CN111472021A - Electrolyte solution - Google Patents
Electrolyte solution Download PDFInfo
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- CN111472021A CN111472021A CN201910067471.7A CN201910067471A CN111472021A CN 111472021 A CN111472021 A CN 111472021A CN 201910067471 A CN201910067471 A CN 201910067471A CN 111472021 A CN111472021 A CN 111472021A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/14—Electrolytic production, recovery or refining of metals by electrolysis of solutions of tin
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Abstract
The electrolyte solution of the present invention includes: two compounds and two acids for providing stannous ions; the two compounds are stannous sulfate and stannous chloride with the weight ratio of 1:1 to 20: 1; the two acids are hydrochloric acid and silicofluoric acid in a weight ratio of 0.5:1 to 1000:1, and the concentration of hydrogen ions formed by the hydrochloric acid and the silicofluoric acid is 0.25M to 2.88M; thus, an electrolyte solution is obtained which is simultaneously suitable for electrorefining high-purity crude tin and low-purity crude tin into refined tin.
Description
Technical Field
The invention relates to an electrolyte, in particular to an electrolyte which is simultaneously suitable for refining high-purity crude tin and low-purity crude tin into refined tin by electrolysis.
Background
At present, a crude tin alloy separation method comprises the steps of purifying crude tin into refined tin by adopting a vacuum furnace, a crystallizer and an electrolytic refining method; depending on the purity of the tin to be treated and the content of impurities in the crude tin, the choice of refining method may be influenced. For example, crude tin with high lead and bismuth content is refined by a crystallizer matched with a vacuum furnace, so that refined tin with the weight percentage of more than 99.95 percent can be refined, but the process of the method is complicated, and the required equipment and energy cost are high.
The electrolytic refining method uses crude tin with low purity, such As tin (Sn) >80%, lead (Pb) <8%, iron (Fe) <8% and arsenic (As) <2%, As raw materials to directly produce refined tin by the electrolytic refining method, which can produce refined tin with weight percentage of more than 99.99%, but the content of corresponding metal impurities is limited, for example, the content of lead can not exceed 8%.
In the existing method, no electrolyte is available, which is suitable for electrolytic refining of high-purity crude tin (tin content is more than or equal to 92%) and low-purity crude tin (tin content is less than 92%) into refined tin (tin content is more than 99.99%) and even high-impurity crude tin (lead content is more than 4%) into refined tin; therefore, in the technical field of refined tin electrorefining metallurgy, how to provide an electrolyte solution with wide application of crude tin component has long been a problem to be solved in the industry and academia.
Disclosure of Invention
In view of the above, the present invention provides an electrolyte solution suitable for refining high-purity crude tin and low-purity crude tin into refined tin by electrolysis.
The technical means adopted by the invention are as follows.
The electrolyte is suitable for electrolytic refining of crude tin with tin content of 70-95 wt% and lead content of more than 4% into refined tin with tin content of more than 99.99 wt%. The electrolyte is particularly suitable for electrolytic refining of crude tin with 70-99% of tin content by weight into refined tin with more than 99.99% of tin content by weight, and at least comprises the following components: two methods for providing stannous ion (Sn)2+) The two compounds for providing stannous ions are stannous sulfate (SnSO)4) And stannous chloride (SnCl)2) The weight ratio of the stannous sulfate to the stannous chloride is 1:1 to 20:1, the concentration of the stannous ions is 20 g/L to 100 g/L, and the two acids are hydrochloric acid (HCl) and silicofluoric acid (H)2SiF6) The weight ratio of the hydrochloric acid to the silicofluoric acid is 0.5:1 to 1000:1, and the concentration of hydrogen ions formed by the hydrochloric acid and the silicofluoric acid [ H ] is+]Is 0.25M to 2.88M.
By utilizing the technical characteristics of the method, the device,the prepared electrolyte can be filled in an electrolytic cell and a circulating system, an anode cast by crude tin alloy (the weight percentage of tin content is 70-99%) and a cathode made of high-purity refined tin are fixed in the electrolytic cell, the cell voltage is less than 0.3V, and the current density is 50-200A/m2The electrolytic bath is electrified at normal temperature (15-25 ℃) to electrolyze under the condition of (1), and high-purity refined tin with tin content more than 99.99 percent (or 4 refined tin with 9, 4N) can be produced on the cathode plate.
According to the technical characteristics, the concentration of the hydrochloric acid can be 10 g/L to 100 g/L.
According to the above technical characteristics, the concentration of the silicofluoric acid can be 0.1 g/L to 20 g/L.
