CN102220487A - Method for extracting vanadium and aluminum from vanadium-containing stone coal and clay vanadium ore - Google Patents
Method for extracting vanadium and aluminum from vanadium-containing stone coal and clay vanadium ore Download PDFInfo
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- CN102220487A CN102220487A CN2011101471944A CN201110147194A CN102220487A CN 102220487 A CN102220487 A CN 102220487A CN 2011101471944 A CN2011101471944 A CN 2011101471944A CN 201110147194 A CN201110147194 A CN 201110147194A CN 102220487 A CN102220487 A CN 102220487A
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- vanadium
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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
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Abstract
The invention relates to a method for extracting vanadium and aluminum from vanadium-containing stone coal and clay vanadium ore, which belongs to the technical field of extraction of rare metals. A vanadium source is reacted with a leaching agent comprising silicofluoric acid and water for getting a solution containing the vanadium and the aluminum, vanadic oxide is further obtained through the ion exchange method or the solvent extraction method, and aluminum salts are finally recovered from the solution after vanadium extraction. By adopting the method, hydrofluosilic acid can be recycled for a plurality of times and the environmental pollution is reduced; and the problem that a by-product, namely tschermigite with limited purposes is generated in the prior art can be further solved, and iron-free aluminum sulfate which can be used for paper-making is generated through the solvent extraction method.
Description
Technical field
What the present invention relates to is the method in a kind of rare metal extractive technique field, specifically is a kind of method of extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite.
Background technology
Vanadium is a kind of important rare metal, is widely used for catalyzer of producing steel alloy, non-ferrous metal alloy and chemical industry etc.China extensively distributes contains the scherbinaite coal and the clay navajoite is important vanadium extraction raw material.Also contain valuable metals such as aluminium in these class mineral.
The technology of extracting vanadium at present from this class navajoite is divided into two classes: a class is to select for use pyrometallurgy to handle, promptly add different salt with containing the vanadium raw materials roasting, is divided into oxidizing roasting, sodiumizing-oxidizing roasting, calcification baking, sodium calcification baking again.Roasting material water or dilute sulphuric acid are leached, make vanadium and other element enter solution.Another kind ofly directly use high concentration, heavy dose of sulfuric acid in high temperature (greater than 95 degrees centigrade) long-time (about 10 to 30 hours) leaching for containing vanadium raw materials, perhaps add other additive or claim promoter with sulfuric acid, such as calcirm-fluoride, sodium fluoride, fluosilicic acid, hydrogen peroxide, hypochlorite etc., under normal temperature and/or high temperature, leach with different solid-liquid ratios.After changing vanadium over to solution, available existing method: ion-exchange or solvent extraction obtain to meet the vanadic anhydride more than 98 grades among the GB3283-87 from contain vanadium solution.
Produce a large amount of toxic and harmfuls during the roasting of first kind technology, environmental pollution is serious, complex process, and the rate of recovery of vanadium low (50%-60%).The second class technology extraction time is long, the energy consumption height, and acid consumption is big, and cost is very high, and the leaching rate of vanadium is the highest to be had only about 80%.And this technology is very low to the dissolution rate of the so costly metal of the aluminium in Rock coal containing alum and the clay vanadium mineral, and the value of comprehensive utilization is also low.Up to now, it is good still to lack a kind of metal recovery rate height, environmental friendliness, comprehensive utilization of resources, the method for extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite that adaptability to raw material is wide.
