CN103667744A - Production method of grade tin containing 99.99% of Sn - Google Patents
Production method of grade tin containing 99.99% of Sn Download PDFInfo
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Abstract
A production method of grade tin containing 99.99% of Sn comprises steps as follows: the grade tin containing 99.99% of Sn is added into helical blade crystallization equipment with six temperature control sections, and the temperature and the temperature gradient are controlled, so that a material can be continuously and repeatedly crystallized and smelt, and a tin alloy rich in arsenic, copper, ferrum, silicon, aluminum, magnesium, nickel, thallium and sulfur elements is produced at a high-temperature section outlet of the crystallization equipment; and then, the temperature and the temperature gradient of the inside of the crystallization equipment are changed, so that the material can be continuously crystallized and smelt, a tin alloy rich in silver, tin, lead, bismuth, cadmium and zinc elements is produced at a low-temperature section outlet of the equipment, and the grade tin containing 99.99% of Sn is obtained at the high-temperature section outlet of the crystallization equipment.
Description
Technical field
The present invention relates to the high-grade products production of non-ferrous metal field, particularly a kind of production method containing Sn99.99% grade tin.
Background technology
Containing Sn99.99% grade tin, also claim four or nine tin, 4N tin or high-quality tin, main composition Sn >=99.990%, major impurity composition Fe≤0.0025%, Cu≤0.001%, Pb≤0.0035%, Sb≤0.0020%, As≤0.0007%, Bi≤0.0025%, S≤0.0005%, Ag≤0.0005%, In≤0.0025%.
Containing Sn99.99% grade tin, mainly for the preparation of high-grade lead-free solder, be also widely used in making semiconductor compound and the superconductor alloies such as nitrogenize tin, antimony tin, arsenic tin, as fluor and high-grade ITO target raw material, semiconductor dopant, semi-conductor outlet line etc.
At present, the production method containing Sn99.99% grade tin mainly contains following four kinds:
1, electrolytic process.It is mainly to utilize tin metal and other foreign metal to exist potential difference that electrolytic process is purified, the foreign metal of current potential corrigendum is deposited in the anode sludge, the more negative foreign metal of current potential is deposited in solution, only have tin metal to enter solution from anode and from solution, precipitate into again negative plate, thereby reach the metallic tin object separated with foreign metal.The method is first cast into anode by raw material 99.9% grade tin, then in solvable tin ion solution, carries out electrolysis, and what on negative electrode, obtain is the tin metal that purity is higher.The method can guarantee product purity, and tin smelting recovery is high, but complex process, productivity is low, the production cycle is long, and current assets takies greatly, and production cost is high.
2, zone melting method.The difference of the solubleness of utilizing metallic tin and impurity under differing temps, metal is carried out to multiple bearing heat fused and directed crystallisation by cooling, make impurity finally be enriched in the two ends of metal alloy body, interlude is purified, after interlude is separated with two ends, obtain high pure metal.The method obtains high-quality tin, good product quality, and technological process is simple.Its shortcoming is that product yield is low, conventionally only has 50%, and plant efficiency is very low, and single device output every day is 0.1 kilogram of left and right, cannot carry out industrial-scale production.
3, vacuum distillation method.Under vacuum condition, utilize the boiling-point difference of metallic tin and other element, make low-boiling metallic element volatilization gas phase, the non-volatile liquid phase that is deposited in of metallic element that boiling point is high, thus reach separated object.The method can efficiently be sloughed lower boiling metal, and as zinc, cadmium, thallium, arsenic, lead etc., and production efficiency is high, and the treatment capacity of every day can reach more than 1 ton.But the method can not remove the metal that boiling point is high, as indium, iron, copper, nickel, silver cannot remove, therefore, the method is produced the quality product obtaining cannot reach requirement.
4, pyrogenic process degree of depth refining.The technological process of the method is identical with traditional thick tin fire refining process, by the grade tin containing Sn99.9%, then re-starts pyrorefining; But in removing each impurity process, removing impurities reagent add coefficient of excess very large, and the temperature of removing impurities process control very strict, during as decopper(ing), the superfluous system of sulphur reaches 200%, during dearsenification antimony, the superfluous system of aluminium flake reaches 250%, and while making high alumina slag and low aluminium slag, front and back temperature fluctuation must be controlled in 20 ℃, otherwise can cause the remelt of antimony and exceed standard, crystallization is when separation of lead, bismuth, silver, and input speed and speed of screw shaft are for producing 50% left and right containing Sn99.9% grade tin.When the method is produced containing Sn99.99% grade tin, have advantages of and do not need to increase any production facility, its shortcoming is that technical qualification are controlled requirement strictly, and impurity removal reagents consumption is large, and equipment capacity seriously reduces, and the process quantity of slag of output is large, and smelting recovery is low.
