CN1030450A - Technology with producing high purity Sn from raw soldering tin - Google Patents
Technology with producing high purity Sn from raw soldering tin Download PDFInfo
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- CN1030450A CN1030450A CN 88101044 CN88101044A CN1030450A CN 1030450 A CN1030450 A CN 1030450A CN 88101044 CN88101044 CN 88101044 CN 88101044 A CN88101044 A CN 88101044A CN 1030450 A CN1030450 A CN 1030450A
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Abstract
The present invention is a kind of vacuum distillation furnace that utilizes, the purify new production technique of thick scolding tin of screw machine crystallizer and sulfuric acid-silicofluoric acid electrolytic solution anode electrolysis, this technical process is brief, production cost is low, the metal recovery rate height, stable and reliable product quality, with containing Sn60-70%, the thick scolding tin of Pb30-40% and other a small amount of unavoidable impurity can be produced the high purity tin that contains Sn＞=99.95%.
Description
The invention belongs to a kind of technology with producing high purity Sn from raw soldering tin.
To contain Sn60-70%, Pb30-40% and small amount of Fe, Sb, Cu, As, the thick scolding tin of unavoidable impurity element such as Bi is raw material, production contains the high purity tin of Sn＞=99.95%, generally to pass through the several times refining, removing a large amount of impurity just can accomplish, the deimpurity method of refining is known vacuum distilling, machinery crystallization deleading, bismuth, the centrifuging arsenic removal, iron adds the aluminium arsenic removal, antimony, add pyrorefining such as sulphur copper removal and stannous sulfate-sulfuric acid and (see JP59064790, JP87001478), tin protochloride-hydrochloric acid, the wet-process refining of stannous sulfate-silicofluoric acid Ya Xi-sulfuric acid-electrolytic solution anode electrolysis such as silicofluoric acid, these methods and equipment thereof are widely used in the refinery process of all kinds of tin-smelting plants, but concrete purposes operational condition is different, these methods and plant machinery thereof ground can not be combined into general refinery practice, is what to be difficult to by independent a kind of method and the purification of equipment fork-like farm tool used in ancient China thereof for resembling the such raw material of thick scolding tin, therefore, existing refining techniques of what use is made of and equipment makes it organically make up the production technique that fork-like farm tool used in ancient China forms a kind of thick scolding tin of purifying economically, with regard to the problem that has become to fail fine solution for a long time.
The objective of the invention is to propose the new thick scolding tin refinery practice that existing method of refining of a kind of usefulness and equipment thereof combine.
The technology that the present invention proposes is by vacuum distillation furnace, the screw machine crystallizer, and stannous sulfate-silicofluoric acid Ya Xi-sulfuric acid-silicofluoric acid electrolytic solution anode electrolysis and their less important work are formed, and its production process is as follows:
Remove lead with vacuum distillation furnace and screw machine crystallizer; bismuth; output contains the thick tin of Sn＞95% and contains the lead bullion of Sn＜0.3%; thick tin is cast anode block through molding machine; put into electrolytic tank electrolysis; the used negative electrode starting sheet of electrolysis operation is cast by high purity tin, and the conduction copper rod is handled through the optical wand machine, and electrolysis took out that anode cleans once in 4 days and then electrolysis 4 days; return the molding machine ingot bar after the anode scrap washing; handle to reclaim Sn wherein, Ag, Pb with chemical process behind the anode sludge washing and filtering; valuable metals such as Sb; negative electrode took out and renews cloudy starting sheet again in per 4 days, and electrolytic solution concentrates on a collecting tank enrichment earlier after flowing out from electrolyzer; add a part of electrolytic solution with stylish; pump to one header tank is pressed into electrolyzer by drop then, goes out under enterprising like this; the single-stage circulation; ambient operation, vacuum distillation furnace, the technological operation condition of screw machine crystallizer and electrolysis operation is as follows:
Vacuum distillation furnace: operating pressure 0.02-0.03 holder in the stove, working current 2700-3000 peace, operating voltage 18-20 volt, consumption of cooling-water 2-2.5 cubic meter/hour.
