CN107034365A - A kind of method of thick tin pyro-refining - Google Patents
A kind of method of thick tin pyro-refining Download PDFInfo
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- CN107034365A CN107034365A CN201710425565.8A CN201710425565A CN107034365A CN 107034365 A CN107034365 A CN 107034365A CN 201710425565 A CN201710425565 A CN 201710425565A CN 107034365 A CN107034365 A CN 107034365A
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- tin
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- filter residue
- mixed liquor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/08—Refining
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/02—Obtaining tin by dry processes
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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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- Manufacturing & Machinery (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Filtering Materials (AREA)
Abstract
The present invention discloses a kind of method of thick tin purification, including following operating procedure：（1）The thick tin product of drying obtained after thick refining, is put into mixed liquor, the temperature of mixed liquor is risen into 70 90 DEG C, after being incubated 23 hours, filter to obtain filter residue；（2）Filter residue is cleaned with water, dries, then filter residue is crushed to after 100 150 mesh, aluminium borate, nano zine oxide are added thereto, after being mixed evenly, the temperature of mixture is risen to 500 550 DEG C, after being incubated 35 hours, the material of molten condition is collected；（3）By step（2）After the material cooling of middle molten, it is crushed to after 100 150 mesh, the temperature of mixture is risen to after 245 260 DEG C, after being incubated 46 hours, collects the pure tin of molten condition.The tin refinement method that the present invention is provided, operating method is simple, and the energy of consumption is low, in obtained pure tin, and the purity of tin is high, and the rate of recovery of tin is high, greatly improves the quality of pure tin.
Description
Technical field
The invention belongs to tin refinement field, and in particular to a kind of method of thick tin pyro-refining.
Background technology
Tin is a kind of argenteous metal, and its fusing point is low, plasticity is good, corrosion-resistant, antifatigue, nontoxicity.Tin and copper
Alloy is exactly bronze, and its fusing point is low compared with fine copper, and casting character is better than fine copper, and hardness is also bigger than fine copper.So they are one by people
Class is found, is just widely applied quickly, and has write extremely brilliant one page on history of human civilization, and this is " bronze ware
Epoch ".Tin is for manufacture tinplate（Tin plate）Based on, account for the 40% of consumption figure.Solder can also be made and various
Alloy such as bronze, brass.The tin plating and various sn-containing compounds of generation.Reduction melting is to produce one of main method of tin, it
Using Tin concentrate more than medium grade as raw material.Mainly by refining pre-treatment, reduction melting, clinker melting, and tin refinement etc.
Composition.At present, it will be contention future-oriented strategy money that resource regeneration and recovery, particularly resource reclaim waste containing noble metals, which are reclaimed,
The important channel in source, metallic tin is reclaimed from waste and old indium stannum alloy, it has also become an important sources of metallic tin.At present, use
The method of reduction, the obtained thick tin product from waste material, still containing more foreign metal, due in the prior art, thick
The refining stage of tin, technology is not very ripe, is caused in obtained pure tin, the content of tin is only 96% or so, and refining process
In, substantial amounts of tin raw material is wasted, the rate of recovery of refining stage tin is only 95% or so.
The content of the invention
In order to lift the content of tin and the rate of recovery of lifting tin in pure tin, the present invention provides a kind of side of thick tin pyro-refining
Method.
The present invention is achieved by the following technical solutions.
A kind of method of thick tin pyro-refining, including following operating procedure：
（1）The thick tin product of drying that will be obtained after thick refining, is put into mixed liquor, and the temperature of mixed liquor is risen into 70-90 DEG C, insulation
After 2-3 hours, filter residue is filtered to obtain, wherein mixed liquor is made up of the component of following parts by weight：11-16 parts of methylpropene sodium sulfonate,
4-7 parts of sodium hexafluoro phosphate, 6-8 parts of hydroxyl phosphonoacetic acid, 190-210 parts of water；
（2）Filter residue is cleaned with water, dries, then filter residue is crushed to after 100-150 mesh, aluminium borate, nanometer are added thereto
Zinc oxide, after being mixed evenly, 500-550 DEG C is risen to by the temperature of mixture, after being incubated 3-5 hours, collects molten condition
Material；
（3）By step（2）After the material cooling of middle molten, it is crushed to after 100-150 mesh, the temperature of mixture is risen into 245-
After 260 DEG C, after being incubated 4-6 hours, the pure tin of molten condition is collected.