According to the technical characteristics, the concentration of the hydrochloric acid is 10 g/L to 100 g/L, and the concentration of the silicofluoric acid is g/L0.1.1 to 20 g/L.
According to the technical characteristics, the weight ratio of the stannous sulfate to the stannous chloride is 2.27: 1.
according to the technical characteristics, the weight ratio of the hydrochloric acid to the silicofluoric acid is 10: 1.
according to the technical characteristics, the weight ratio of the hydrochloric acid to the silicofluoric acid is 50: 1.
according to the technical characteristics, the weight ratio of the stannous sulfate to the stannous chloride is 3.40: 1.
according to the technical characteristics, the weight ratio of the hydrochloric acid to the silicofluoric acid is 10: 1.
according to the technical characteristics, the weight ratio of the hydrochloric acid to the silicofluoric acid is 50: 1.
the technical effects produced by the present invention are as follows.
The electrolyte disclosed by the invention mainly comprises: two compounds and two acids for providing stannous ions; the two compounds are stannous sulfate and stannous chloride with the weight ratio of 1:1 to 20: 1; the two acids are hydrochloric acid and silicofluoric acid in a weight ratio of 0.5:1 to 1000:1, and the concentration of hydrogen ions formed by the hydrochloric acid and the silicofluoric acid is 0.25M to 2.88M; the electrolyte is suitable for electrolytic refining of crude tin with tin content of 70-95 wt% and lead content of more than 4% into refined tin with tin content of more than 99.99 wt%, and is particularly suitable for electrolytic refining of crude tin with tin content of 70-99 wt% into refined tin with tin content of more than 99.99 wt%; in particular, the method has the advantages of simple operation process, wide applicable crude tin component, few equipment types, low equipment investment cost, low capital investment, capability of being carried out at normal temperature, low energy consumption, low operation cost of refined tin production and the like.
Detailed Description
The invention mainly provides electrolyte which is simultaneously suitable for refining high-purity crude tin and low-purity crude tin into refined tin by electrolysis; the electrolyte is suitable for electrolytic refining of crude tin with 70-95 wt% of tin content and more than 4 wt% of lead content into refined tin with more than 99.99 wt% of tin content, in particular to electrolytic refining of crude tin with 70-99 wt% of tin content into refined tin with more than 99.99 wt% of tin content, and at least comprises: two methods for providing stannous ion (Sn)2+) And two acids.
Wherein the two compounds for providing stannous ions are stannous sulfate (SnSO)4) And stannous chloride (SnCl)2) The weight ratio of the stannous sulfate to the stannous chloride is 1:1 to 20:1, and the concentration of the stannous ions is 20 g/L to 100 g/L.
As for the two acids, hydrochloric acid (HCl) and silicofluoric acid (H) are used2SiF6) The weight ratio of the hydrochloric acid to the silicofluoric acid is 0.5:1 to 1000: 1; and the concentration of hydrogen ions formed by the hydrochloric acid and the silicofluoric acid [ H+]Is 0.25M to 2.88M.
In the electrolyte of the present invention, the concentration of the hydrochloric acid may be preferably 10 g/L to 100 g/L, or the concentration of the silicofluoric acid may be 0.1 g/L to 20 g/L, and it is preferable that the concentration of the hydrochloric acid is 10 g/L to 100 g/L, and the concentration of the silicofluoric acid is 0.1 g/L to 20 g/L.
In the electrolyte of the invention, under the implementation mode that the concentration of the hydrochloric acid is 10 g/L-100 g/L and the concentration of the silicofluoric acid is 0.1 g/L-20 g/L, the weight ratio of the stannous sulfate to the stannous chloride can be 2.27: 1.
In the electrolyte of the invention, under the implementation mode that the concentration of the hydrochloric acid is 10 g/L-100 g/L, the concentration of the silicofluoric acid is 0.1 g/L-20 g/L, and the weight ratio of the stannous sulfate to the stannous chloride is 2.27: 1, the weight ratio of the hydrochloric acid to the silicofluoric acid can be 10: 1.
The electrolyte of the invention contains 10 g/L-100 g/L of hydrochloric acid, and the silicofluoric acid [ H ]2SiF6]In the embodiment where the concentration of (a) is 0.1 g/L to 20 g/L and the weight ratio of the stannous sulfate to the stannous chloride is 2.27: 1, the weight ratio of the hydrochloric acid to the silicofluoric acid may also be 50: 1.
In the electrolyte of the invention, under the implementation mode that the concentration of the hydrochloric acid is 10 g/L-100 g/L and the concentration of the silicofluoric acid is 0.1 g/L-20 g/L, the weight ratio of the stannous sulfate to the stannous chloride can be 3.40: 1.
