CN105671590A - Method for electrolytically refining lead in sulfamate bath - Google Patents
Method for electrolytically refining lead in sulfamate bath Download PDFInfo
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- CN105671590A CN105671590A CN201510875275.4A CN201510875275A CN105671590A CN 105671590 A CN105671590 A CN 105671590A CN 201510875275 A CN201510875275 A CN 201510875275A CN 105671590 A CN105671590 A CN 105671590A
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- thionamic acid
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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
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
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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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- Electrolytic Production Of Metals (AREA)
Abstract
In the electrolytic refining of lead in a sulfamate bath, the production of a white residue is suppressed, and a decrease in the lead concentration in the electrolytic solution is suppressed. A method for electrolytically refining lead in a sulfamate bath, comprising performing electrolytic refining at a decomposition rate of sulfamic acid controlled at 0.06%/day or less.
Description
Technical field
The present invention relates to the electrolysis purification process of lead based on thionamic acid bath, in particular to the electrolysis purification process to the lead based on thionamic acid bath that contained lead in the dry-type soot produced from the melting furnace of the recirculation raw materials such as nonferrous smelting, substrate (base) or electronic component and being carried out by trade waste in the dry type stove of melting treatment reclaims.
Background technology
In order to reclaim lead contained in the dry-type soot of nonferrous smelting from the melting furnace of the recirculation raw materials such as nonferrous smelting, substrate or electronic component and during trade waste is carried out the dry type stove of melting treatment, it is that flue dust is carried out sulfuric acid leaching, make lead sulfate, then melting and reducing in electric furnace. The metal isolated by melting and reducing is carried out soda process, then metal is carried out anode casting, in thionamic acid is bathed, carry out electrolysis purifying afterwards, thus reclaim lead.
As the electrolysis purification technique of such lead, such as, Patent Document 1 discloses the electrolysis process of a kind of lead, wherein, in the electrolysis purifying utilizing thionamic acid to bathe, the current density making for the 1st stage is 50A/m2Carry out the electrolysis of more than 2 hours below, then as the 2nd stage, at 100A/m2Hereinafter carry out electrolysis, thus reclaim the lead of high purity. And record, according to such formation, the lead of high purity can also be reclaimed for the anode of high Bi grade.
Prior art literature
Patent documentation
Patent documentation 1: Japanese Patent No. 5163988 publication.
Summary of the invention
Invent problem to be solved
If implementing the electrolysis purifying of the conventional lead based on thionamic acid bath, then can produce visible White residule in body lotion, and the problem that the lead concentration in electrolytic solution reduces. That is, the residue of white is deposited in the bottom of electrolyzer, is stacked into and to a certain degree then must take out from electrolyzer, therefore needs to stop electrolysis, and White residule its frequency increase more at most. Also have the lead concentration in electrolytic solution that the situation reducing then plumbous galvanic deposit situation variation occurs. Its reason is: by following reaction, decomposes based on the thionamic acid in the electrolysis purifying of the lead of thionamic acid bath, and White residule is piled up with the form of lead sulfate, and the lead concentration in electrolytic solution reduces.
SO3NH2 -+ H2O→SO4 2-+ NH4+
Pb2++ SO4 2-→PbSO4↓
Solve the scheme of problem
The present inventor has carried out research repeatedly for solving above-mentioned problem, found that: by the rate of decomposition of thionamic acid is controlled below prescribed value, in the electrolysis of the lead bathed based on thionamic acid, it is possible to suppress the generation of White residule, suppress the reduction of lead concentration in electrolytic solution.
Taking in the aspect recognizing the present invention completed as background above, it is in the electrolysis purification process of the lead based on thionamic acid bath using lead anode, the rate of decomposition of thionamic acid controls to carry out the electrolysis purification process of the lead based on thionamic acid bath of electrolysis purifying below 0.06%/sky.