The screw machine crystallizer: revolution speed of screw 0.5-1.0 rev/min, 355-385 ℃ of trough temperature, (I) district temperature is 365-395 ℃ in the groove, and (II) district temperature is 209-325 ℃ in the groove, 115-145 ℃ of groove tail temperature.
Electrolysis: bath composition: Sn
+ 2The 18-35 grams per liter, Sn
+ 4＜5 grams per liters, total H
2SiF
645 grams per liters, free H
2SO
440 grams per liters, ox glue and 2-Naphthol 0.5-1.0 kilogram/electric tin of ton is with interpole gap 80-90 millimeter, bath voltage 0.3-0.5 volt, current density 50-75 peace/square metre, circulation of elecrolyte amount 20-40 liter/minute, electrolysing period: negative electrode 4 days, anode 8 days washs once electrolysis more for the second time every taking-up in 4 days.
By above-mentioned technological operation conditional operation, and according to the variation of feedstock property adjusting process parameter within the limits prescribed suitably, just can output purity greater than 99.95% high purity tin, usually, when the anode Composition Control for containing Sn＞=95%, Pb＜=4% o'clock, but output contains tin of spy of Sn＞=99.95%, when the anode Composition Control for containing Sn＞=97%, Pb＜=1% o'clock, but output contains the senior tin of Sn＞=99.99%, and the direct yield of tin is 97-99%.
Technology proposed by the invention, it is brief to have flow process, and the intermediate material that returns processing is few, and the metal trend is concentrated, the tin recovery rate height, generally can reach 97-99%, tooling cost is low, only needs 830-860 unit/electric tin of ton, not dilution of divalent tin ion in the electrolytic process, stable production process is reliable, quality product height, association valuable element advantage such as can be used preferably.
Example
Under the technical qualification of afore mentioned rules, be processed into to be divided into and contain: Sn60.46%, Pb38.86%, Sb0.127%, As0.091%, Cu0.228%, Bi0.22%, and 361.0814 tons in the thick scolding tin of Fe0.0007%, 32.1454 tons in the special tin of output, composition is for containing: Sn99.965%, As＜0.001% Fe＜0.002%, Cu＜0.002%, Pb＜0.02%, Bi＜0.005%, Sb＜0.003%, S＜0.0005%, 182.1060 tons in senior tin, its composition is: Sn99.993%, Fe＜0.001%, Pb＜0.003%, As＜0.0005%, Cu＜0.0005%, Sb＜0.001%, S＜0.0003%, Bi＜0.001%, tin recovery rate are 98.13%, and tooling cost is 839.2 yuan of/ton electric tin.
Claims (4)
1, a kind of technology with producing high purity Sn from raw soldering tin use vacuum distillation furnace, and the screw machine crystallizer takes off lead, bismuth, produce thick tin usefulness stannous sulfate-silicofluoric acid Ya Xi-sulfuric acid-silicofluoric acid electrolytic solution anode electrolysis, output contains the high purity tin of Sn＞=99.95%.
2, by the described technology of claim 1, it is characterized in that the technological operation condition of vacuum distillation furnace is: operating pressure 0.02-0.03 holder in the stove, working current 2700-3000 peace, operating voltage 18-20 volt.
3, by claim 1 or 2 described technologies, the technological operation condition that it is characterized in that the screw machine crystallizer is: revolution speed of screw 0.5-1.0 rev/min, and 355-385 ℃ of trough temperature, (I) district temperature is 365-395 ℃ in the groove, (II) district temperature is 209-325 ℃ in the groove, 115-145 ℃ of groove tail temperature.