Further retrieval is found, Chinese patent literature CN 101624649A, open day on January 13rd, 2010, put down in writing a kind of method that from contain the scherbinaite colliery, leaches vanadium with the collaborative sulfuric acid of silicofluoric acid, this technology will contain the fragmentation of scherbinaite colliery, wet grinding to granularity less than 0.15mm, water is 1-3 with the volume mass ratio that contains the scherbinaite colliery in the ore pulp that ore grinding obtains: 1, add silicofluoric acid and sulfuric acid and carry out the leaching of vanadium, the silicofluoric acid consumption is calculated as the 5%-15% that contains scherbinaite colliery quality with the silicofluoric acid of 100% mass concentration, the sulfuric acid consumption is the 10%-25% that contains scherbinaite colliery quality, 80 ℃-95 ℃ of leaching process temperature. extraction time 2h-20h, leach after liquid-solid separation obtains containing vanadium leachate.Leachate iron powder reducing ferric ion, with lime and ammoniacal liquor the pH value is adjusted to 2.8-3.0 after, through solvent extraction, oxidation, adding ammoniacal liquor, obtain the ammonium poly-vanadate precipitation, ammonium poly-vanadate is through calcining preparation powdery vanadic anhydride product.Leach for a long time but must expend sulfuric acid high temperature during this technology implementation, and complex technical process, the energy consumption height, except that vanadium, other valuable metals can not efficient recovery.The colloidal sol shape material that contains impurity such as iron and a large amount of silicon and aluminium in the leach liquor makes very difficulty of subsequent treatment process such as solid-liquid separation, and the difficulty of liquid waste disposal and cost are all very high.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of method of extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite is provided, from contain scherbinaite coal and clay navajoite, extract vanadium and aluminium.
The present invention is achieved by the following technical solutions, the present invention obtains containing the solution of vanadium and aluminium by the leaching agent reaction that vanadium source and silicofluoric acid and water are formed, and further obtain Vanadium Pentoxide in FLAKES by ion exchange method, after vanadium extraction, reclaim iron-free aluminium salt with solvent extration the liquid at last.
Concrete technological process of the present invention is: at first add sodium chlorate in the leachate or the oxidants such as clorox or potassium permanganate are oxidized to pentavalent with Low Valent Vanadium, with pulverized limestone pH value of solution is transferred to 2.0-2.5 again, the calcium slag is filtered obtain liquid before the exchange.With the vanadium in the liquid before the D301 ion exchange resin absorption exchange, and aluminium is stayed in the rear liquid of exchange.With the rich resin that carries vanadium of the sodium hydroxide solution wash-out of 1mol/L-3mol/L, obtaining concentration is the V of 40-120g/L
2O
5Rich vanadium solution.In rich vanadium solution, add ammonium chloride, obtain ammonium meta-vanadate.Ammonium meta-vanadate is 500～550 ℃ of following calcinations, produces the powdery Vanadium Pentoxide in FLAKES that quality is better than among the GB3283-87 98 grades.
In the liquid of exchange back, add Sodium sulfate anhydrous.min(99) (Na while stirring
2SO
4), obtain sodium silicofluoride and Sodium Fluoride mixture.Add pulverized limestone in the solution after the separate fluorine compound, pH is transferred to 6.5-7.0 aluminium is entered in the slag.After the Separation of Solid and Liquid, obtain the aluminium slag.With an amount of sulfuric acid to leach aluminium slag, obtain aluminum sulfate solution.With the iron in the solvent extration extraction alum liquor, the extraction agent component is (V/V): N235:20%; TBP:10%; No. 260 solvent oils: 70%.Alum liquor after the deironing is heated to 118 ℃ of boiling points, and crystallisation by cooling obtains non-iron aluminium sulfate, and it is one of raw material of papermaking.
The mixture of prodan and sodium fluoride is put into reaction vessels, add the concentrated sulfuric acid, 250-350 ℃ of lower reaction, produce hydrogen fluoride gas, water absorbs hydrogen fluoride gas, obtains hydrofluoric acid.In hydrofluoric acid, add silica flour, stirred at normal temperatures 1-5 hour, obtain fluosilicic acid.The silicofluoric acid that obtains is used for leaching raw ore again.So move in circles.
Described vanadium source is: fineness is the ashes after 60 order to 170 purpose powdery Rock coal containing alums, clay vanadium mineral or the Rock coal containing alum fluidized bed combustion, and wherein: the component of Rock coal containing alum and mass percent (%) are SiO
2: 52.76; Fe:3.01; Al
2O
3: 13.72; CaO:0.83; V
2O
5: 1.28; The component of clay vanadium mineral and mass percent (%) are SiO
2: 69.76; Fe:2.16; Al
2O
3: 17.1; CaO:0.93; V
2O
5: 1.27; The component of the ashes after the Rock coal containing alum fluidized bed combustion and mass percent (%) are SiO
2: 63.41; Fe
2O
3: 4.83; Al
2O
3: 20.35; CaO:0.40; V
2O
5: 1.36.