The present invention based on thionamic acid bath lead electrolysis purification process in one embodiment, be by thionamic acid bathe in thionamic acid concentration be adjusted to than thionamic acid bathe in lead concentration also high 20-60g/L concentration carry out electrolysis purifying simultaneously.
The present invention based on thionamic acid bath lead electrolysis purification process in another embodiment, be the electrolyte temperature that thionamic acid is bathed is adjusted to 15-30 DEG C carry out electrolysis purifying simultaneously.
Invention effect
According to the present invention, in the electrolysis purifying of the lead bathed based on thionamic acid, it is possible to suppress the generation of White residule, suppress the reduction of lead concentration in electrolytic solution. So the frequency of White residule can be suppressed to take out from electrolyzer. In addition, by suppressing the reduction of lead concentration in electrolytic solution, the management of lead concentration becomes easy, can obtain the galvanic deposit situation of good lead. And the effect that the supplementary frequency also having thionamic acid in electrolysis purifying reduces.
Accompanying drawing explanation
Fig. 1 is the chart of the relation represented between the thionamic acid concentration of embodiment 1 and the rate of decomposition of thionamic acid.
Fig. 2 is the chart of the relation represented between the electrolyte temperature of embodiment 2 and the rate of decomposition of thionamic acid.
Embodiment
Hereinafter further describe the present invention.
In the electrolysis purification process of the lead based on thionamic acid bath of the present invention, the rate of decomposition of thionamic acid controls to carry out electrolysis purifying below 0.06%/sky. Further preferably the thionamic acid concentration adjustment in thionamic acid is bathed be the lead concentration in bathing than thionamic acid also high 20-60g/L concentration carry out electrolysis purifying simultaneously, and preferably the electrolyte temperature that thionamic acid is bathed is adjusted to 15-30 DEG C carry out electrolysis purifying simultaneously.
Based on, in the electrolysis purifying of the lead of thionamic acid bath, anodic reaction and cathodic reaction are as follows:
Anodic reaction: Pb+2SO3NH2-→Pb(SO3NH2)2+ 2e-
Cathodic reaction: Pb (SO3NH2)2+ 2e-→ Pb+2SO3NH2-
Raw material (containing plumbous thing) as electrolysis purifying object is not particularly limited, such as can enumerate by following gained containing plumbous thing etc.: copper mine stone is carried out flash smelting furnace (self-dissolving stove, flashfurnace) process and converter process, then the lead sulfate after converter ashes vitriolization is made lead carbonate by sodium carbonate, then in electric furnace, carry out melting and reducing, the metal soda isolated is processed. As the composition of the raw material (containing plumbous thing) of electrolysis purifying object, lead be principal constituent, if more than 60 quality %, can be such as containing lead 70-90 quality %, tin 0.04 quality %, bismuth 5-30 quality % contain lead thing.
Use the above-mentioned shape being cast as anode containing plumbous thing, carry out electrolysis purifying as anode. The size of the dimension ratio negative electrode of anode is little, is thus possible to prevent fringing effect, it is possible to reclaim good galvanic deposit plumbous smooth and easyly.
By the rate of decomposition of the thionamic acid in electrolytic solution is controlled below 0.06%/sky, it is possible to reduce the accumulation of lead sulfate. Also can suppress the reduction of lead concentration in electrolytic solution. And then can well suppress the deterioration of thionamic acid in the electrolysis purifying of the lead based on thionamic acid bath, suppress the supplementary frequency of thionamic acid. And more than 0.06%/sky, then the generation of lead sulfate increases, the lead from anode has little time stripping, causes lead concentration in electrolytic solution to reduce. And the generation of a large amount of lead sulfate makes to stop electrolysis purifying and takes out the frequency being piled up in the lead sulfate bottom electrolyzer and increase. If the decomposition of thionamic acid advances, then in order to keep the normality of thionamic acid, it is necessary to frequently supplement thionamic acid. The rate of decomposition of thionamic acid is preferably below 0.04%/sky, it is more preferable to below 0.02%/sky.