Specifically, above-mentioned steps（1）The mass volume ratio of the middle thick tin product of drying and mixed liquor is 1:18-22.
Specifically, above-mentioned steps（2）Middle filter residue, aluminium borate, the mass ratio of nano zine oxide are 60-70:1:3.
Technical scheme more than, the beneficial effects of the invention are as follows：
The tin refinement method that the present invention is provided, operating method is simple, and the energy of consumption is low, in obtained pure tin, the purity of tin
Height, and the rate of recovery of tin is high, greatly improves the quality of pure tin.The mixed liquor that the present invention is provided, can effectively be removed thick
The relatively low halogen salts substances of some fusing points in tin, and may be such that the porosity of thick tin product is bigger, it is easy to follow-up powder
Broken operation, and may be such that the tin in thick tin is easier to separate out in melting, improve the rate of recovery of tin；It is aluminium borate, nano oxidized
The addition of zinc, can effectively lift the melting effect of thick tin powder, may be such that the metallics after melting is easy to higher with fusing point
Material separation, and then improve the purity of obtained product.
Embodiment
In order that those skilled in the art can be further understood that the feature and technology contents of the present invention, referring to following has
Close detailed description of the invention.
Embodiment 1
A kind of method of thick tin pyro-refining, including following operating procedure：
（1）The thick tin product of drying that will be obtained after thick refining, is put into mixed liquor, the temperature of mixed liquor is risen into 70 DEG C, insulation 2 is small
Shi Hou, filters to obtain filter residue, and wherein mixed liquor is made up of the component of following parts by weight：11 parts of methylpropene sodium sulfonate, hexafluorophosphoric acid
4 parts of sodium, 6 parts of hydroxyl phosphonoacetic acid, 190 parts of water；
（2）Filter residue is cleaned with water, dries, then filter residue is crushed to after 100 mesh, aluminium borate, nano oxidized is added thereto
Zinc, after being mixed evenly, 500 DEG C are risen to by the temperature of mixture, after being incubated 3 hours, collect the material of molten condition；
（3）By step（2）After the material cooling of middle molten, it is crushed to after 100 mesh, the temperature of mixture is risen to after 245 DEG C,
After insulation 4 hours, the pure tin of molten condition is collected.
Specifically, above-mentioned steps（1）The mass volume ratio of the middle thick tin product of drying and mixed liquor is 1:18.
Specifically, above-mentioned steps（2）Middle filter residue, aluminium borate, the mass ratio of nano zine oxide are 60:1:3.
Embodiment 2
A kind of method of thick tin pyro-refining, including following operating procedure：
（1）The thick tin product of drying that will be obtained after thick refining, is put into mixed liquor, and the temperature of mixed liquor is risen into 80 DEG C, insulation 2.5
After hour, filter residue is filtered to obtain, wherein mixed liquor is made up of the component of following parts by weight：13 parts of methylpropene sodium sulfonate, hexafluoro phosphorus
Sour 5 parts of sodium, 7 parts of hydroxyl phosphonoacetic acid, 200 parts of water；
（2）Filter residue is cleaned with water, dries, then filter residue is crushed to after 130 mesh, aluminium borate, nano oxidized is added thereto
Zinc, after being mixed evenly, 530 DEG C are risen to by the temperature of mixture, after being incubated 4 hours, collect the material of molten condition；
（3）By step（2）After the material cooling of middle molten, it is crushed to after 130 mesh, the temperature of mixture is risen to after 250 DEG C,
After insulation 5 hours, the pure tin of molten condition is collected.
Specifically, above-mentioned steps（1）The mass volume ratio of the middle thick tin product of drying and mixed liquor is 1:20.
Specifically, above-mentioned steps（2）Middle filter residue, aluminium borate, the mass ratio of nano zine oxide are 65:1:3.