Summary of the invention
The object of this invention is to provide a kind of production method containing Sn99.99% grade tin, the method technical process is short, only need a main equipment just can output contain Sn99.99% grade tin, production efficiency is high, equipment capacity reaches more than 1 ton/day, first product rate is up to 50%, and production process clean environment firendly, does not have three wastes output.
The present invention is achieved through the following technical solutions above-mentioned purpose: a kind of production method containing Sn99.99% grade tin, comprises the steps:
(1), peritectic or metallic compound removing impurities: will be containing Sn99.9% grade tin, in temperature, be under 250~300 ℃ of conditions, quantitatively join in the screw-blade crystallizer that is provided with 6 temperature control sections, and the temperature of interior 6 temperature sections of crystallization control equipment is 180~195 ℃ respectively, 195~205 ℃, 205~215 ℃, 215~225 ℃, 225~235 ℃, 235~240 ℃, material passes through continuously periodic crystallisation and fusing in crystallizer, after 12~20 hours, in crystallizer high temperature section, export, output enrichment arsenic, copper, iron, silicon, aluminium, magnesium, nickel, thallium, the tin alloy that element sulphur is higher,
(2), eutectic alloy removing impurities: by the temperature change in crystallizer, in crystallization control equipment, the temperature of 6 temperature sections is 210~215 ℃, 215~220 ℃, 220~225 ℃, 225~230 ℃, 230~233 ℃, 233~235 ℃ respectively, after 6~8 hours, in crystallizer low-temperature zone, export, output enrichment silver, tin, lead, bismuth, cadmium, eutectic alloy that zinc element is higher, meanwhile, in the outlet of crystallizer high temperature section, obtain containing Sn99.99% grade tin.
Peritectic of the present invention or metallic compound removing impurities process and eutectic alloy removing impurities process are to complete in same screw-blade crystallizer, and directly output contains Sn99.99% grade tin.
Unless otherwise indicated, per-cent of the present invention is mass percent, and each component concentration percentage ratio sum is 100%.
Outstanding advantages of the present invention is:
Adopt the present invention to there is technical process short, in a screw-blade crystallizer, by temperature and the thermograde of operating device, directly output is containing Sn99.99% grade tin, and production efficiency is high, and equipment capacity reaches more than 1 ton/day, first product rate qualification rate reaches 50%, there is not chemical reaction in production process, not output waste residue, waste gas and waste water, clean environment firendly.
When be liquid state containing Sn99.9% grade tin, quantitatively join in the screw-blade crystallizer that is provided with 6 temperature control sections, tin metal alloy is subject to the temperature controllable heater heats under cell body simultaneously and heat up fusing and cell body dispel the heat and decrease temperature crystalline, and under the promotion of the screw-blade in crystallization cell body, constantly repeat fusing and crystallization, and fusing and crystallisation process are constantly mutually alternately, in crystallizer, to control be respectively 180~195 ℃ to the temperature of 6 temperature sections, 195~205 ℃, 205~215 ℃, 215~225 ℃, 225~235 ℃, in the time of 235~240 ℃, material is by after periodic crystallisation continuously and fusing, arsenic, copper, iron, silicon, aluminium, magnesium, nickel, thallium, the elements such as sulphur and tin metal form peritectic or metallic compound, and peritectic or metallic compound fusing point, higher than metallic tin, are enriched in the outlet of crystallizer high temperature section, along with the promotion of screw-blade, enrichment arsenic, copper, iron, silicon, aluminium, magnesium, nickel, thallium, the peritectic of element sulphur or metallic compound constantly, from separated in cell body, finally reach main metallic tin and arsenic, copper, iron, silicon, aluminium, magnesium, nickel, thallium, sulphur content from object.