Thionamic acid rate of decomposition (d) is expressed from the next:
d=Ad/A0
·Ad: the thionamic acid amount decomposed
Ad=residue weight × Pb grade × (97/207)
Above-mentioned " 97 " are thionamic acid molecular weight, and above-mentioned " 207 " are Pb nucleidic mass
·A0: initial thionamic acid amount
The present invention is set to the thionamic acid rate of decomposition of every day, it is preferable that the thionamic acid amount decomposed is the amount being averaged calculated every 1 day by the residue weight after 5 days.
It is preferably the concentration (below also referred to as excess portion) than the also high 20-60g/L of the lead concentration (g/L) in electrolytic solution by the thionamic acid concentration adjustment in electrolytic solution. Such as, about the thionamic acid concentration in the electrolytic solution of the present invention, when the lead concentration in electrolytic solution is 80g/L, it is preferable that be 100-140g/L by the thionamic acid concentration adjustment in electrolytic solution. Wherein accurate, the concentration of thionamic acid should represent the concentration of the mole number for the mole number relative to lead, but the molecular weight of thionamic acid is close with plumbous nucleidic mass, and it is also no problem therefore in fact direct for the concentration of thionamic acid and lead concentration to be contrasted.
It should be noted that, also exceed the concentration higher than 60g/L if the thionamic acid concentration in electrolytic solution being set as than the concentration of the lead concentration (g/L) in electrolytic solution, then the rate of decomposition of thionamic acid increases, it is difficult to be controlled to below 0.06%/sky. And lower than 20g/L, then may lose the additive effect of thionamic acid. In electrolysis thionamic acid decompose advance, concentration continue reduce, therefore, although thionamic acid can be added as required, to keep more than 20g/L, but the rate of decomposition of thionamic acid more than 0.06%/sky time, the frequency of interpolation increases, and the accumulation of lead sulfate increases.
The electrolyte temperature of thionamic acid bath is preferably 15 DEG C-30 DEG C. More than 30 DEG C, then may increasing based on the decomposition of thionamic acid in the electrolysis purifying of the lead of thionamic acid bath, and then cause the accumulation of lead sulfate to increase due to the decomposition increase of thionamic acid, in electrolytic solution, lead concentration may reduce. But, electrolyte temperature is too low, then plumbous galvanic deposit situation may be deteriorated, it is preferred to more than 15 DEG C, it is more preferable to more than 20 DEG C.
Lead concentration in preferred electrolytic solution is 60-80g/L. By such formation, it is possible to obtain the good galvanic deposit situation of lead on negative electrode of by electrolysis purifying galvanic deposit. When the rate of decomposition of thionamic acid is more than 0.06%/sky, it is seen that the lead concentration in electrolytic solution reduces, therefore, it is difficult to control in suitable scope. Therefore, if being below 0.06%/sky, then easily the lead concentration in electrolytic solution is regulated in the narrow scope of 60-80g/L. More preferably the lead concentration in electrolytic solution is 70-80g/L.
(level and smooth as other composition smooth agent in electrolytic solution, smoothingagent), preferably add 1-700mg/LNOIGENBN-1390 (following, " NOIGEN (ノ イ ゲ Application) " is registered trademark) or NOIGENBN-2560. Thus can reclaim good galvanic deposit plumbous more smooth and easyly. NOIGENBN-1390, NOIGENBN-2560 are the nonionogenic tensides taking polyoxyethylene list naphthyl ether as principal constituent, are the commodity of the first industry pharmacy. NOIGENBN-1390 be containing 90% polyoxyethylene list naphthyl ether, all the other be the nonionogenic tenside of water.
The current density of electrolysis is preferably controlled to 50-100A/m2. Thus can reclaim good galvanic deposit plumbous more smooth and easyly.
Embodiment
Hereinafter illustrating embodiments of the invention, these embodiments provide to understand the present invention and advantage thereof better, are not intended to limit invention.
