CN102534229A - Method for selectively leaching vanadium from vanadium-bearing converter slag - Google Patents
Method for selectively leaching vanadium from vanadium-bearing converter slag Download PDFInfo
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- CN102534229A CN102534229A CN2011104046706A CN201110404670A CN102534229A CN 102534229 A CN102534229 A CN 102534229A CN 2011104046706 A CN2011104046706 A CN 2011104046706A CN 201110404670 A CN201110404670 A CN 201110404670A CN 102534229 A CN102534229 A CN 102534229A
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- vanadium
- leaching
- pulp slurry
- vanadium slag
- converter
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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
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Abstract
The invention discloses a method for selectively leaching vanadium from vanadium-bearing converter slag. The method comprises the following steps: mixing the powdery roasted vanadium-bearing converter slag, a sulfuric acid, tributyl phosphate and sulfonated kerosene to prepare ore pulp, and arranging the ore pulp in a diaphragmless leaching tank with electrodes; stirring the ore pulp, and turning on a power supply to subject the ore pulp to leaching reaction under the action of an electric field to leach vanadyl sulfate; performing solid-liquid separation on the ore pulp subjected to the leaching reaction to obtain vanadyl sulfate-containing filtrate; and the like. Compared with pyrogenic vanadium extraction, the method has the advantages of obtaining more vanadyl sulfate in the filtrate and greatly facilitating post vanadium extraction; and compared with aqueous vanadium extraction in the prior art, the method has the advantage of greatly increasing an output-to-input ratio.
Description
Technical field
The present invention relates under electric field action to leach the method for vanadium from the converter vanadium slag.
Background technology
Vanadium (V) and compound thereof all are important industrial raw material, and vanadium extraction is one of method of using always from the converter vanadium slag.So-called " vanadium extraction " comprises with the converter vanadium slag being that main raw material leaches the vanadylic sulfate (VOSO that belongs to industrial raw material
4), on the basis of vanadylic sulfate, further produce the ammonium poly-vanadate (NH that also belongs to industrial raw material again
4VO
3), make common raw material Vanadium Pentoxide in FLAKES (V with ammonium poly-vanadate
2O
5), be that raw material restores vanadium etc. with the Vanadium Pentoxide in FLAKES.That is to say that the committed step of vanadium extraction is at first to obtain vanadylic sulfate from the converter vanadium slag; The height of the extraction yield of vanadium or the leaching yield of vanadium has also been decided in this committed step basically.With the converter vanadium slag is that main raw material comes the method for vanadium extraction that pyrogenic process and wet method two big classes are arranged.In the pyrogenic process vanadium extraction; It mainly is the thing phase of destroying the converter vanadium slag in advance through roasting; Later stage is come vanadium extraction through acidleach again, though the leaching yield of its vanadium is higher relatively, other metals ion also can be leached in the lump during owing to acidleach; Therefore, make the technology of follow-up precipitation become complicated and strengthen cost.In the wet method vanadium extraction, commonly used have a direct pickling process, and its step comprises: (1) is with sulfuric acid (H
2SO
4) be mixed with pulp slurry with the converter vanadium slag; (2) stir, leave standstill to leach vanadylic sulfate (VOSO
4); (3) filter, get the filtrating of sulfur acid vanadyl; At last, more as required, perhaps just directly from this filtrating, extract vanadylic sulfate, or in the filtrating of this sulfur acid vanadyl, add ammonium sulfate ［ (NH again
4)
2SO
4(being ammonia salt precipitation method), obtaining containing the throw out of ammonium poly-vanadate, and make pure ammonium poly-vanadate; Or calcining ammonium poly-vanadate in oxidizing atmosphere further, to make Vanadium Pentoxide in FLAKES etc.Yet but there is the lower deficiency of extraction yield of vanadium in traditional direct pickling process.As previously mentioned, this is because the vanadylic sulfate leaching yield in committed step is hanged down institute extremely.For this reason, publication No. is that CN102134640A, name are called " with the method for catalytic oxidation leaching converter vanadium slag " and have proposed improved method, specifically is in the step of leaching vanadylic sulfate, to have increased catalytic oxidation.Compare with traditional direct pickling process, this vanadium leaching yield of improving one's methods has improved much really.Yet; (the average anode current density of better example is 900 A/m with embodying what anodic current density of its energy consumption from the vanadium extraction yield that embodies its effect ［ under the identical situation of leaching temperature, leaching time and anodic current density, the average vanadium extraction yields of better three examples are 72.20%=(65.20%+75.20%+76.20%) ÷ 3 ］
2) result that compares sees that its output, input ratio are also still not high enough.
Summary of the invention
The objective of the invention is, provide the higher relatively selectivity from the converter vanadium slag of a kind of output, input ratio to leach the method for vanadium.
