CN102534249B - Method for refining tin from high-silver crude tin - Google Patents
Method for refining tin from high-silver crude tin Download PDFInfo
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- CN102534249B CN102534249B CN 201210041041 CN201210041041A CN102534249B CN 102534249 B CN102534249 B CN 102534249B CN 201210041041 CN201210041041 CN 201210041041 CN 201210041041 A CN201210041041 A CN 201210041041A CN 102534249 B CN102534249 B CN 102534249B
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Abstract
The invention discloses a method for refining tin from high-silver crude tin. According to the method, high-silver crude tin from which copper, iron, arsenic and antimony are removed in a tin melting pot is used, the temperature in an electrothermal crystallizing machine is raised and controlled to be 190 to 260 DEG C. The method mainly comprises the following steps: raising the temperature in the electrothermal crystallizing machine, allowing the electrothermal crystallizing machine to spray water and crystallize the molten coarse tin, casting the fine tin and the like, wherein in the temperature raising and water spraying and crystallizing processes of the electrothermal crystallizing machine, the rotation speed of the crystallizing machine is controlled, the temperatures of four stages of the crystallizing machine are regulated to the melting point range of the lead, tin and sliver alloy, and the crystallization of the lead, tin and sliver alloy and liquation of metals in the alloy are performed continuously. The silver content in the fine tin treated by the method is less than 100g/t, which is much lower compared with the silver content of 500 to 10,000g/t achieved by the conventional treatment method. When the method is used, the fine tin is produced by performing crystallization once, only 10 to 30 percent of soldering tin is delivered to be electrolyzed for recovering noble metals such as silver, the required electrolytic equipment investment is 10 to 30 percent of that required by the conventional method, and as less materials are required to be treated during the recovery of noble metals, the production cost is reduced directly.
Description
Technical field
The invention belongs to the tin field of metallurgy, the method for specifically producing refined tin as the raw material refining take the high thick tin of argentiferous.
Background technology
Remove lead and bismuth in the thick tin with electrorefining successive crystallization machine, that continues processes the thick scolding tin of byproduct of crystallizer with vacuum distillation furnace, becomes one of characteristic of China's tin pyrorefining.The general argentiferous of thick tin of processing with the electric heating crystallizer is at 200-1000g/t, and the tin ore argentiferous in area, south, Hunan is higher, the thick tin of high silver that particularly forms by the tin that reclaims in the lead materials, argentiferous 1000-30000g/t, the method of taking off lead, bismuth by general electric heating crystallizer, silver separates undesirable, the silver of 10-50% enters refined tin, must silver thoroughly could be separated through once electrolytic again, or first with precious metals such as the thick tin electrolytic separation silver of height silver, tin is advanced crystallizer separation of lead, bismuth etc. and the output refined tin again.And the inventive method can once remove lead, bismuth, silver etc. in scolding tin by electrorefining successive crystallization machine, and direct production goes out the refined tin that argentiferous is lower than 200g/t, thereby tin, silver are separated more up hill and dale.
Summary of the invention
The object of the present invention is to provide a kind of solder pot copper removal, iron, arsenic, antimony of passing through, crystallizer takes off lead, silver, bismuth etc. and the method for refining production refined tin.
Present method is with the thick tin of high silver by solder pot copper removal, iron, arsenic, antimony, by heightening electric heating crystallizer temperature, reach 190-260 ℃ in the fusing point zone of lead, tin, silver alloys, uninterruptedly carrying out of lead, tin, silver alloys crystallization, liquate, finally obtain argentiferous and be lower than the refined tin of 100g/t and the scolding tin of stanniferous 65-80%, specifically may further comprise the steps:
1, the electric heating crystallizer heats up
Crystallizer speed adjustment to 1.5 turns/min, open one, two, three, four section, be warming up to one section behind the 30-90min: 190-220 ℃, two sections: 350-450 ℃, three sections: 400-500 ℃, four sections: 450-550 ℃, to pump into fireless cooker except the thick tin of high silver of Fe, As, Sb, Cu from solder pot, and put into crystallizer from fireless cooker, after one section of extremely thick tin liquor face covering scolding tin exit end crystallographic axis, be 1-4 liter/min with the speed setting of fireless cooker feed liquor, beginning at opening for feed to even water spray between the scolding tin discharge gate;
2, electric heating crystallizer water spray crystallization
The crystallizer speed adjustment turns/min to 1.5-5.0, the feed liquor speed setting is 1-4 liter/min, injection flow rate is the weight 2-10% of feed liquor amount, when beginning crystal to four sections, it is one section with each section temperature regulation: 190-260 ℃, two sections: 350-500 ℃, three sections: 400-650 ℃, four sections: 450-800 ℃, feed liquor amount, injection flow rate are constant, regular discharge scolding tin, after 4-8 hour, four sections product tin that go out are leaded less than 0.03%, argentiferous 10-200g/t, reach the refined tin standard, pour refined tin founding pot into, scolding tin send electrolytic recovery gold and silver precious metal;
3, refined tin founding
Pour the product tin that crystallizer produces into refined tin founding pot, heat up and melt to temperature 280-320 ℃, start stirrer 10-20min, drag for clean oxidation sludge, tin liquor is put into the moulding of tin ingot casting.