The ratio of water and industrial silicofluoric acid is (v/v) in the described leaching agent: 10: 13～15.
Silicofluoric acid concentration is 3-40% (weight percent concentration) in the described leaching agent.
Described reaction is meant: reaction is 15 minutes-200 minutes under 70 ℃ of-130 ℃ of environment.
Described aluminium salt is: aluminum fluoride, Tai-Ace S 150 or aluminium hydroxide.
Compared with prior art, the reaction times of the present invention is short, and energy consumption is lower, and solid-liquid separation and subsequent disposal are easy, silicofluoric acid repeatedly can be recycled, and have reduced environmental pollution widely; When extracting Vanadium Pentoxide in FLAKES, the present invention has further solved the very little byproduct tschermigite of market capacity that produces in the prior art, produce market capacity big, can be as the non-iron aluminium sulfate of paper making raw material.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
Rock coal containing alum 100g, granularity-170 order adds water 100mL, and industrial fluosilicic acid 130mL at 95 ℃ of lower reaction 2h, filters and with running water drip washing three times, acquisition leachate 309.6mL, leached mud 89.5g, leachate contains V
2O
53.90g/L, Al
2O
331.06g/L leached mud contains V
2O
50.068%, Al
2O
34.12%.In leachate, add glauber salt (Na
2SO
4) 32g, obtain prodan 41.2g, in the later solution of separate fluorine sodium metasilicate, add NaClO
30.4g, pulverized limestone 14g, pH value of solution 2.20 with D301 resin 7mL absorption vanadium, with the rich resin that carries of 8% sodium hydroxide solution washing, produces V
2O
5Concentration is the eluent 27.1mL of 43.6g/L, adds industrial ammonium chloride 2.5g in eluent, obtains ammonium metavanadate, and ammonium metavanadate at 530 ℃ of lower calcination 3h, is obtained powdery V
2O
51.09g, its V
2O
5Content is 99.1%.Sodium Silicofluoride is put into reactor, add the vitriol oil (98%) 12mL, react 1.5h down at 310 ℃, the silicofluoric acid gas that the water absorption reaction produces obtains silicate fluoride solution 100.5mL, and silicofluoric acid concentration is 28.2%.
Add pulverized limestone (CaO) 5.6 grams in the rear liquid of absorption, control solution endpoint pH is 6.6, and the aluminium slag namely precipitates.Aluminium slag after filtering with running water drip washing three times, is added the 150mL running water again and sizes mixing, add while stirring concentrated sulfuric acid 16mL, with the slag elimination and with the clear water washing, obtain Aluminum Sulfate Solution solution 220mL.(it consists of (V/V): N23520% with extraction agent; TBP 10%; No. 260 solvent oils 70%) iron in the four-stage counter-current extraction Aluminum Sulfate Solution solution.Aluminum sulfate solution after the deironing is concentrated into 118 ℃ of boiling points, and crystallisation by cooling gets non-iron aluminium sulfate 54.2 gram, wherein Al
2O
3Content is 16.01%, and iron content is 0.004%.
Embodiment 2:
Clay vanadium mineral 100g, granularity-60 order adds water 90mL, and industrial fluosilicic acid 140mL at 98 ℃ of lower reaction 2h, filters and with running water drip washing three times, acquisition leachate 303.2mL, leached mud 88g, leachate contains V
2O
53.80g/L, Al
2O
336.98g/L leached mud contains V
2O
50.12%, Al
2O
35.83%.In leachate, add glauber salt (Na
2SO
4) 34.5g, obtain prodan 43.2g, in the later solution of separate fluorine sodium metasilicate, add NaClO
30.4g, pulverized limestone 13g, pH value of solution 2.15 with D301 resin 7mL absorption vanadium, with the rich resin that carries of 8% sodium hydroxide solution washing, produces V
2O
5Concentration is the eluent 25.4mL of 40.2g/L, adds industrial ammonium chloride 2.4g in eluent, obtains ammonium metavanadate, and ammonium metavanadate at 530 ℃ of lower calcination 3h, is obtained powdery V
2O
51.09g, its V
2O
5Content is 98.7%.Sodium Silicofluoride is put into reactor, add the vitriol oil (98%) 13mL, react 1h down at 305 ℃, the silicofluoric acid gas that the water absorption reaction produces obtains silicate fluoride solution 110.7mL, and silicofluoric acid concentration is 26.9%.
