CN102828042B - Method for extracting silver from silver-containing crude tin alloy - Google Patents
Method for extracting silver from silver-containing crude tin alloy Download PDFInfo
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- CN102828042B CN102828042B CN2012103257155A CN201210325715A CN102828042B CN 102828042 B CN102828042 B CN 102828042B CN 2012103257155 A CN2012103257155 A CN 2012103257155A CN 201210325715 A CN201210325715 A CN 201210325715A CN 102828042 B CN102828042 B CN 102828042B
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- silver
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- tin alloy
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- argentiferous
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 59
- 239000004332 silver Substances 0.000 title claims abstract description 59
- 229910001128 Sn alloy Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 26
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 46
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 16
- 239000011701 zinc Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 5
- 239000002893 slag Substances 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- BSWGGJHLVUUXTL-UHFFFAOYSA-N silver zinc Chemical compound [Zn].[Ag] BSWGGJHLVUUXTL-UHFFFAOYSA-N 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 4
- 229910000679 solder Inorganic materials 0.000 description 4
- 229910001316 Ag alloy Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910017944 Ag—Cu Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QCEUXSAXTBNJGO-UHFFFAOYSA-N [Ag].[Sn] Chemical compound [Ag].[Sn] QCEUXSAXTBNJGO-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000009189 diving Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for extracting silver from silver-containing crude tin alloy. The method comprises the following steps of: heating the silver-containing crude tin alloy to reach the temperature of 430 to 500 DEG C for melting; feeding a zinc ingot into the molten silver-containing crude tin alloy, and agitating to dissolve; cooling the dissolved mixture to reach the temperature of 390 to 400 DEG C; and centrifugally separating at a rotating speed of 200-700rpm until the surface of the liquid at the upper layer has no floating slags, so as to obtain the tin liquid at the upper layer and the sliver-zinc slags at the lower layer; naturally cooling and condensing the tin layer to obtain the tin alloy without silver; and distilling the silver-zinc slags under the vacuum to obtain the silver and the crude zinc, wherein the silver in the tin alloy subjected to silver extracting is less than 10g/t. According to the method, the whole process is safe and controllable; the method is convenient to operate, and has no exhaustion of three wastes; and the method has high universality to the raw materials; the tin alloys with different silver contents can be effectively processed; the continuous industrial production can be achieved; and high recovery rate of the tin and the silver can be ensured; the silver in the silver-containing tin alloy can be efficiently extracted; with adoption of the method, the quality of the tin can be improved, and large amounts of silver can be recovered for the enterprises.
Description
Technical field
The invention belongs to non-ferrous metal pyrometallurgical smelting technical field, relate to a kind of pyrometallurgy technology of using and extract silver-colored method from thick tin.
Background technology
The thick tin of tin ore retailoring output contains much impurity, even the tin of producing from rich tin concentrate, its purity can not meet user's requirement usually.Silver is a kind of comparatively common associated metal, and the silver that usually in the resulting thick tin of retailoring, contains 40～600g/t, although the existence of silver does not affect the quality of tin, extracts silver-colored and is used and has great importance from tin.
Due to the use of large-scale restriction plumber's solder, a large amount of Sn-Ag-Cu scolders are used, and in this kind of scolder, containing having an appointment 3% silver, this just causes the silver-colored problem of recovery in the waste and old electric product to become increasingly conspicuous.
Currently used tin refinement desilver is mainly the method for electrolysis, generally for stanniferous height, thick tin that foreign matter content is low, adopt pyrorefining, when carrying out crystallizer deleading, bismuth, silver energy and tin, the plumbous eutectic that generates, eutectic is temperature lower than the tin fusing point or approaches the impurity of 183 ℃ of left and right, generally enters scolding tin, thereby afterwards solder electrolytic is made silver enter the anode sludge, reaches and reclaims silver-colored purpose; The high thick tin for foreign matter content, the pyrogenic attack operation is many, and the quantity of slag is large, and the direct yield of tin is low, in thick tin, valuable metal is dispensed into slag, reclaim these metals more difficult, and labor condition is bad, environmental protection is poor, usually directly adopts electrorefining, and the precious metal gold and silver all enter the anode sludge.The electrolytic process investment cost is large, in electrolytic process, usually has a large amount of metals to overstock, and owing in scolding tin and thick tin, usually also containing the plurality of impurities such as copper, antimony, arsenic, bismuth, these impurity have Different Effects to electrolytic efficiency, need strict its content of controlling.
In the patent documentation that is CN101033557 at publication number, a kind of tin and silver-colored method of reclaiming from the Pb-free solder waste material disclosed, the method is by after sn-ag alloy powder or fritter melting, be cast into the sn-ag alloy piece, be connected on the negative pole of power supply with block tin, the sn-ag alloy piece is connected on to positive source, the electrolyzer that ion-exchange membrane is housed is put at the two poles of the earth, add electrolytic solution energising to start electrolysis, the alloy on positive pole dissolves and negative pole is separated out pure tin; Take off the pure tin of separating out from negative pole, through washing, fusion-cast becomes ingot, the fine silver obtained after electrolyte filtering, and fusion-cast becomes ingot.It is limited that this method is processed raw material, mainly for lead-free solder, processes and could better realize that tin, silver separate.