In the electrolyte of the invention, under the implementation state that the concentration of the hydrochloric acid is 10 g/L-100 g/L, the concentration of the silicofluoric acid is 0.1 g/L-20 g/L, and the weight ratio of the stannous sulfate to the stannous chloride is 3.40: 1, the weight ratio of the hydrochloric acid to the silicofluoric acid can be 10: 1.
In the electrolyte of the invention, under the implementation situation that the concentration of the hydrochloric acid is 10 g/L-100 g/L, the concentration of the silicofluoric acid is 0.1 g/L-20 g/L, and the weight ratio of the stannous sulfate to the stannous chloride is 3.40: 1, the weight ratio of the hydrochloric acid to the silicofluoric acid can also be 50: 1.
The following further discloses the specific composition of the electrolyte in three different embodiments and the actually achieved efficacy.
The integral electrolyte of the first embodiment comprises 80 g/L stannous ions, 100 g/L hydrochloric acid, and 10 g/L silicofluoric acid (wherein the weight ratio of the hydrochloric acid to the silicofluoric acid is 100 g/L: 10 g/L = 10: 1), in this embodiment, 35% of hydrochloric acid 485m L can be measured, 35% of silicofluoric acid 47m L is measured, deionized water of 1.5L is poured, 217.12g of chemically pure stannous sulfate which is weighed and 63.89g of chemically pure stannous chloride are added, and stirring is carried out, and a 2L solution is fixed to volume (in this embodiment, the weight ratio of the stannous sulfate to the stannous chloride is 217.12 g: 63.89g = 3.40: 1).
The electrolyte prepared In the first example was prepared by casting an anode (anode weight: 650g) having an effective area of 10cm × 6.5.5 cm using a crude tin alloy having a composition and weight percentage of tin (Sn)77.5968%, lead (Pb)17.2704%, antimony (Sb)0.0709%, copper (Cu)2.4644%, bismuth (Bi)1.9779%, iron (Fe)0.0053%, cadmium (Cd)0.0027%, silver (Ag)0.5600%, arsenic (As)0.0100%, indium (In)0.0031%, nickel (Ni)0.0144% and other trace metals As cathode plates, and casting a cathode plate (cathode weight: 15g) having an effective area of 10cm × 6.5.5 cm from a high-purity fine tin alloy having a composition and weight percentage of tin (Ag) 99.9918%, lead (Pb) 0.0016%, antimony <0.0001%, copper < 0.0039%, bismuth (Ni) 0.0034%, silver (Ag) 0.0007%, and other trace metals As < 0.0003%.
The electrolyte prepared in the first example is filled into an electrolytic cell and a circulating system of 2L, the cathode and the anode are fixed at corresponding positions (the distance is 10cm), the relevant equipment is connected, the electrolysis is carried out under the electrification and the normal temperature, and the current density is 100A/m2When electrolysis was continued for 45 hours, 82g of anode was consumed, and 55g of cathode tin was produced (15 g of the weight of the cathode plate was subtracted).
And washing the cathode plate with deionized water for three times, drying, and melting and casting ingots. Sampling and analyzing, and obtaining the following results in percentage by weight: 99.9910% of tin, 0.0012% of lead, 0.0001% of antimony, 0.0003% of bismuth, 0.0010% of copper, 0.0003% of indium, 0.0003% of silver, 0.0005% of arsenic and 0.0035% of iron; from the above analysis results, it can be known that the purity of the tin produced by the cathode plate in the first embodiment reaches over 99.99%, and the tin reaches the quality standard of high-purity refined tin.
The whole electrolyte of the second embodiment comprises stannous ion 30 g/L, hydrochloric acid 50 g/L, and silicofluoric acid 1 g/L (wherein, the weight ratio of hydrochloric acid to silicofluoric acid is 50 g/L: 1 g/L = 50: 1), in this embodiment, the electrolyte can measure 35% hydrochloric acid 243m L, measure 35% silicofluoric acid 4.7m L, pour deionized water of 1.5L, add 72.37g of chemical pure stannous sulfate after weighing, and 31.95g of chemical pure stannous chloride, stir, and fix volume to 2L solution (in this embodiment, the weight ratio of stannous sulfate to stannous chloride is 72.37 g: 31.95g = 2.27: 1).