Add pulverized limestone (CaO) 6.2 grams in the rear liquid of absorption, control solution endpoint pH is 6.5, and the aluminium slag namely precipitates.Aluminium slag after filtering with running water drip washing three times, is added the 160mL running water again and sizes mixing, add while stirring concentrated sulfuric acid 17mL, with the slag elimination and with the clear water washing, obtain Aluminum Sulfate Solution solution 240mL.(it consists of (V/V): N23520% with extraction agent; TBP 10%; No. 260 solvent oils 70%) iron in the four-stage counter-current extraction Aluminum Sulfate Solution solution.Aluminum sulfate solution after the deironing is concentrated into 117 ℃ of boiling points, and crystallisation by cooling gets non-iron aluminium sulfate 65.7. gram, wherein Al
2O
3Content is 16.12%, and iron content is 0.004%.
Embodiment 3:
Contain the lime-ash 100g after the fluidized bed burning of scherbinaite, granularity-120 order adds entry 100mL, and industrial silicofluoric acid 150mL at 96 ℃ of reaction 2h down, filters and with tap water drip washing three times, acquisition leach liquor 324.5mL, leached mud 86g.Leachate contains V
2O
54.01g/L, Al
2O
345.2g/L leached mud contains V
2O
50.063%, Al
2O
36.43%.In leachate, add glauber salt (Na
2SO
4) 37g, obtain prodan 46.8g, in the later solution of separate fluorine sodium metasilicate, add NaClO
30.4g, pulverized limestone 15g, pH value of solution 2.30 with D301 resin 7mL absorption vanadium, with the rich resin that carries of 8% sodium hydroxide solution washing, produces V
2O
5Concentration is the eluent 27.3mL of 44.3g/L, adds industrial ammonium chloride 2.6g in eluent, obtains ammonium metavanadate, and ammonium metavanadate at 530 ℃ of lower calcination 3h, is obtained powdery V
2O
51.19g, its V
2O
5Content is 99.10%.Sodium Silicofluoride is put into reactor, add the vitriol oil (98%) 15mL, react 1.5h down at 310 ℃, the silicofluoric acid gas that the water absorption reaction produces obtains silicate fluoride solution 120.8mL, and silicofluoric acid concentration is 27.9%.
Add pulverized limestone (CaO) 8.4 grams in the rear liquid of absorption, control solution endpoint pH is 6.7, and the aluminium slag namely precipitates.Aluminium slag after filtering with running water drip washing three times, is added the 190mL running water again and sizes mixing, add while stirring concentrated sulfuric acid 23mL, with the slag elimination and with the clear water washing, obtain Aluminum Sulfate Solution solution 320mL.(it consists of (V/V): N23520% with extraction agent; TBP 10%; No. 260 solvent oils 70%) iron in the four-stage counter-current extraction Aluminum Sulfate Solution solution.Aluminum sulfate solution after the deironing is concentrated into 119 ℃ of boiling points, and crystallisation by cooling gets non-iron aluminium sulfate 78.30 gram, wherein Al
2O
3Content is 16.82%, and iron content is 0.003%.
Claims (7)
1. method of from contain scherbinaite coal and clay navajoite, extracting vanadium and aluminium, it is characterized in that, obtain containing vanadium and aluminum solutions by the leaching agent reaction that vanadium source and silicofluoric acid and water are formed, and further obtain Vanadium Pentoxide in FLAKES by ion-exchange or solvent extration, after vanadium extraction, reclaim aluminium salt at last the liquid.
2. the method for extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite according to claim 1, it is characterized in that described vanadium source is: fineness is the ashes after 60 order to 170 purpose powdered contain scherbinaite coal, clay navajoite or contain the fluidized bed burning of scherbinaite.