Summary of the invention
The object of the present invention is to provide a kind of silver-colored method of extraction in argentiferous crude tin alloy, realize tin silver high efficiency separation, the method is environmentally friendly, safe and practical.
The present invention realizes by following technical proposal: extract silver-colored method in a kind of argentiferous crude tin alloy, following each step of process:
(1) the argentiferous crude tin alloy being warming up to 430～500 ℃ is melted;
(2) zinc ingot metal is joined in the argentiferous crude tin alloy that step (1) gained melted, and stirred fusing;
(3) mixture after step (2) fusing is cooled to 390～400 ℃, then carries out centrifugation under the rotating speed of 200～700 rev/mins, to the upper strata fluid surface without scum silica frost till, obtaining upper strata is tin liquor, lower floor is silver-colored cadmia; The tin alloy of gained tin liquor after natural cooling solidification is desilver;
(4) step (3) gained silver cadmia is obtained to silver and crude zinc after vacuum distilling.
Silver content in the argentiferous crude tin alloy of described step (1) is 40～50000g/t.
Described step (4) gained crude zinc returns to step (2) and recycles.
The present invention adds zinc in the argentiferous crude tin alloy liquid of fusing and constantly and stirs, and makes silver and zinc generate solid chemical compound, and carries out liquid-solid separation, thereby silver is separated with tin, and the silver-colored cadmia obtained obtains silver and crude zinc through vacuum distilling.The advantage that the present invention possesses and effect: silver content<10g/t in the tin alloy after extracting silver.The present invention adopts zincification to extract silver-colored method, and whole process safety is controlled, easy to operate, three-waste free discharge, on personnel and environment, all without impact, high to the raw material universality, the different tin alloy of argentiferous composition all can be effectively addressed, can realize the serialization industrial production, tin, silver raising recovery rate are high, can realize the high efficiency extraction of silver in the argentiferous tin alloy, not only can improve the quality of tin, and can be enterprise and reclaim a large amount of silver, there are to huge environmental benefit and economic benefit in tin manufacturing enterprise.This invention is to extract silver-colored new technology in a tin pyrorefining, can realize the recycling of noble silver in thick tin, has wide market outlook and economic worth.
The accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
(1) the argentiferous crude tin alloy that is 40g/t by the 10t silver content (surplus is Sn) is warming up to 430 ℃ and is melted in the desilver pot;
(2) zinc ingot metal is joined in the argentiferous crude tin alloy that step (1) gained melted, and stirred fusing;
(3) mixture after step (2) fusing is cooled to 390 ℃, the formula of diving centrifuge drum inserts the desilver pot, under the rotating speed of 300 rev/mins, rotation axis rotation 10～15min carries out centrifugation, now silver-colored cadmia enters rotary drum, rotary drum is mentioned on liquid level, centrifugation under the rotating speed of 400 rev/mins, tin liquor is tangential direction along the drum sieve aperture and throws away, the silver cadmia is trapped in rotary drum, again rotary drum is inserted to the desilver pot after slag dumping, then carry out the next cycle operation, until the supernatant liquid surface is without scum silica frost, obtaining upper strata is tin liquor, and lower floor is silver-colored cadmia; The tin alloy of gained tin liquor after natural cooling solidification is desilver;
(4) step (3) gained silver cadmia is obtained to silver and crude zinc after vacuum distilling, the gained crude zinc returns to step (2) and recycles.In tin alloy after extracting silver, silver content is 5g/t.
Embodiment 2
(1) the argentiferous crude tin alloy that is 10000g/t by the 10t silver content (surplus is Sn) is warming up to 460 ℃ and is melted;
(2) zinc ingot metal is joined in the argentiferous crude tin alloy that step (1) gained melted, and stirred fusing;
(3) mixture after step (2) fusing is cooled to 395 ℃, then carries out centrifugation under the rotating speed of 200 rev/mins, to the upper strata fluid surface without scum silica frost till, obtaining upper strata is tin liquor, lower floor is silver-colored cadmia; The tin alloy of gained tin liquor after natural cooling solidification is desilver;
(4) step (3) gained silver cadmia is obtained to silver and crude zinc after vacuum distilling.In tin alloy after extracting silver, silver content is 6g/t.
Embodiment 3
(1) the argentiferous crude tin alloy that is 50000g/t by the 10t silver content (surplus is Sn) is warming up to 500 ℃ and is melted;
(2) zinc ingot metal is joined in the argentiferous crude tin alloy that step (1) gained melted, and stirred fusing;
(3) mixture after step (2) fusing is cooled to 400 ℃, then carries out centrifugation under the rotating speed of 700 rev/mins, to the upper strata fluid surface without scum silica frost till, obtaining upper strata is tin liquor, lower floor is silver-colored cadmia; The tin alloy of gained tin liquor after natural cooling solidification is desilver;
(4) step (3) gained silver cadmia is obtained to silver and crude zinc after vacuum distilling, the gained crude zinc returns to step (2) and recycles.In tin alloy after extracting silver, silver content is 8g/t.