Beneficial effect of the present invention:
1, the silver in the thick tin of the high silver of present method energy effective separation, direct production goes out qualified refined tin, and the decreasing ratio of silver reaches more than 99%, and the method for the thick tin of the high silver of conventional processing, the refined tin argentiferous has 500-10000g/t, and the refined tin after the present invention processes is lower than 100g/t, improves significantly;
2, facility investment is few, production cost is low, present method adopts primary crystallization to produce refined tin, only have total amount 10-30% scolding tin to send to electrolytic recovery silver and wait precious metal, the facility investment of required electrolysis also is the 10-30% of ordinary method, and handled material is few during because of the recovery precious metal, has directly reduced production cost.
Embodiment
Embodiment one
Thick tin: the 7.450t of the high silver of impurity removing, the chemical examination composition sees Table 1,
Equipment: 1 of 10t electric heating crystallizer
Time: 24 hours
The thick tin chemical examination of the high silver of table 1 composition
1, the electric heating crystallizer heats up
Crystallizer speed adjustment to 1.5 turns/min, opens one, two, three, four section, is warming up to one section behind the 45min: 195 ℃, and two sections: 380 ℃, three sections: 420 ℃, four sections: 506 ℃.To pump into fireless cooker except the thick tin of high silver of Fe, As, Sb, Cu from closing the tin pot, and the fireless cooker tap valve all opened, the thick tin of high silver is put into crystallizer, to one section (scolding tin exit end) crystallographic axis of liquid level covering, be 1-1.5 liter/min with the speed setting of fireless cooker feed liquor, beginning at opening for feed to even water spray between the scolding tin discharge gate;
2, electric heating crystallizer water spray crystallization operation
Regulating the crystallizer rotating speed and be 2.5 turns/min, the feed liquor speed setting is 1-1.5 liter/min, injection flow rate is the weight 2-10% of feed liquor amount, when beginning crystal to four sections, is one section with each section temperature regulation: 210-260 ℃, two sections: 350-450 ℃, three sections: 400-500 ℃, four sections: 550-700 ℃, the feed liquor amount, injection flow rate is constant, 20-40min discharges a scolding tin, after 6 hours, four sections product tin that goes out is leaded 0.028%, argentiferous 86g/t, continue crystallization operation, after 7 hours, crystallization operation is finished, and moves back the groove common property and goes out finished product tin: 4.868t, scolding tin: 2.571t, the scolding tin composition sees Table 2.
Table 2 scolding tin composition
3, refined tin founding
Pour the product tin that crystallizer produces into refined tin founding pot, heat up and melt to 300 ° of C of temperature, start stirrer 10min, drag for clean oxidation sludge, tin liquor is put into the moulding of tin ingot casting, produces refined tin 4.790t, and the refined tin composition sees Table 3.
Table 3 refined tin composition
Embodiment two
Raw material: thick tin: the 32.86t of the high silver of removal of impurities, the chemical examination composition sees Table 4.
Equipment: 1 of 10t electric heating crystallizer.
Time: 48 hours.
The thick tin chemical examination of the high silver of table 4 composition
1, the electric heating crystallizer heats up
Crystallizer speed adjustment 1.5 turns/min, is warming up to one section after opening one, two, three, four section 45min: 198 ℃, and two sections: 416 ℃, three sections: 458 ℃, four sections: 523 ℃.To pump into fireless cooker except the thick tin of high silver of Fe, As, Sb, Cu from closing the tin pot, and the fireless cooker tap valve all opened, the thick tin of high silver is put into crystallizer, to one section (scolding tin exit end) crystallographic axis of liquid level covering, be 1-1.5 liter/min with the speed setting of fireless cooker feed liquor, beginning at opening for feed to even water spray between the scolding tin discharge gate;
2, electric heating crystallizer water spray crystallization operation
Regulate crystallizer speed adjustment to 2.5 and turn/min, the feed liquor speed setting is 1-1.5 liter/min, and injection flow rate is the 2-10% (weight ratio) of feed liquor amount.When beginning crystal tin to four sections, it is one section with each section temperature regulation: 210-260 ℃, two sections: 380-520 ℃, three sections: 440-560 ℃, four sections: 550-780 ℃, feed liquor amount, injection flow rate are constant, 20-40min discharges a scolding tin, after 6.5 hours, and four sections product tin that go out leaded 0.023%, argentiferous 92g/t reaches the refined tin standard.Continue crystallization operation, after 40 hours, crystallization operation is finished, and moves back groove, and common property goes out finished product tin: 24.652t, scolding tin: 8.018t, the scolding tin composition sees Table 5.