Work as arsenic impurities, copper, iron, silicon, aluminium, magnesium, nickel, thallium, after sulphur is separated with tin, change temperature and thermograde in screw-blade crystallizer, the material in equipment will re-establish the another kind of homeostasis process mutually replacing with crystallization that melts, by the temperature of 6 temperature sections in crystallizer, it is 210~215 ℃, 215~220 ℃, 220~225 ℃, 225~230 ℃, 230~233 ℃, 233~235 ℃, material is by after periodic crystallisation continuously and fusing, silver, indium, plumbous, bismuth, cadmium, zinc element and tin metal form eutectic alloy, the fusing point of eutectic alloy is lower than metallic tin, with molten state, be enriched in the outlet of screw-blade crystallizer low-temperature zone, regularly by enrichment silver, indium, plumbous, bismuth, cadmium, outside the low melting point eutectic tin alloy discharge channel of zinc element, reach main metallic tin and impurity silver, indium, plumbous, bismuth, cadmium, the object of zinc separation, meanwhile, in the outlet of screw-blade crystallizer high temperature section, obtain containing Sn99.99% grade tin product.
Adopt present method to produce containing Sn99.99% grade tin, only need a main equipment, i.e. a screw-blade crystallizer, by temperature and the thermograde of operating device, can one time output qualified containing Sn99.99% grade tin product, technological process is simple.Meanwhile, in process of producing product, temperature is below 250 ℃, and whole technological process is the physical process of crystallization and fusing, do not add any removing impurities reagent, chemical reaction does not occur, material remains metallic state in crystallizer, therefore, the quantity of slag of process output is very little, and metal recovery rate is high, and field condition is good, energy-output ratio is little, and production cost is low.In addition, because chemical reaction does not occur process, first product rate is up to 50%.
Screw-blade crystallizer, by outer cell body, interior cell body, screw shaft, blade, rotating mechanism, temperature controlling system, formed, interior cell body size can reach Φ 680mm * 6400mm, each cycle is processed containing Sn99.9% grade tin amount for approximately 24 hours can reach 12 tons, and every day output containing 6 tons, Sn99.99% grade tin, equipment can meet industrialized mass production requirement.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the production method containing Sn99.99% grade tin of the present invention.
Fig. 2 is the structural front view of screw-blade crystallizer of the present invention.
Fig. 3 is the structure vertical view of screw-blade crystallizer of the present invention.
In figure, be labeled as: cell body, 6-screw shaft, 7-blade, the outlet of 8-low-temperature zone in 1-motor, 2-speed regulator, the outlet of 3-high temperature section, 4-temperature controllable well heater, 5-equipment.
Embodiment
By drawings and Examples, technical scheme of the present invention is described further below.
Embodiment 1
The present embodiment is the first example of the production method containing Sn99.99% grade tin of the present invention, comprises the steps:
(1), peritectic or metallic compound removing impurities: in temperature, be under 250 ℃ of conditions, progressively by 1 ton, contain Sn99.92%, Fe0.005%, Cu0.0032%, Pb0.018%, Sb0.017%, As0.004%, Bi0.011%, S0.003%, Ag0.0005%, the Sn99.9% grade tin of In0.018% joins the interior cell body size Φ 280mm * 2000mm of equipment and is provided with in the screw-blade crystallizer of 6 temperature control sections, the temperature of 6 temperature sections of crystallization control equipment is 180 ℃ respectively simultaneously, 195 ℃, 205 ℃, 215 ℃, 225 ℃, 235 ℃, helical-blade bobbin rotating speed is 0.4n/min, make material in crystallizer, realize continuously crystallization and fusing, after 12 hours, in crystallizer high temperature section, export, output is containing Sn99.73%, Fe0.015%, Cu0.010%, Pb0.021%, Sb0.051%, As0.012%, Bi0.019%, S0.009%, Ag0.0006%, 0.3 ton of the tin alloy of In0.0005%, returning to thick tin pyrorefining operation produces containing Sn99.9% grade tin,
(2), eutectic alloy removing impurities: by the temperature change in crystallizer, in crystallization control equipment, the temperature of 6 temperature sections is 210 ℃ respectively, 215 ℃, 220 ℃, 225 ℃, 230 ℃, 233 ℃, speed of screw shaft is 0.4n/min, after 6 hours, in crystallizer low-temperature zone, export, with liquid molten bodily form formula output, contain Sn99.85%, Fe0.0009%, Cu0.0001%, Pb0.082%, Sb0.0011%, As0.0003%, Bi0.045%, S0.0009%, Ag0.0018%, 0.2 ton of the eutectic alloy of In0.004%, eutectic alloy returns to pyrorefining operation and produces containing Sn99.9% grade tin, in crystallizer high temperature section, export, obtain the tin product containing Sn99.996%, Fe0.0014%, Cu0.0003%, Pb0.0018%, Sb0.0017%, As0.0004%, Bi0.0016%, S0.0003%, Ag0.0002%, In0.0014%, reach the specification of quality containing Sn99.99% grade tin.