Embodiment 4
(1) the argentiferous crude tin alloy that is 45000g/t by the 10t silver content (surplus is Sn) is warming up to 450～500 ℃ and is melted;
(2) zinc ingot metal is joined in the argentiferous crude tin alloy that step (1) gained melted, and stirred fusing;
(3) mixture after step (2) fusing is cooled to 400 ℃, then carries out centrifugation under the rotating speed of 500～700 rev/mins, to the upper strata fluid surface without scum silica frost till, obtaining upper strata is tin liquor, lower floor is silver-colored cadmia; The tin alloy of gained tin liquor after natural cooling solidification is desilver;
(4) step (3) gained silver cadmia is obtained to silver and crude zinc after vacuum distilling, the gained crude zinc returns to step (2) and recycles.In tin alloy after extracting silver, silver content is 7g/t.
Claims (3)
1. extract silver-colored method in an argentiferous crude tin alloy, it is characterized in that through following each step:
(1) the argentiferous crude tin alloy being warming up to 430～500 ℃ is melted;
(2) zinc ingot metal is joined in the argentiferous crude tin alloy that step (1) gained melted, and stirred fusing;
(3) mixture after step (2) fusing is cooled to 390～400 ℃, then carries out centrifugation under the rotating speed of 200～700 rev/mins, to the upper strata fluid surface without scum silica frost till, obtaining upper strata is tin liquor, lower floor is silver-colored cadmia; The tin alloy of gained tin liquor after natural cooling solidification is desilver;
(4) step (3) gained silver cadmia is obtained to silver and crude zinc after vacuum distilling.
2. extract silver-colored method in argentiferous crude tin alloy according to claim 1, it is characterized in that: the silver content in the argentiferous crude tin alloy of described step (1) is 40～50000g/t.
3. extract silver-colored method in argentiferous crude tin alloy according to claim 1 and 2, it is characterized in that: described step (4) gained crude zinc returns to step (2) and recycles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103257155A CN102828042B (en) | 2012-09-06 | 2012-09-06 | Method for extracting silver from silver-containing crude tin alloy |
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|---|---|---|---|
| CN2012103257155A CN102828042B (en) | 2012-09-06 | 2012-09-06 | Method for extracting silver from silver-containing crude tin alloy |
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| CN102828042A CN102828042A (en) | 2012-12-19 |
| CN102828042B true CN102828042B (en) | 2013-12-18 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104928491B (en) * | 2015-07-07 | 2017-09-26 | 昆明理工大学 | It is a kind of in containing silver-tin alloy plus wood chip desilver method |
| CN105349796A (en) * | 2015-11-30 | 2016-02-24 | 来宾华锡冶炼有限公司 | Method for extracting coarse silver from coarse soldering tin |
| CN106319234B (en) * | 2016-08-23 | 2018-05-08 | 魏清松 | A kind of method for recycling zinc-aluminium iron lead in plating cadmia |
| CN108277358B (en) * | 2018-03-13 | 2019-07-05 | 昆明理工大学 | A method of adding magnesium desilver in containing silver-tin alloy |
| CN108950246A (en) * | 2018-07-03 | 2018-12-07 | 昆明理工大学 | A kind of hypergravity is removed containing method silver-colored in silver-tin alloy |
| CN115029554A (en) * | 2022-02-17 | 2022-09-09 | 昆明理工大学 | Method for recovering silver from waste circuit board solder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE2930693A1 (en) * | 1979-07-28 | 1981-02-12 | Kloeckner Humboldt Deutz Ag | Refining of metals with low m.pts., esp. lead, tin or zinc - which are pored into vibratory mixer reactor with reagents which combine with impurities in the molten metal |
| JPS56146834A (en) * | 1980-04-15 | 1981-11-14 | Nippon Mining Co Ltd | Recovering method for valuable substance such as indium |
| JP2004315865A (en) * | 2003-04-14 | 2004-11-11 | Dowa Mining Co Ltd | Method for recovering tin from tin-containing material |
| CN101358298B (en) * | 2008-09-25 | 2010-06-02 | 昆明理工大学 | Desilverization method during bismuth refining procedure |
| CN101886174B (en) * | 2010-06-23 | 2012-08-29 | 郴州雄风稀贵金属材料股份有限公司 | Process for refining high-purity bismuth from bismuth-containing material generated from anode mud recovery |
| CN201933133U (en) * | 2010-12-24 | 2011-08-17 | 株洲科能新材料有限责任公司 | Device for producing high-purity bismuth from raw bismuth in desilverizing mode |
| CN102162035A (en) * | 2011-04-07 | 2011-08-24 | 赵志强 | Vacuum distillation process for extracting silver from silver zinc slag |
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