Table 5 scolding tin composition
3, refined tin founding
Pour the product tin that crystallizer produces into refined tin founding pot, heat up and melt to 300 ° of C of temperature, start stirrer 10min, drag for clean oxidation sludge, tin liquor is put into the moulding of tin ingot casting.Produce refined tin 23.912t, the refined tin composition sees Table 6.
Table 6 refined tin composition
Claims (1)
1. method from the silver-colored tin refinement tin of height, present method is with the thick tin of high silver by solder pot copper removal, iron, arsenic, antimony, by heightening electric heating crystallizer temperature, reach the fusing point zone of lead, tin, silver alloys, uninterruptedly carrying out of lead, tin, silver alloys crystallization, liquate, it is characterized in that, specifically may further comprise the steps:
1), the electric heating crystallizer heats up
Crystallizer speed adjustment to 1.5 turns/min, open one, two, three, four section, be warming up to one section behind the 30-90min: 190-220 ℃, two sections: 350-450 ℃, three sections: 400-500 ℃, four sections: 450-550 ℃, to pump into fireless cooker except the thick tin of high silver of Fe, As, Sb, Cu from solder pot, and put into crystallizer from fireless cooker, after one section of extremely thick tin liquor face covering scolding tin exit end screw shaft, be 1-4 liter/min with the speed setting of fireless cooker feed liquor, beginning at opening for feed to even water spray between the scolding tin discharge gate;
2), electric heating crystallizer water spray crystallization
The crystallizer speed adjustment turns/min to 1.5-5.0, the feed liquor speed setting is 1-4 liter/min, injection flow rate is the weight 2-10% of feed liquor amount, when beginning crystal to four sections, it is one section with each section temperature regulation: 190-260 ℃, two sections: 350-500 ℃, three sections: 400-650 ℃, four sections: 450-800 ℃, feed liquor amount, injection flow rate are constant, regular discharge scolding tin, after 4-8 hour, four sections product tin that go out are leaded less than 0.03%, argentiferous 10-200g/t, reach the refined tin standard, pour refined tin founding pot into, scolding tin send electrolytic recovery gold and silver precious metal;
3), refined tin founding
Pour the product tin that crystallizer produces into refined tin founding pot, heat up and melt to temperature 280-320 ℃, start stirrer 10-20min, drag for clean oxidation sludge, tin liquor is put into the moulding of tin ingot casting.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201210041041 CN102534249B (en) | 2012-02-22 | 2012-02-22 | Method for refining tin from high-silver crude tin |
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| CN 201210041041 CN102534249B (en) | 2012-02-22 | 2012-02-22 | Method for refining tin from high-silver crude tin |
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| CN102534249B true CN102534249B (en) | 2013-03-06 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105970003A (en) * | 2016-07-13 | 2016-09-28 | 来宾华锡冶炼有限公司 | Device and method for gathering silver metal from rough soldering tin |
| CN109923225B (en) | 2016-09-27 | 2021-08-10 | 梅塔洛比利时公司 | Improved solder and method for producing high-purity lead |
| CA3055263A1 (en) | 2017-04-10 | 2018-10-18 | Metallo Belgium | Improved process for the production of crude solder |
| PE20212094A1 (en) | 2019-01-30 | 2021-11-04 | Metallo Belgium | ENHANCED TIN PRODUCTION |
| BE1027002B1 (en) | 2019-01-30 | 2020-08-28 | Metallo Belgium | Improved process for producing high purity lead |
| CN109930012A (en) * | 2019-03-21 | 2019-06-25 | 红河绿地环保科技发展有限公司 | A kind of multi-point automatic water jetting tin refining crystallization apparatus |
| CN115029554A (en) * | 2022-02-17 | 2022-09-09 | 昆明理工大学 | Method for recovering silver from waste circuit board solder |
| CN114833490B (en) * | 2022-06-02 | 2024-04-05 | 云南锡业集团（控股）有限责任公司研发中心 | Method for improving oxidation resistance of tin raw material or tin-based solder |
| CN115369262B (en) * | 2022-09-20 | 2023-08-01 | 云南锡业股份有限公司锡业分公司 | Green and efficient refining method for complex crude tin |
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| CN101705372B (en) * | 2009-11-25 | 2011-09-21 | 郴州市金贵银业股份有限公司 | Process for extracting tin from wet lead with high tin content |
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