Embodiment 3
A kind of method of thick tin pyro-refining, including following operating procedure：
（1）The thick tin product of drying that will be obtained after thick refining, is put into mixed liquor, the temperature of mixed liquor is risen into 90 DEG C, insulation 3 is small
Shi Hou, filters to obtain filter residue, and wherein mixed liquor is made up of the component of following parts by weight：16 parts of methylpropene sodium sulfonate, hexafluorophosphoric acid
7 parts of sodium, 8 parts of hydroxyl phosphonoacetic acid, 210 parts of water；
（2）Filter residue is cleaned with water, dries, then filter residue is crushed to after 150 mesh, aluminium borate, nano oxidized is added thereto
Zinc, after being mixed evenly, 550 DEG C are risen to by the temperature of mixture, after being incubated 5 hours, collect the material of molten condition；
（3）By step（2）After the material cooling of middle molten, it is crushed to after 150 mesh, the temperature of mixture is risen to after 260 DEG C,
After insulation 6 hours, the pure tin of molten condition is collected.
Specifically, above-mentioned steps（1）The mass volume ratio of the middle thick tin product of drying and mixed liquor is 1:22.
Specifically, above-mentioned steps（2）Middle filter residue, aluminium borate, the mass ratio of nano zine oxide are 70:1:3.
Comparative example 1
Step（1）In mixed liquor be clear water, remaining step is identical with embodiment 1.
Comparative example 2
Step（2）In without aluminium borate, nano zine oxide, remaining step is identical with embodiment 2.
Respectively with the method in each embodiment and comparative example to being purified with batch of thick tin product, wherein each in thick tin
The quality composition of impurity is as shown in the table：
The thick tin of table 1 is constituted
| Component | Sn | Pb | Cu | Fe | Zn | As | Other |
| Composition/% | 79.5 | 6.8 | 5.1 | 3.7 | 0.3 | 0.1 | 4.5 |
The refining effect of each embodiment and comparative example is as shown in table 2：
A kind of method compliance test result of thick tin pyro-refining of table 2
| Project | Theil indices/% | The rate of recovery/% of tin |
| Embodiment 1 | 99.1 | 98.1 |
| Comparative example 1 | 98.4 | 96.0 |
| Embodiment 2 | 99.5 | 98.3 |
| Comparative example 2 | 97.2 | 96.9 |
| Embodiment 3 | 99.7 | 98.4 |
As shown in Table 2, the method that the present invention is provided, the rate of recovery and obtained pure tin of tin when greatly improving thick tin purification
The purity of product.
The present invention can have various modifications and variations.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (3)
1. a kind of method of thick tin pyro-refining, it is characterised in that including following operating procedure：
（1）The thick tin product of drying that will be obtained after thick refining, is put into mixed liquor, and the temperature of mixed liquor is risen into 70-90 DEG C, insulation
After 2-3 hours, filter residue is filtered to obtain, wherein mixed liquor is made up of the component of following parts by weight：11-16 parts of methylpropene sodium sulfonate,
4-7 parts of sodium hexafluoro phosphate, 6-8 parts of hydroxyl phosphonoacetic acid, 190-210 parts of water；
（2）Filter residue is cleaned with water, dries, then filter residue is crushed to after 100-150 mesh, aluminium borate, nanometer are added thereto
Zinc oxide, after being mixed evenly, 500-550 DEG C is risen to by the temperature of mixture, after being incubated 3-5 hours, collects molten condition
Material；
（3）By step（2）After the material cooling of middle molten, it is crushed to after 100-150 mesh, the temperature of mixture is risen into 245-
After 260 DEG C, after being incubated 4-6 hours, the pure tin of molten condition is collected.
2. a kind of method of thick tin pyro-refining according to claim 1, it is characterised in that step（1）Dry thick tin
The mass volume ratio of product and mixed liquor is 1:18-22.
3. a kind of method of thick tin pyro-refining according to claim 1, it is characterised in that step（2）Middle filter residue, boron
Sour aluminium, the mass ratio of nano zine oxide are 60-70:1:3.
