆市大鸿明贵金属有限公司 | Method of refining noble lead or dore silver |
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| CN101880777B (en) | 2012-02-22 |
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Effective date of registration: 20180110 Address after: 261441, No. 888, dragon village, Jin Town, Yantai City, Shandong, Laizhou Patentee after: Shandong gold smelting Co., Ltd. Address before: 261441 Jincheng Jiaojia, Laizhou City, Shandong Province Patentee before: Shandong Gold Mine (Laizhou) Co., Ltd. Refinery |
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Granted publication date: 20120222 Termination date: 20180715 |
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