The present embodiment is the second example of the production method containing Sn99.99% grade tin of the present invention, comprises the steps:
(1), peritectic or metallic compound removing impurities: in temperature, be under 270 ℃ of conditions, progressively by 9 tons, contain Sn99.93%, Fe0.006%, Cu0.0035%, Pb0.019%, Sb0.016%, As0.003%, Bi0.012%, S0.003%, Ag0.0005%, the Sn99.9% grade tin of In0.0016% joins the interior cell body size Φ 650mm * 6000mm of equipment and is provided with in the screw-blade crystallizer of 6 temperature control sections, the temperature of 6 temperature sections of crystallization control equipment is 190 ℃ respectively simultaneously, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 238 ℃, helical-blade bobbin rotating speed is 0.35n/min, make material in crystallizer, realize continuously crystallization and fusing, after 16 hours, in crystallizer high temperature section, export, continuous output Sn99.76%, Fe0.017%, Cu0.011%, Pb0.003%, Sb0.056%, As0.013%, Bi0.002%, S0.008%, Ag0.0001%, 2.5 tons of the tin alloys of In0.0002%, returning to thick tin pyrorefining operation produces containing Sn99.9% grade tin,
(2), eutectic alloy removing impurities: by the temperature change in crystallizer, in crystallization control equipment, the temperature of 6 temperature sections is 213 ℃ respectively, 218 ℃, 223 ℃, 228 ℃, 232 ℃, 234 ℃, speed of screw shaft is 0.35n/min, after 7 hours, in crystallizer low-temperature zone, export, with liquid molten bodily form formula output, contain Sn99.89%, Fe0.0007%, Cu0.0005%, Pb0.093%, Sb0.0006%, As0.0003%, Bi0.056%, S0.0001%, Ag0.0021%, 2.0 tons of the eutectic alloys of In0.0034%, eutectic alloy returns to pyrorefining operation and produces containing Sn99.9% grade tin, in crystallizer high temperature section, export, obtain, containing 4.5 tons of the products of Sn99.994%, Fe0.0011%, Cu0.0006%, Pb0.0015%, Sb0.0012%, As0.0005%, Bi0.0013%, S0.0002%, Ag0.0003%, In0.0012%, reaching the specification of quality containing Sn99.99% grade tin.
The present embodiment is the 3rd example of the production method containing Sn99.99% grade tin of the present invention, comprises the steps:
(1), peritectic or metallic compound removing impurities: in temperature, be under 300 ℃ of conditions, progressively by 12 tons, contain Sn99.96%, Fe0.004%, Cu0.002%, Pb0.010%, Sb0.010%, As0.002%, Bi0.008%, S0.002%, Ag0.0002%, the Sn99.9% grade tin of In0.0018% joins the interior cell body size Φ 680mm * 6400mm of equipment and is provided with in the screw-blade crystallizer of 6 temperature control sections, and the temperature of 6 temperature sections of crystallization control equipment is 195 ℃ respectively simultaneously, 205 ℃, 215 ℃, 225 ℃, 235 ℃, 240 ℃, helical-blade bobbin rotating speed is 0.3n/min, makes material in crystallizer, realize continuously crystallization and fusing, and after 20 hours, in the outlet of crystallizer high temperature section, output is containing Sn99.88% continuously, Fe0.010%, Cu0.046%, Pb0.002%, Sb0.025%, As0.005%, Bi0.002%, S0.005%, Ag0.0001%, 3.4 tons of the tin alloys of In0.0003%, return to thick tin pyrorefining operation and produce containing Sn99.9% grade tin,
(2), eutectic alloy removing impurities: by the temperature change in crystallizer, in crystallization control equipment, the temperature of 6 temperature sections is 215 ℃ respectively, 220 ℃, 225 ℃, 230 ℃, 233 ℃, 235 ℃, speed of screw shaft is 0.3n/min, after 8 hours, in crystallizer low-temperature zone, export, with liquid molten bodily form formula output, contain Sn99.91%, Fe0.0012%, Cu0.0003%, Pb0.04%, Sb0.0009%, As0.0002%, Bi0.036%, S0.0002%, Ag0.0016%, 2.6 tons of the eutectic alloys of In0.0023%, eutectic alloy returns to pyrorefining operation and produces containing Sn99.9% grade tin, in crystallizer high temperature section, export, obtain, containing 6 tons of the products of Sn99.993%, Fe0.0017%, Cu0.0005%, Pb0.0011%, Sb0.0016%, As0.0004%, Bi0.0015%, S0.0004%, Ag0.0004%, In0.0016%, reaching the specification of quality containing Sn99.99% grade tin.