The electrolyte prepared in the second embodiment is prepared by using a crude tin alloy to cast an anode (weight of the anode is 652g) with an effective area of 10cm × 6.5.5 cm and a cathode (weight of the cathode is 26g) with an effective area of 10cm × 6.5.5 cm and a thickness of 1mm, wherein the crude tin alloy of the anode comprises 92.6492% by weight of tin, 4.6314% by weight of lead, 0.0703% by weight of antimony, 1.2875% by weight of copper, 0.1748% by weight of bismuth, 0.0197% by weight of iron, 0.0018% by weight of cadmium, 1.1001% by weight of silver, 0.0025% by weight of arsenic, 0.0130% by weight of indium, 0.0358% by weight of nickel and other trace metals, and the cathode comprises high-purity refined tin of 99.9913% by weight of tin, 0.0008% by weight of lead, 0.0001% by weight of antimony, 0.0013% by weight of copper, 0.0002% by weight of bismuth, 0.0036% by weight of iron, 0.0002% by weight of silver, 0..
The electrolyte prepared in the second embodiment is filled into an electrolytic cell and a circulating system of 2L, the cathode and the anode are fixed at corresponding positions (the distance is 10cm), the relevant equipment is connected, the electrolysis is carried out under the electrification and the normal temperature, and the current density is 150A/m2When electrolysis was continued for 45 hours, 90g of the anode was consumed, and 72g of cathode tin (26 g of the weight of the cathode plate was subtracted) was produced.
And washing the cathode plate with deionized water for three times, drying, and melting and casting ingots. Sampling and analyzing, and obtaining the following results in percentage by weight: 99.9915% tin, 0.0031% lead, 0.0001% antimony, 0.0003% bismuth, 0.0004% cadmium, 0.0007% copper, 0.0003% indium, 0.0001% silver, 0.0003% arsenic, 0.0016% iron and other trace metals; from the above analysis results, it can be known that the purity of the tin (Sn) produced by the cathode plate in the second embodiment reaches over 99.99%, and the quality standard of high-purity refined tin is achieved.
The overall electrolyte of the third embodiment comprises stannous ion 60 g/L, hydrochloric acid 50 g/L, and silicofluoric acid 5 g/L (wherein, the weight percentage ratio of hydrochloric acid to silicofluoric acid is 50 g/L: 5 g/L = 10: 1), in this embodiment, the electrolyte can measure 35% hydrochloric acid 243m L, measure 35% silicofluoric acid 24m L, pour deionized water of 1.5L, add 144.75g of chemically pure stannous sulfate, and 63.89g of chemically pure stannous chloride, stir, and fix volume to 2L solution (in this embodiment, the weight percentage ratio of stannous sulfate to stannous chloride is 144.75 g: 63.89g = 2.27: 1).
The electrolyte prepared in the third example was used in combination with an anode (anode weight: 605g) cast from a crude tin alloy having an effective area of 10cm × 6.5.5 cm and a cathode (cathode weight: 20g) cast from a high purity refined tin having an effective area of 10cm × 6.5.5 cm and a thickness of 1mm, wherein the crude tin alloy of the anode had a composition and weight percentage of tin 82.3696%, lead 14.3199%, antimony <0.0005%, copper 2.0708%, bismuth 0.2037%, iron 0.0040%, cadmium <0.0001%, silver 0.9753%, arsenic 0.0025%, indium 0.0137%, nickel 0.0135% and other trace metals, and the high purity refined tin of the cathode had a composition and weight percentage of tin 99.9931%, lead 0.0012%, antimony <0.0001%, copper 0.0007%, bismuth 0.0004%, iron 0.0010%, cadmium 0.0002%, silver 0.0001%, arsenic 0.0022%, indium 0.0003% and other trace metals.
The electrolyte prepared in the third embodiment is filled into an electrolytic cell and a circulating system of 2L, the cathode and the anode are fixed at corresponding positions (the distance is 10cm), the relevant equipment is connected, the electrolysis is carried out under the electrification and the normal temperature, and the current density is 125A/m2After 60 hours of continuous electrolysis, 126g of anode was consumed, yielding 86g of cathode tin (20 g of the cathode plate weight was subtracted).
And washing the cathode plate with deionized water for three times, drying, and melting and casting ingots. Sampling and analyzing, and obtaining the following results in percentage by weight: 99.9913% tin, 0.0008% lead, 0.0001% antimony, 0.0002% bismuth, 0.0013% copper, 0.0003% indium, 0.0002% silver, 0.0003% arsenic, 0.0026% iron and other trace metals; from the above analysis results, it can be known that the purity of the tin (Sn) produced by the cathode plate in the third embodiment reaches over 99.99%, and the quality standard of high-purity refined tin is achieved.
