CN102534229B - 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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- CN102534229B CN102534229B CN2011104046706A CN201110404670A CN102534229B CN 102534229 B CN102534229 B CN 102534229B CN 2011104046706 A CN2011104046706 A CN 2011104046706A CN 201110404670 A CN201110404670 A CN 201110404670A CN 102534229 B CN102534229 B CN 102534229B
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- vanadium
- leaching
- bearing slag
- leach
- pulp slurry
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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
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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 the method from the From Converter Vanadium-bearing Slag Leaching Vanadium.
Background technology
Vanadium (V) and compound thereof all are important industrial raw material, and vanadium extraction is one of method of commonly using from From Converter Vanadium-bearing Slag.So-called " vanadium extraction " comprises and leaches the vanadylic sulfate (VOSO that belongs to industrial raw material take From Converter Vanadium-bearing Slag as main raw material
4), on the basis of vanadylic sulfate, further produce again the ammonium poly-vanadate (NH that also belongs to industrial raw material
4VO
3), make common raw material Vanadium Pentoxide in FLAKES (V with ammonium poly-vanadate
2O
5), restore vanadium etc. take Vanadium Pentoxide in FLAKES as raw material.That is to say, the committed step of vanadium extraction is at first to obtain vanadylic sulfate from From Converter Vanadium-bearing Slag; The height of the extraction yield of vanadium or the leaching yield of vanadium has also been decided in this committed step substantially.Come the method for vanadium extraction that pyrogenic process and wet method two large classes are arranged take From Converter Vanadium-bearing Slag as main raw material.In the pyrogenic process vanadium extraction, it mainly is the phase of destroying in advance From Converter Vanadium-bearing Slag by roasting, later stage is come vanadium extraction by acidleach again, although the leaching yield of its vanadium is relatively high, but other metal ion also can be leached in the lump during owing to acidleach, therefore, so that the technique of follow-up precipitation become complicated and strengthened 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 From Converter Vanadium-bearing Slag; (2) stir, leave standstill to leach vanadylic sulfate (VOSO
4); (3) filter the filtrate that gets the sulfur acid vanadyl; At last, more as required, perhaps just directly from this filtrate, extract vanadylic sulfate, or in the filtrate 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 From Converter Vanadium-bearing Slag " and have proposed Innovative method, has specifically increased catalytic oxidation in the step of leaching vanadylic sulfate.Compare with traditional direct pickling process, this V leaching rate of improving one's methods has improved much really.Yet, from the vanadium extraction yield that embodies its effect ［ in the situation that leaching temperature, leaching time and anodic current density are identical, the average vanadium extraction yield of better three examples is 72.20%=(65.20%+75.20%+76.20%) ÷ 3 ］ with embody what anodic current density of its energy consumption (better the Average anode current density of example is 900 A/m
2) result that compares sees, its output, input ratio are also still not high enough.
Summary of the invention
The objective of the invention is, provide the relatively high selectivity from From Converter Vanadium-bearing Slag of a kind of output, input ratio to leach the method for vanadium.
The technical scheme that realizes described goal of the invention be a kind of like this from From Converter Vanadium-bearing Slag selectivity leach the method for vanadium, aspect same as the prior art is that the method comprises the steps:
(1) pulverous From Converter Vanadium-bearing Slag, leaching agent sulfuric acid are mixed to be mixed with pulp slurry, and with this pulp slurry place be equipped with electrode without barrier film leaching groove;
(2) stir also plugged, allow pulp slurry under electric field action, leach reaction, to leach vanadylic sulfate;
(3) will leach reaction pulp slurry afterwards and carry out solid-liquid separation, to get the filtrate of sulfur acid vanadyl;
Its improvements are: in the pulp slurry of step (1), described From Converter Vanadium-bearing Slag is the From Converter Vanadium-bearing Slag after the roasting, and its powder size was 100 mesh sieves, and the concentration of sulfuric acid is 2～4mol/L, has also added in addition tributyl phosphate (TBP) and sulfonated kerosene; The ratio of each component is sulfuric acid: tributyl phosphate: sulfonated kerosene: the vanadium in this From Converter Vanadium-bearing Slag=7.84～15.68mL: 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 to leach as degree without vanadylic sulfate again.