Claims (3)
1. containing a production method for Sn99.99% grade tin, it is characterized in that, comprise the steps:
(1), peritectic or metallic compound removing impurities: will be containing Sn99.9% grade tin, in temperature, be under 250~300 ℃ of conditions, quantitatively join in the screw-blade crystallizer that is provided with 6 temperature control sections, and the temperature of interior 6 temperature sections of crystallization control equipment is 180~195 ℃ respectively, 195~205 ℃, 205~215 ℃, 215~225 ℃, 225~235 ℃, 235~240 ℃, material passes through continuously periodic crystallisation and fusing in crystallizer, after 12~20 hours, in crystallizer high temperature section, export, output enrichment arsenic, copper, iron, silicon, aluminium, magnesium, nickel, thallium, the tin alloy of element sulphur,
(2), eutectic alloy removing impurities: by the temperature change in crystallizer, in crystallization control equipment, the temperature of 6 temperature sections is 210~215 ℃, 215~220 ℃, 220~225 ℃, 225~230 ℃, 230~233 ℃, 233~235 ℃ respectively, after 6~8 hours, in crystallizer low-temperature zone, export, output enrichment the eutectic tin alloy of silver, tin, lead, bismuth, cadmium, zinc element, meanwhile, in the outlet of crystallizer high temperature section, obtain containing Sn99.99% grade tin.
2. the production method containing Sn99.99% grade tin according to claim 1, is characterized in that, described peritectic or metallic compound removing impurities process and eutectic alloy removing impurities process are to complete in same screw-blade crystallizer.
3. one kind is applicable to screw-blade crystallizer claimed in claim 1, it is characterized in that, comprise cell body in motor, speed regulator, high temperature section outlet, temperature controllable well heater, equipment, screw shaft, blade, low-temperature zone outlet, its structure and annexation are: the bottom of temperature controllable well heater cell body in equipment, in equipment, the bottom of cell body connects low-temperature zone outlet, in equipment, cell body top connects high temperature section outlet, screw shaft in cell body centre in equipment, blade is welded on screw shaft, the front end of screw shaft is connected with speed regulator, and the other end of speed regulator is connected with motor.
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Cited By (5)
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 |
CN107841636A (en) * | 2017-09-27 | 2018-03-27 | 昆明理工大学 | A kind of preparation method of high purity tin |
CN108277358A (en) * | 2018-03-13 | 2018-07-13 | 昆明理工大学 | A method of adding magnesium desilver in containing silver-tin alloy |
CN111172394A (en) * | 2019-09-02 | 2020-05-19 | 昆明理工大学 | Equipment and method for separating, purifying and recovering aluminum-tin alloy through vacuum continuous crystallization |
WO2020157167A2 (en) | 2019-01-30 | 2020-08-06 | Metallo Belgium | Improved tin production |
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CN85107356A (en) * | 1985-09-26 | 1986-09-03 | 云南锡业公司 | The method of tin refinement deleading, bismuth and device |
US20090098012A1 (en) * | 2005-07-01 | 2009-04-16 | Nippon Mining & Metals Co., Ltd. | High-Purity Tin or Tin Alloy and Process for Producing High-Purity Tin |
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CN85107356A (en) * | 1985-09-26 | 1986-09-03 | 云南锡业公司 | The method of tin refinement deleading, bismuth and device |
US20090098012A1 (en) * | 2005-07-01 | 2009-04-16 | Nippon Mining & Metals Co., Ltd. | High-Purity Tin or Tin Alloy and Process for Producing High-Purity Tin |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN107841636A (en) * | 2017-09-27 | 2018-03-27 | 昆明理工大学 | A kind of preparation method of high purity tin |
CN108277358A (en) * | 2018-03-13 | 2018-07-13 | 昆明理工大学 | A method of adding magnesium desilver in containing silver-tin alloy |
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 |
WO2020157167A2 (en) | 2019-01-30 | 2020-08-06 | Metallo Belgium | Improved tin production |
US11913091B2 (en) | 2019-01-30 | 2024-02-27 | Metallo Belgium | Tin production, which includes a composition comprising tin, lead, silver and antimony |
CN111172394A (en) * | 2019-09-02 | 2020-05-19 | 昆明理工大学 | Equipment and method for separating, purifying and recovering aluminum-tin alloy through vacuum continuous crystallization |
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