(embodiment 1: the impact of thionamic acid concentration)
As the composition of electrolytic solution, it is being that the solution of concentration described in table 1 adds NOIGENBN-1390 as smooth agent using lead concentration and thionamic acid concentration adjustment so that it is concentration is 10mg/L. To cast the stereotype obtained as anode containing plumbous thing, using stainless steel plate as negative electrode, load electrolyzer alternately. In electrolyzer, above-mentioned electrolytic solution is supplemented, to make electrolytic solution residence time in electrolyzer as the mode feeding of 1 hours, thus make the uniform concentration distribution in electrolyzer after loading electrode. The liquid temperature of electrolytic solution is adjusted to the temperature described in table 1, is energized with the current density described in table 1 simultaneously, carries out the electrolysis purifying of 5 days, reclaim galvanic deposit plumbous. In example 1-2, example 1-3, example 1-4, example 1-5, the thionamic acid rate of decomposition [%] of 5 days are controlled to less than 0.3%.
As a result, in example 1-1, galvanic deposit surface irregularity is obvious, and in example 1-6, example 1-7, in electrolytic solution, the reduction of lead concentration cannot suppress. In example 1-6, the rate of decomposition of thionamic acid is 0.4%, and in example 1-7, the rate of decomposition of thionamic acid is 0.9%. And in example 1-2, example 1-3, example 1-4, example 1-5, the generation of White residule can be suppressed, suppress the reduction of lead concentration in electrolytic solution. Fig. 1 illustrates the chart of the thionamic acid rate of decomposition of representation case 1-3 (excess portion of thionamic acid concentration is 30g/L), example 1-6 (excess portion of thionamic acid concentration is 80g/L), example 1-7 (excess portion of thionamic acid concentration is 130g/L). In table 1 and 2, " thionamic acid concentration (excess portion) represents " the thionamic acid concentration (exceeding the part of plumbous concentration in electrolytic solution) of electrolytic solution ".
[table 1]
(embodiment 2: the impact of electrolysis temperature)
As the composition of electrolytic solution, it is being that the solution of concentration described in table 2 adds NOIGENBN-1390 as smooth agent using lead concentration and thionamic acid concentration adjustment so that it is concentration is 10mg/L. To cast the stereotype obtained as anode containing plumbous thing, using stainless steel plate as negative electrode, load electrolyzer alternately. In electrolyzer, above-mentioned electrolytic solution is supplemented, to make electrolytic solution residence time in electrolyzer as the mode feeding of 1 hours, thus make the uniform concentration distribution in electrolyzer after loading electrode. The liquid temperature of electrolytic solution is adjusted to the temperature described in table 2, is energized with the current density described in table 2 simultaneously, carries out the electrolysis purifying of 5 days, reclaim galvanic deposit plumbous. In example 2-2, example 3-3, the thionamic acid rate of decomposition [%] of 5 days are controlled to less than 0.3%.
As a result, in example 2-1, plumbous galvanic deposit is deteriorated. And in example 2-5, example 2-6, the reduction of lead concentration in electrolytic solution cannot be suppressed. In example 2-5, the rate of decomposition of thionamic acid is more than 3.5%, and in example 2-6, the rate of decomposition of thionamic acid is more than 7%. And in example 2-2, example 2-3, example 2-4, it is possible to suppress the generation of White residule, suppress the reduction of lead concentration in electrolytic solution. Fig. 2 illustrates the chart of the thionamic acid rate of decomposition of representation case 2-2 (electrolysis liquid temperature 15 DEG C), example 2-4 (electrolysis liquid temperature 30 DEG C), example 2-6 (electrolysis liquid temperature 50 DEG C).
[table 2]
Claims (3)
1. the electrolysis purification process of the lead bathed based on thionamic acid, in the electrolysis purification process of the lead based on thionamic acid bath using lead anode, controls to carry out electrolysis purifying below 0.06%/sky by the rate of decomposition of thionamic acid.
2. the electrolysis purification process of lead based on thionamic acid bath according to claim 1, wherein, the thionamic acid concentration adjustment in thionamic acid is bathed be the lead concentration in bathing than thionamic acid also high 20-60g/L concentration carry out electrolysis purifying simultaneously.