From scheme, can find out in the pulp slurry component of step (1) preparation, to also have in addition tributyl phosphate and sulfonated kerosene.In the present invention, tributyl phosphate and sulfonated kerosene are selective agents, after both and leaching agent sulfuric acid mix, in the time of can allowing the From Converter Vanadium-bearing Slag of sulfuric acid after roasting Leaching Vanadium, no longer as existing pyrogenic process vanadium extraction, when the later stage acidleach, other metal ion is also leached in the lump, but allow other a large amount of metal ions still be retained in the tailings in vanadium extraction that to do to process in addition, in filtrate, obtain more vanadylic sulfate, also for further vanadium extraction of later stage provides greatly cheap, certainly also just provide cost savings simultaneously.Be that the scheme of CN102134640A application is compared with publication No., because the anodic current density of electric field of the present invention on average only is 700A/m
2(600～800A/m
2), less than the prior art; And the mean value of (will prove in checking) V leaching rate (being said in this application " vanadium extraction yield ") is again than the height of the prior art.So output of the present invention, input ratio also improve a lot.
The present invention is further illustrated below in conjunction with embodiment.
Embodiment
Selectivity leaches the method for vanadium from From Converter Vanadium-bearing Slag, and the method comprises the steps:
(1) pulverous From Converter Vanadium-bearing Slag, leaching agent sulfuric acid are mixed to be mixed with pulp slurry, and with this pulp slurry place be equipped with electrode without barrier film leaching groove;
(2) stir also plugged, allow pulp slurry under electric field action, leach reaction, to leach vanadylic sulfate;
(3) will leach reaction pulp slurry afterwards and carry out solid-liquid separation, to get the filtrate of sulfur acid vanadyl;
The present invention is in the pulp slurry of step (1), and described From Converter Vanadium-bearing Slag is the From Converter Vanadium-bearing Slag after the roasting, and its powder size was 100 mesh sieves, and the concentration of sulfuric acid is 2～4mol/L, has also added in addition tributyl phosphate and sulfonated kerosene; The ratio of each component is sulfuric acid: tributyl phosphate: sulfonated kerosene: the vanadium in this From Converter Vanadium-bearing Slag=7.84～15.68mL: 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 generally 2～4 hours to leach as degree without vanadylic sulfate again.It will be apparent to those skilled in the art that large in anodic current density, when leaching temperature is higher, leaching time is shorter; Otherwise leaching time is longer).
After the filtrate that obtains the sulfur acid vanadyl, those skilled in the art can according to actual needs, make vanadylic sulfate, ammonium poly-vanadate, Vanadium Pentoxide in FLAKES and/or vanadium with existing method fully.Therefore 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 described step of this embodiment.Obtain after the filtrate of sulfur acid vanadyl, adopt wherein content of vanadium of tantalum reagent spectrophotometric analysis, then by contrast, calculate V leaching rate.The result is shown in the following table.
In From Converter Vanadium-bearing 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 From Converter Vanadium-bearing Slag " is abbreviated as " each component proportion ", and proportioning is worth identical with described in this embodiment of related unit.Used time when leaching time is each example checking.
Table 1
Table 2
Table 3
Can find out from checking, in the situation that leaching temperature, leaching time and anodic current density are identical, checking example 3,6,9 effect are better, and the mean value of its V leaching rate is 78.17%, and is much higher more than the mean value 72.20% of better three examples of prior art; The anodic current density of electric field of the present invention on average only is 700A/m in addition
2, and than the 900A/m of prior art
2Little, namely 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 From Converter Vanadium-bearing Slag, and the method comprises the steps:
(1) pulverous From Converter Vanadium-bearing Slag, leaching agent sulfuric acid are mixed to be mixed with pulp slurry, and with this pulp slurry place be equipped with electrode without barrier film leaching groove;
(2) stir also plugged, allow described pulp slurry under electric field action, leach reaction, to leach vanadylic sulfate;
(3) will leach reaction pulp slurry afterwards and carry out solid-liquid separation, to get the filtrate of sulfur acid vanadyl;
It is characterized in that: in the pulp slurry of step (1), described From Converter Vanadium-bearing Slag is the From Converter Vanadium-bearing Slag after the roasting, and its powder size was 100 mesh sieves, and the concentration of described sulfuric acid is 2～4mol/L, has also added in addition tributyl phosphate and sulfonated kerosene; The ratio of each component is sulfuric acid: tributyl phosphate: sulfonated kerosene: the vanadium in this From Converter Vanadium-bearing Slag=7.84～15.68mL: 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 is to leach as degree without vanadylic sulfate again.
According to claim 1 described from From Converter Vanadium-bearing Slag selectivity leach the method for vanadium, it is characterized in that, the anode of the described 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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102534229A CN102534229A (en) | 2012-07-04 |
| CN102534229B true 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2732854C3 (en) * | 1977-07-21 | 1981-12-03 | GfE Gesellschaft für Elektrometallurgie mbH, 4000 Düsseldorf | Process for processing chromium-containing vanadium slags |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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