The technical scheme that realizes said goal of the invention be a kind of like this from the converter vanadium slag selectivity leach the method for vanadium, the aspect identical with prior art is that this method comprises the steps:
(1) pulverous converter vanadium slag, leaching agent sulfuric acid are mixed being mixed with pulp slurry, and this pulp slurry is placed the no barrier film leaching groove that electrode is installed;
(2) stir also energized, let pulp slurry under electric field action, carry out leaching reaction, to leach vanadylic sulfate;
(3) will carry out leaching reaction pulp slurry afterwards and carry out solid-liquid separation, to get the filtrating of sulfur acid vanadyl;
Its improvements are: in the pulp slurry of step (1), said converter vanadium slag is the converter vanadium slag after the roasting, and its powder size was 100 mesh sieves, and vitriolic concentration is 2～4mol/L, has also added tributyl phosphate (TBP) and sulfonated kerosene in addition; The ratio of each component is sulfuric acid: tributyl phosphate: sulfonated kerosene: the vanadium=7.84～15.68mL in this converter vanadium slag: 1～2mL: 0.5～1.5mL: 0.04 g;
The anodic current density of electric field is 600～800A/m in step (2)
2Leaching temperature is 40～60 ℃, and leaching time does not leach degree of being there to be vanadylic sulfate again.
From scheme, can find out in the pulp slurry component of step (1) preparation, to also have tributyl phosphate and sulfonated kerosene in addition.In the present invention; Tributyl phosphate and sulfonated kerosene are selective agents, after both and leaching agent sulfuric acid mix, can let when leaching vanadium the converter vanadium slag of sulfuric acid after roasting; No longer as existing pyrogenic process vanadium extraction; When the later stage acidleach, other metals ion is also leached in the lump, but let other a large amount of metals ions still be retained in, in filtrating, obtain more vanadylic sulfate in the tailings in vanadium extraction of doing to handle in addition; Also for further vanadium extraction of later stage provides greatly cheap, also just provide cost savings certainly simultaneously.With publication No. is that the scheme that CN102134640A applies for is compared, because the anodic current density of electric field of the present invention on average is merely 700A/m
2(600～800A/m
2), little than this prior art; And the MV of (will in checking, prove) vanadium leaching yield (being said in this application " vanadium extraction yield ") is again than the height of this prior art.So output of the present invention, input ratio also improve a lot.
Below in conjunction with embodiment the present invention is further described.
Embodiment
Selectivity leaches the method for vanadium from the converter vanadium slag, and this method comprises the steps:
(1) pulverous converter vanadium slag, leaching agent sulfuric acid are mixed being mixed with pulp slurry, and this pulp slurry is placed the no barrier film leaching groove that electrode is installed;
(2) stir also energized, let pulp slurry under electric field action, carry out leaching reaction, to leach vanadylic sulfate;
(3) will carry out leaching reaction pulp slurry afterwards and carry out solid-liquid separation, to get the filtrating of sulfur acid vanadyl;
The present invention is in the pulp slurry of step (1), and said converter vanadium slag is the converter vanadium slag after the roasting, and its powder size was 100 mesh sieves, and vitriolic concentration is 2～4mol/L, has also added tributyl phosphate and sulfonated kerosene in addition; The ratio of each component is sulfuric acid: tributyl phosphate: sulfonated kerosene: the vanadium=7.84～15.68mL in this converter vanadium slag: 1～2mL: 0.5～1.5mL: 0.04 g;
The anodic current density of electric field is 600～800A/m in step (2)
2Leaching temperature is 40～60 ℃, and leaching time (is not generally 2～4 hours there to be vanadylic sulfate leaching degree of being again.It will be apparent to those skilled in the art that big in anodic current density, when leaching temperature is higher, leaching time is shorter; Otherwise leaching time is longer).
After the filtrating that obtains the sulfur acid vanadyl, those skilled in the art can make vanadylic sulfate, ammonium poly-vanadate, Vanadium Pentoxide in FLAKES and/or vanadium with existing method fully according to actual needs.So do not give unnecessary details.
For obtaining reliable and better effect, in this embodiment, the anode of step (2) electric field electrode used therein is the DSA anode of iridium tantalum pentoxide coating, and negative electrode is the titanium negative electrode.
The present invention has passed through laboratory proofing.Verification step is identical with the said step of this embodiment.Obtain after the filtrating of sulfur acid vanadyl, adopt wherein content of vanadium of tantalum reagent spectrophotometric analysis, through contrast, calculate the vanadium leaching yield then.Checking is the result be shown in the following table.
In converter vanadium slag during checking after the used roasting, the mass content of vanadium is 4.33%, and each routine consumption is 10.00g.In the following table, " sulfuric acid: tributyl phosphate: sulfonated kerosene: the vanadium in this converter vanadium slag " is abbreviated as " each set of dispense than ", and proportioning is worth related unit identical with described in this embodiment.Used time when leaching time is each example checking.
Table 1
Table 2
Table 3
Can find out that from checking under the identical situation of leaching temperature, leaching time and anodic current density, the effect of checking example 3,6,9 is better, the MV of its vanadium leaching yield is 78.17%, and is much higher more than the MV 72.20% of better three examples of prior art; The anodic current density of electric field of the present invention on average is merely 700A/m in addition
2, and than the 900A/m of prior art
2Little, promptly energy consumption is lower.So output of the present invention, input ratio improve a lot really.
