CN101210287A - Acidolysis oxidation conversion method for extracting vanadium from stone coal - Google Patents
Acidolysis oxidation conversion method for extracting vanadium from stone coal Download PDFInfo
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- CN101210287A CN101210287A CNA2007101927005A CN200710192700A CN101210287A CN 101210287 A CN101210287 A CN 101210287A CN A2007101927005 A CNA2007101927005 A CN A2007101927005A CN 200710192700 A CN200710192700 A CN 200710192700A CN 101210287 A CN101210287 A CN 101210287A
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- vanadium
- water
- vitriol oil
- stone coal
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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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
A method for extracting vanadium in stone coal by acidolysis, oxidation and conversion comprises the following steps: (1) pulverizing stone coal and grinding to powder of 60 to 120 meshes; (2) adding water and concentrated sulfuric acid according to a weight ratio of stone coal powder to concentrated sulfuric acid to water of 100:(15-25):(6-10), stirring uniformly and standing for 16 to 60 days in an open manner; (3) adding water according to a solid-to-liquid ratio of 1:(1-5) and stirring for 1 to 4 h; (4) adding reducer sodium hyposulfite according to the content of Fe contained in the solution to reduce Fe in the solution if Fe(II) or/and Fe(III) is/are contained in the solution; and (5) adjusting pH value to 2 to 3, heating to 30 to 60 DEG C, and filtering to obtain a blue filtrate containing vanadyl sulfate. The invention has the advantages of simple process, low requirement for equipment, high vanadium leaching efficiency (not less than 88%), less reagent consumption, less pollution, etc.
Description
Technical field
The present invention relates to a kind of method of from contain the scherbinaite coal, extracting vanadium, specifically, relate to a kind of acid hydrolysis oxidative and transform the method that leaches vanadium in the bone coal.
Background technology
Bone coal system is characterized in ash-rich, low heat value, outward appearance such as black stone by the high-quality degree incendivity mineral products that the fungus algae unicellular lower eukaryote forms under the reducing environment of shallow sea.Bone coal contains valuable metals such as vanadium, phosphorus, copper, aluminium, uranium, manganese mostly, and the bone coal that wherein contains vanadium is unique single mineral wealth of vanadium, thereby, be important vanadium resource.
The material that contains the scherbinaite coal is formed complicated, the occurrence status and the occurrence status of vanadium are varied, disperse trickle, in same ore body, there is the vanadium minerals more than five kinds usually, vanadium major part in the bone coal is present in the clay minerals such as mica group and kaolin with the trivalent vanadium form, part replaces the silica octahedron, the Al in " multiple stratum reticulare " and the alumina octahedron " single stratum reticulare "
3+, Tl
3+Or Fe
3+Deng, in addition, also can form titanium scherbinaite garnet, mineral such as chromium barium garnet, pozzuolite vanadium copper also have the metallo-organic complex that exists with vanadium quinoline form, also may be the attached state of leaf with complex anion and exist.Multiple valence state oxide compound is composed and is deposited, and mix mutually and mix life, and disseminated grain size is thinner, and the argillization state is serious, and the granularity thickness is extremely inhomogeneous, and microfine is quartzy and clay content is very high, and the existence of vanadium presents complicacy, variation, characteristics such as changeableization.
Thereby the separation of these class mineral and enrichment be difficulty and complicated quite.For vanadium minerals complicated and changeable in the coal is extracted, on the principles of chemistry, must make insoluble trivalent vanadium be converted into the vanadium of soluble tetravalence vanadium or pentavalent. aspect mineral processing craft, must make vanadium minerals complicated and changeable change single mineral into.
At present, routine techniques mainly is the method that adopts with the salt high-temperature roasting, and its roasting reaction is a surface chemical reaction basically, and owing to content of vanadium low (about 1%) in the bone coal, the addition of salt is limited, baryta mineral behavior complexity, metal recovery rate low (40%), valuable metal disperses, reagent consumption is big, be difficult to overcome the complicacy of mineral, make the vanadium in mineral separation difficulty, big for environment pollution.Even the acidleach technology of announcing also is to finish under peracid, high temperature, high pressure recently, the device structure complexity, investment is big, the cost height.
Summary of the invention
The objective of the invention is to overcome the defective that prior art exists, a kind of metal recovery rate height is provided, environmental pollution is few, and equipment is simple, invest lessly, and the acid hydrolysis oxidative that production cost is lower transforms the method for vanadium in the leaching bone coal.
The objective of the invention is to be achieved through the following technical solutions, it may further comprise the steps:
(1) bone coal is pulverized, worn into 60-120 order powder; (2) press stone coal powder: the vitriol oil: the weight proportion of water=100: 15-25 (preferred 16-20, more preferably 17): 6-10 (preferred 7-8, more preferably 7.65) adds the entry and the vitriol oil, stirs, and opens wide and stacks 16-60 days (preferred 20-40 days); (3) again by 1: (preferred 1: solid-to-liquid ratio 1.5-2.5) adds water to 1-5, stirs 1-4 hour; (4) as containing ferrous iron in the solution or/and ferric iron, then also should add reductive agent according to what of iron-holder in the solution, make iron reduction contained in the solution; (5) adjust pH is heated to 30-60 ℃ to 2-3 (preferred 2.5), filters, and obtains the filtrate of blue sulfur acid vanadium acyl.