4, by claim 1 or 2 or 3 described technologies, it is characterized in that the technological operation condition of electrolysis operation is: contain in the electrolytic solution: Sn
+ 2The 18-35 grams per liter, Sn
+ 4＜5 grams per liters, total H
2SiF
645 grams per liters, free H
2SO
440 grams per liters, with interpole gap 80-90 millimeter, bath voltage 0.3-0.4 volt, current density 50-75 peace/square metre, circulation of elecrolyte amount 20-40 liter/minute, cathode deposition period 4 days, anodic cycle 8 days and every electrolysis were taken out and are cleaned once electrolysis more for the second time in 4 days.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88101044 CN1016366B (en) | 1988-02-24 | 1988-02-24 | Process for producing high purity sn from raw soldering tin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88101044 CN1016366B (en) | 1988-02-24 | 1988-02-24 | Process for producing high purity sn from raw soldering tin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1030450A true CN1030450A (en) | 1989-01-18 |
| CN1016366B CN1016366B (en) | 1992-04-22 |
Family
ID=4831617
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88101044 Expired CN1016366B (en) | 1988-02-24 | 1988-02-24 | Process for producing high purity sn from raw soldering tin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1016366B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104060296A (en) * | 2014-06-16 | 2014-09-24 | 深圳市弘星威焊锡制品有限公司 | High-efficiency environment-friendly high-purity tin refining system |
| CN104060103A (en) * | 2014-06-16 | 2014-09-24 | 深圳市弘星威焊锡制品有限公司 | Recyclable high-purity electric-furnace tin smelting method |
| CN105714329A (en) * | 2014-12-05 | 2016-06-29 | 上海奇谋能源技术开发有限公司 | Method for directly electrolyzing metal scraps |
| CN105839130A (en) * | 2011-07-26 | 2016-08-10 | 吉坤日矿日石金属株式会社 | Method for producing indium hydroxide |
| CN110050089A (en) * | 2016-12-19 | 2019-07-23 | 威立雅环境公司 | For extract include tin and/or lead in conductive mixture electrolytic method |
| CN111472021A (en) * | 2019-01-24 | 2020-07-31 | 升贸科技股份有限公司 | Electrolyte solution |
-
1988
- 1988-02-24 CN CN 88101044 patent/CN1016366B/en not_active Expired
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105839130A (en) * | 2011-07-26 | 2016-08-10 | 吉坤日矿日石金属株式会社 | Method for producing indium hydroxide |
| CN105839130B (en) * | 2011-07-26 | 2018-02-13 | 吉坤日矿日石金属株式会社 | The manufacture method of indium hydroxide |
| CN104060296A (en) * | 2014-06-16 | 2014-09-24 | 深圳市弘星威焊锡制品有限公司 | High-efficiency environment-friendly high-purity tin refining system |
| CN104060103A (en) * | 2014-06-16 | 2014-09-24 | 深圳市弘星威焊锡制品有限公司 | Recyclable high-purity electric-furnace tin smelting method |
| CN104060103B (en) * | 2014-06-16 | 2016-01-27 | 深圳市弘星威焊锡制品有限公司 | Capable of circulation, highly purified electric furnace tin-smelting method |
| CN105714329A (en) * | 2014-12-05 | 2016-06-29 | 上海奇谋能源技术开发有限公司 | Method for directly electrolyzing metal scraps |
| CN105714329B (en) * | 2014-12-05 | 2017-10-20 | 上海奇谋能源技术开发有限公司 | A kind of method of Direct Electrolysis scrap |
| CN110050089A (en) * | 2016-12-19 | 2019-07-23 | 威立雅环境公司 | For extract include tin and/or lead in conductive mixture electrolytic method |
| CN110050089B (en) * | 2016-12-19 | 2021-06-25 | 威立雅环境公司 | Electrolytic process for extracting tin and/or lead contained in an electrically conductive mixture |
| US11280011B2 (en) | 2016-12-19 | 2022-03-22 | Veolia Environment VE | Electrolytic method for extracting tin and/or lead contained in an electrically conductive mixture |
| CN111472021A (en) * | 2019-01-24 | 2020-07-31 | 升贸科技股份有限公司 | Electrolyte solution |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1016366B (en) | 1992-04-22 |
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