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| CN201710425565.8A CN107034365B (en) | 2017-06-08 | 2017-06-08 | A kind of method of thick tin pyro-refining |
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| CN201710425565.8A CN107034365B (en) | 2017-06-08 | 2017-06-08 | A kind of method of thick tin pyro-refining |
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| CN107034365A true CN107034365A (en) | 2017-08-11 |
| CN107034365B CN107034365B (en) | 2019-03-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176188A (en) * | 2020-08-27 | 2021-01-05 | 广东省科学院稀有金属研究所 | Method for deeply removing antimony and copper impurities in regenerated crude tin |
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| JPS5040103B1 (en) * | 1969-10-08 | 1975-12-22 | ||
| GB2109008A (en) * | 1981-10-07 | 1983-05-25 | Capper Pass Limited | Refining non-ferrous alloys |
| SU611538A1 (en) * | 1977-03-09 | 1992-10-07 | Новосибирский оловянный комбинат | Method of refining tin from lead and aluminum |
| JP2004307885A (en) * | 2003-04-03 | 2004-11-04 | Dowa Mining Co Ltd | Method for reducing impurity in metal |
| CN101886182A (en) * | 2009-05-15 | 2010-11-17 | 理翰应用科技有限公司 | Synthesized chemical powder capable of purifying tin melt liquid and application fixture and using method thereof |
| CN102102154A (en) * | 2010-12-22 | 2011-06-22 | 中南大学 | Low-temperature fused salt clean smelting method for tin |
| CN102851514A (en) * | 2012-10-08 | 2013-01-02 | 来宾华锡冶炼有限公司 | Treatment method of coarse tin decoppered slag |
| CN102876903A (en) * | 2012-10-08 | 2013-01-16 | 来宾华锡冶炼有限公司 | Direct acidity oxygen pressure leaching treatment method of crude tin copper removal residues |
| CN104651625A (en) * | 2015-02-05 | 2015-05-27 | 昆明理工大学 | Method for removing antimony-lead-arsenic from antimony-containing crude tin alloy by vacuum distillation |
| CN106544518A (en) * | 2016-12-13 | 2017-03-29 | 云南锡业股份有限公司冶炼分公司 | A kind of method for preparing pure tin with the thick stannum of electrolysis |
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2017
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Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5040103B1 (en) * | 1969-10-08 | 1975-12-22 | ||
| SU611538A1 (en) * | 1977-03-09 | 1992-10-07 | Новосибирский оловянный комбинат | Method of refining tin from lead and aluminum |
| GB2109008A (en) * | 1981-10-07 | 1983-05-25 | Capper Pass Limited | Refining non-ferrous alloys |
| JP2004307885A (en) * | 2003-04-03 | 2004-11-04 | Dowa Mining Co Ltd | Method for reducing impurity in metal |
| CN101886182A (en) * | 2009-05-15 | 2010-11-17 | 理翰应用科技有限公司 | Synthesized chemical powder capable of purifying tin melt liquid and application fixture and using method thereof |
| CN102102154A (en) * | 2010-12-22 | 2011-06-22 | 中南大学 | Low-temperature fused salt clean smelting method for tin |
| CN102851514A (en) * | 2012-10-08 | 2013-01-02 | 来宾华锡冶炼有限公司 | Treatment method of coarse tin decoppered slag |
| CN102876903A (en) * | 2012-10-08 | 2013-01-16 | 来宾华锡冶炼有限公司 | Direct acidity oxygen pressure leaching treatment method of crude tin copper removal residues |
| CN104651625A (en) * | 2015-02-05 | 2015-05-27 | 昆明理工大学 | Method for removing antimony-lead-arsenic from antimony-containing crude tin alloy by vacuum distillation |
| CN106544518A (en) * | 2016-12-13 | 2017-03-29 | 云南锡业股份有限公司冶炼分公司 | A kind of method for preparing pure tin with the thick stannum of electrolysis |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176188A (en) * | 2020-08-27 | 2021-01-05 | 广东省科学院稀有金属研究所 | Method for deeply removing antimony and copper impurities in regenerated crude tin |
| CN112176188B (en) * | 2020-08-27 | 2022-03-25 | 广东省科学院稀有金属研究所 | Method for deeply removing antimony and copper impurities in regenerated crude tin |
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| CN107034365B (en) | 2019-03-15 |
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