Compared with the conventional technology, the electrolyte disclosed by the invention mainly comprises the following components: two compounds and two acids for providing stannous ions; the two compounds are stannous sulfate and stannous chloride with the weight ratio of 1:1 to 20: 1; the two acids are hydrochloric acid and silicofluoric acid in the weight ratio of 0.5:1 to 1000:1, and the concentration of hydrogen ions formed by the hydrochloric acid and the silicofluoric acid [ H+]From 0.25M to 2.88M; particularly suitable for electrolytic refining of crude tin with 70 to 99 weight percent of tin content into refined tin with more than 99.99 weight percent of tin content; in particular, has an operationSimple process, wide applicable crude tin component, few equipment types, low equipment investment cost, low capital investment, low energy consumption, low production and operation cost of refined tin and the like, and can be carried out at normal temperature.
Claims (10)
1. An electrolyte suitable for electrorefining crude tin having a tin content of 70 to 99% by weight into refined tin having a tin content of more than 99.99% by weight, the electrolyte comprising at least:
two stannous ion providing compounds, wherein the two stannous ion providing compounds are stannous sulfate and stannous chloride, the weight ratio of the stannous sulfate to the stannous chloride is 1:1 to 20:1, and the concentration of the stannous ion is 20 g/L to 100 g/L;
two acids, the two acids are hydrochloric acid and silicofluoric acid, the weight ratio of the hydrochloric acid to the silicofluoric acid is 0.5:1 to 1000:1, and the concentration of hydrogen ions formed by the hydrochloric acid and the silicofluoric acid is 0.25M to 2.88M.
2. The electrolyte of claim 1, wherein the hydrochloric acid has a concentration of 10 g/L to 100 g/L.
3. The electrolyte of claim 1, wherein the concentration of the silicofluoric acid is 0.1 g/L to 20 g/L.
4. The electrolyte of claim 1, wherein the hydrochloric acid has a concentration of 10 g/L to 100 g/L and the silicofluoric acid has a concentration of 0.1 g/L to 20 g/L.
5. The electrolyte of claim 4, wherein the weight ratio of the stannous sulfate to the stannous chloride is 2.27: 1.
6. the electrolyte of claim 5, wherein the weight ratio of the hydrochloric acid to the silicofluoric acid is 10: 1.
7. the electrolyte of claim 5, wherein the weight ratio of the hydrochloric acid to the silicofluoric acid is 50: 1.
8. the electrolyte of claim 4, wherein the weight ratio of the stannous sulfate to the stannous chloride is 3.40: 1.
9. the electrolyte of claim 8, wherein the weight ratio of the hydrochloric acid to the silicofluoric acid is 10: 1.
10. the electrolyte of claim 8, wherein the weight ratio of the hydrochloric acid to the silicofluoric acid is 50: 1.
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| CN201910067471.7A CN111472021A (en) | 2019-01-24 | 2019-01-24 | Electrolyte solution |
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| CN201910067471.7A CN111472021A (en) | 2019-01-24 | 2019-01-24 | Electrolyte solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7168900B1 (en) * | 2022-08-08 | 2022-11-10 | 千住金属工業株式会社 | Sn electrolytic refining method, method for producing Sn, and anode material for Sn electrolytic refining |
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| CN1150182A (en) * | 1995-11-15 | 1997-05-21 | 个旧市冶金研究所 | Direct electrolyzing method for producing high-quality fine Sn using low-quality crude Sn |
| JP2003183871A (en) * | 2001-12-14 | 2003-07-03 | Mitsubishi Materials Corp | Electrolytic refining method for producing high-purity tin, and apparatus therefor |
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| 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 |
| CN107849716A (en) * | 2016-03-09 | 2018-03-27 | Ｊｘ金属株式会社 | High-purity tin and its manufacture method |
| EP3385409A1 (en) * | 2017-04-04 | 2018-10-10 | Estanos y Soldaduras Senra, S.L.U. | Electrolytic sulphuric acid bath and method for tin electrorefinig |
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| CN1030450A (en) * | 1988-02-24 | 1989-01-18 | 个旧市焊料厂 | Technology with producing high purity Sn from raw soldering tin |
| JPH02228487A (en) * | 1989-03-02 | 1990-09-11 | Mitsui Mining & Smelting Co Ltd | Production of high purity tin |
| CN1150182A (en) * | 1995-11-15 | 1997-05-21 | 个旧市冶金研究所 | Direct electrolyzing method for producing high-quality fine Sn using low-quality crude Sn |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP7168900B1 (en) * | 2022-08-08 | 2022-11-10 | 千住金属工業株式会社 | Sn electrolytic refining method, method for producing Sn, and anode material for Sn electrolytic refining |
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