3. the method for extracting vanadium and aluminium from Rock coal containing alum and clay vanadium mineral according to claim 2 is characterized in that the component of described Rock coal containing alum and mass percent (%) are SiO
2: 52.76, Fe:3.01, Al
2O
3: 13.72, CaO:0.83, V
2O
5: 1.28; The component of clay vanadium mineral and mass percent (%) are SiO
2: 69.76, Fe:2.16, Al
2O
3: 17.1, CaO:0.93, V
2O
5: 1.27; The component of the ashes after the Rock coal containing alum fluidized bed combustion and mass percent (%) are SiO
2: 63.41, Fe
2O
3: 4.83, Al
2O
3: 20.35, CaO:0.40, V
2O
5: 1.36.
4. the method for extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite according to claim 1 is characterized in that the volume ratio of water and industrial silicofluoric acid is 10: 13～15 in the described leaching agent.
5. the method for extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite according to claim 4 is characterized in that described silicofluoric acid concentration is 3-40%.
6. the method for extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite according to claim 1 is characterized in that described reaction is meant: reaction is 15 minutes-200 minutes under 70 ℃ of-130 ℃ of environment.
7. the method for extracting vanadium and aluminium from contain scherbinaite coal and clay navajoite according to claim 1 is characterized in that described aluminium salt is: aluminum fluoride, Tai-Ace S 150 or aluminium hydroxide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560104A (en) * | 2012-02-07 | 2012-07-11 | 九江佰盾钒技术贸易有限公司 | Method for increasing leaching rate of vanadium from stone coal vanadium ores |
| CN107983764A (en) * | 2017-12-19 | 2018-05-04 | 湖南华麒资源环境科技发展有限公司 | A kind of method that chromium-polluted soil repairs upgrading |
| CN115198116A (en) * | 2022-07-21 | 2022-10-18 | 上海寰泰绿钒科技有限公司 | Method for extracting vanadium from vanadium-containing stone coal |
| CN116516180A (en) * | 2023-07-04 | 2023-08-01 | 北京科技大学 | Method for extracting vanadium by high-efficiency direct leaching of stone coal |
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| CN101285132A (en) * | 2008-06-05 | 2008-10-15 | 贵州省地质矿产中心实验室 | Method for cleanly extracting vanadium from vanadium-containing carbonaceous shale |
| CN101624649A (en) * | 2009-08-04 | 2010-01-13 | 长沙达华矿业技术开发有限公司 | Method for leaching vanadium from vanadous stone coal ore with fluosilicic acid and sulphuric acid |
| CN102010984A (en) * | 2010-12-23 | 2011-04-13 | 中南大学 | Method for extracting vanadium in coal gangue |
-
2011
- 2011-06-02 CN CN2011101471944A patent/CN102220487B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101285132A (en) * | 2008-06-05 | 2008-10-15 | 贵州省地质矿产中心实验室 | Method for cleanly extracting vanadium from vanadium-containing carbonaceous shale |
| CN101624649A (en) * | 2009-08-04 | 2010-01-13 | 长沙达华矿业技术开发有限公司 | Method for leaching vanadium from vanadous stone coal ore with fluosilicic acid and sulphuric acid |
| CN102010984A (en) * | 2010-12-23 | 2011-04-13 | 中南大学 | Method for extracting vanadium in coal gangue |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560104A (en) * | 2012-02-07 | 2012-07-11 | 九江佰盾钒技术贸易有限公司 | Method for increasing leaching rate of vanadium from stone coal vanadium ores |
| CN107983764A (en) * | 2017-12-19 | 2018-05-04 | 湖南华麒资源环境科技发展有限公司 | A kind of method that chromium-polluted soil repairs upgrading |
| CN115198116A (en) * | 2022-07-21 | 2022-10-18 | 上海寰泰绿钒科技有限公司 | Method for extracting vanadium from vanadium-containing stone coal |
| CN116516180A (en) * | 2023-07-04 | 2023-08-01 | 北京科技大学 | Method for extracting vanadium by high-efficiency direct leaching of stone coal |
| CN116516180B (en) * | 2023-07-04 | 2023-09-22 | 北京科技大学 | Method for extracting vanadium by high-efficiency direct leaching of stone coal |
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