Claims (2)
1. selectivity leaches the method for vanadium from the converter vanadium slag, and this method comprises the steps:
(1) pulverous converter vanadium slag, leaching agent sulfuric acid are mixed being mixed with pulp slurry, and this pulp slurry is placed the no barrier film leaching groove that electrode is installed;
(2) stir also energized, let said pulp slurry under electric field action, carry out leaching reaction, to leach vanadylic sulfate;
(3) will carry out leaching reaction pulp slurry afterwards and carry out solid-liquid separation, to get the filtrating of sulfur acid vanadyl;
It is characterized in that: in the pulp slurry of step (1), said converter vanadium slag is the converter vanadium slag after the roasting, and its powder size was 100 mesh sieves, and said vitriolic concentration is 2～4mol/L, has also added tributyl phosphate and sulfonated kerosene in addition; The ratio of each component is sulfuric acid: tributyl phosphate: sulfonated kerosene: the vanadium=7.84～15.68mL in this converter vanadium slag: 1～2mL: 0.5～1.5mL: 0.04 g;
Anodic current density at electric field described in the step (2) is 600～800A/m
2Leaching temperature is 40～60 ℃, and leaching time does not leach degree of being there to be vanadylic sulfate again.
According to claim 1 said from the converter vanadium slag selectivity leach the method for vanadium, it is characterized in that the anode of the said electric field electrode used therein of step (2) is the DSA anode of iridium tantalum pentoxide coating, negative electrode is the titanium negative electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104046706A CN102534229B (en) | 2011-12-08 | 2011-12-08 | Method for selectively leaching vanadium from vanadium-bearing converter slag |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104046706A CN102534229B (en) | 2011-12-08 | 2011-12-08 | Method for selectively leaching vanadium from vanadium-bearing converter slag |
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|---|---|
| CN102534229A true CN102534229A (en) | 2012-07-04 |
| CN102534229B CN102534229B (en) | 2013-03-27 |
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|---|---|---|---|
| CN2011104046706A Expired - Fee Related CN102534229B (en) | 2011-12-08 | 2011-12-08 | Method for selectively leaching vanadium from vanadium-bearing converter slag |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046786A (en) * | 2013-10-15 | 2014-09-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering metals from vanadium slag |
| CN107287452A (en) * | 2017-06-20 | 2017-10-24 | 东北大学 | A kind of titanizing oxidizing roasting acid-leaching vanadium-extracted method of vanadium slag |
| CN110117714A (en) * | 2019-05-29 | 2019-08-13 | 北京科技大学 | A kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium |
| CN112921190A (en) * | 2021-02-05 | 2021-06-08 | 四川大学 | Method for directly preparing low-valence vanadium-containing solution from vanadium slag |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATA526778A (en) * | 1977-07-21 | 1980-10-15 | Elektrometallurgie Gmbh | METHOD FOR TREATING CHROMED VANDIN SLAGS |
| CN102134640A (en) * | 2011-03-01 | 2011-07-27 | 重庆大学 | Method for leaching vanadium slag in converter by electro-catalytic oxidation |
| CN102168178A (en) * | 2011-04-15 | 2011-08-31 | 重庆大学 | Method for extracting vanadium again from tailing after extracting vanadium from vanadium tailing of converter |
-
2011
- 2011-12-08 CN CN2011104046706A patent/CN102534229B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ATA526778A (en) * | 1977-07-21 | 1980-10-15 | Elektrometallurgie Gmbh | METHOD FOR TREATING CHROMED VANDIN SLAGS |
| AT362590B (en) * | 1977-07-21 | 1981-05-25 | Elektrometallurgie Gmbh | METHOD FOR TREATING CHROME-CONTAINING VANADINE SLAG |
| CN102134640A (en) * | 2011-03-01 | 2011-07-27 | 重庆大学 | Method for leaching vanadium slag in converter by electro-catalytic oxidation |
| CN102168178A (en) * | 2011-04-15 | 2011-08-31 | 重庆大学 | Method for extracting vanadium again from tailing after extracting vanadium from vanadium tailing of converter |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046786A (en) * | 2013-10-15 | 2014-09-17 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for recovering metals from vanadium slag |
| CN104046786B (en) * | 2013-10-15 | 2016-08-31 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method reclaiming metal from vanadium slag |
| CN107287452A (en) * | 2017-06-20 | 2017-10-24 | 东北大学 | A kind of titanizing oxidizing roasting acid-leaching vanadium-extracted method of vanadium slag |
| CN110117714A (en) * | 2019-05-29 | 2019-08-13 | 北京科技大学 | A kind of method of room temperature saturated oxalic acid solution Anodic electrolysis Leaching Vanadium |
| CN110117714B (en) * | 2019-05-29 | 2020-03-17 | 北京科技大学 | Method for leaching vanadium by anode electrolysis in normal-temperature saturated oxalic acid solution |
| CN112921190A (en) * | 2021-02-05 | 2021-06-08 | 四川大学 | Method for directly preparing low-valence vanadium-containing solution from vanadium slag |
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|---|---|
| CN102534229B (en) | 2013-03-27 |
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Granted publication date: 20130327 Termination date: 20201208 |