3. the electrolysis purification process of lead based on thionamic acid bath described in claim 1 or 2, wherein, the electrolyte temperature that thionamic acid is bathed is adjusted to 15 DEG C-30 DEG C carry out electrolysis purifying simultaneously.
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| CN201811463689.6A CN110079827B (en) | 2014-12-03 | 2015-12-03 | Electrolysis purification method of lead based on sulfamic acid bath |
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| JP2015221585A JP6453743B2 (en) | 2014-12-03 | 2015-11-11 | Method for electrolytic purification of lead using sulfamic acid bath |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4098658A (en) * | 1974-07-25 | 1978-07-04 | Ginatta Marco | Method of extracting metals from spent electric storage batteries |
| JPS5964791A (en) * | 1982-09-30 | 1984-04-12 | Mitsubishi Metal Corp | Lead with low count number of radioactive alpha particle and electrolytic purification thereof |
| CN1083868A (en) * | 1991-03-13 | 1994-03-16 | M.A.工业有限公司 | A kind of from oxidiferous material, particularly from the active material of gleanings, extract the hydrometallurgical method of metallic lead |
| JP2009242845A (en) * | 2008-03-31 | 2009-10-22 | Nippon Mining & Metals Co Ltd | Electrolytic process of lead |
| JP2010222627A (en) * | 2009-03-23 | 2010-10-07 | Nippon Mining & Metals Co Ltd | Electrolytic process of lead |
| JP2010248608A (en) * | 2009-03-23 | 2010-11-04 | Jx Nippon Mining & Metals Corp | Lead electrolytic method (1) |
| CN102011141A (en) * | 2009-03-23 | 2011-04-13 | 吉坤日矿日石金属株式会社 | Lead electrolytic method |
| CN103510109A (en) * | 2013-10-24 | 2014-01-15 | 北京化工大学 | Method for recycling lead-containing grid of waste lead-acid battery through self-gravity contact electrolysis |
-
2015
- 2015-11-11 JP JP2015221585A patent/JP6453743B2/en active Active
- 2015-12-03 CN CN201510875275.4A patent/CN105671590A/en active Pending
- 2015-12-03 CN CN201811463689.6A patent/CN110079827B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4098658A (en) * | 1974-07-25 | 1978-07-04 | Ginatta Marco | Method of extracting metals from spent electric storage batteries |
| JPS5964791A (en) * | 1982-09-30 | 1984-04-12 | Mitsubishi Metal Corp | Lead with low count number of radioactive alpha particle and electrolytic purification thereof |
| CN1083868A (en) * | 1991-03-13 | 1994-03-16 | M.A.工业有限公司 | A kind of from oxidiferous material, particularly from the active material of gleanings, extract the hydrometallurgical method of metallic lead |
| JP2009242845A (en) * | 2008-03-31 | 2009-10-22 | Nippon Mining & Metals Co Ltd | Electrolytic process of lead |
| JP2010222627A (en) * | 2009-03-23 | 2010-10-07 | Nippon Mining & Metals Co Ltd | Electrolytic process of lead |
| JP2010248608A (en) * | 2009-03-23 | 2010-11-04 | Jx Nippon Mining & Metals Corp | Lead electrolytic method (1) |
| CN102011141A (en) * | 2009-03-23 | 2011-04-13 | 吉坤日矿日石金属株式会社 | Lead electrolytic method |
| CN103510109A (en) * | 2013-10-24 | 2014-01-15 | 北京化工大学 | Method for recycling lead-containing grid of waste lead-acid battery through self-gravity contact electrolysis |
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| Publication number | Publication date |
|---|---|
| CN110079827A (en) | 2019-08-02 |
| CN110079827B (en) | 2021-10-15 |
| JP6453743B2 (en) | 2019-01-16 |
| JP2016108663A (en) | 2016-06-20 |
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