In pilling up time, sulfuric acid and water generation hydration reaction produce heat, with trivalent vanadium generation redox reaction, generate tetravalence vanadium soluble in water, i.e. vanadium sulfate acyl:
(V
2O
3)X+2H
2SO
4+1/2O
2→V
2O
2(SO
4)
2+2H
2O+X (1)
V
2O
2(OH)
4+2H
2SO
4+1/2O
2→V
2O
2(SO
4)
2+4H
2O (2)
Molecular oxygen in the reaction formula is exactly from airborne oxygen.
The described vitriol oil can use the industrial vitriol oil of sulfuric acid content 〉=98%.
Described reductive agent can be the similar reductive agent of Sulfothiorine or iron powder or other.
In reaction process, other gangue composition becomes not change, and is retained in the ore pulp.
After obtaining vanadium sulfate acyl solution, after known maturation process such as follow-up extraction/precipitation are handled, just can obtain qualified Vanadium Pentoxide in FLAKES product again.
Reaction conditions gentleness of the present invention gets final product so only need do general rotproofing to mechanical means.
It is that cleaning technique are leached in a kind of reinforcement that acid hydrolysis oxidative of the present invention transforms leaching process, and the restriction that not changed by mineral composition.
It is simple that the present invention has technology, not high to equipment requirements, vanadium leaching yield 〉=88%, and reagent consumption is little, pollutes advantages such as few.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
(1) gets 10 tons of bone coals (containing vanadium 0.82%), pulverize, wear into 80 order powder; (2) add 765 kilograms in water, 1.7 tons of 98% industrial sulphuric acids stir, and open wide and stack 16 days; (3) add 15 tons in water, stirred 3 hours; (4) contain ferrous iron and ferric iron 4 grams per liters in the solution,, make iron reduction contained in the solution so add 240 kilograms in reductive agent Sulfothiorine; (5) adjust pH to 2.5 is heated to 30-60 ℃, filters, and obtains the filtrate of blue sulfur acid vanadium acyl.
Tailings cleans, chemical examination, and the tailings vanadiumcontent is 0.095%, the vanadium leaching yield is 88.41%.
Embodiment 2
(1) gets 10 tons of bone coals (containing vanadium 0.82%), pulverize, wear into 120 order powder; (2) add 900 kilograms in water, 2.0 tons of 98% industrial sulphuric acids stir, and open wide and stack 20 days; (3) add 20 tons in water, stirred 3.5 hours; (4) add 240 kilograms in reductive agent Sulfothiorine; (5) adjust pH to 2.5 is heated to 30 ℃, filters, and obtains blue vanadium sulfate acyl solution.
Tailings cleans, chemical examination, and the tailings vanadiumcontent is 0.082%, the vanadium leaching yield is 90.0%.
(1) gets 10 tons of bone coals (containing vanadium 0.82%), pulverize, wear into 80 order powder; (2) add 700 kilograms in water, 1.6 tons of 98% industrial sulphuric acids stir, and open wide and stack 30 days; (3) add 25 tons in water, stirred 3.5 hours; (4) add 240 kilograms in reductive agent Sulfothiorine; (5) adjust pH to 2.5 is heated to 40 ℃, filters, and obtains blue vanadium sulfate acyl solution.
Tailings cleans, chemical examination, and the tailings vanadiumcontent is 0.088%, the vanadium leaching yield is 89.27%.
Claims (5)
1. an acid hydrolysis oxidative transforms the method for extracting vanadium in the bone coal, it is characterized in that, may further comprise the steps: (1) pulverizes bone coal, wears into 60-120 order powder; (2) by stone coal powder: the vitriol oil: the weight proportion of water=100: 15-25: 6-10 adds the entry and the vitriol oil, stirs, and opens wide and stacks 16-60 days; (3) again by 1: the solid-to-liquid ratio of 1-5 adds water, stirs 1-4 hour; (4) as containing ferrous iron in the solution or/and ferric iron, then, add reductive agent according to iron-holder in the solution what, make iron reduction contained in the solution; (5) adjust pH is heated to 30-60 ℃ to 2-3, filters, and obtains the filtrate of blue sulfur acid vanadium acyl.
2. acid hydrolysis oxidative according to claim 1 transforms the method for extracting vanadium in the bone coal, it is characterized in that, in described (2) step, stone coal powder: the vitriol oil: the weight proportion of water is a stone coal powder: the vitriol oil: water=100: 16-20: 7-8.
3. acid hydrolysis oxidative according to claim 2 transforms the method for extracting vanadium in the bone coal, and it is characterized in that described stone coal powder: the vitriol oil: the weight proportion of water is a stone coal powder: the vitriol oil: water=100: 17: 7.65.
4. transform the method for extracting vanadium in the bone coal according to the described acid hydrolysis oxidative of one of claim 1-3, it is characterized in that the described vitriol oil is the industrial vitriol oil of sulfuric acid content 〉=98%.
5. transform the method for extracting vanadium in the bone coal according to the described acid hydrolysis oxidative of one of claim 1-3, it is characterized in that described pH value is 2.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101927005A CN101210287A (en) | 2007-12-24 | 2007-12-24 | Acidolysis oxidation conversion method for extracting vanadium from stone coal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101927005A CN101210287A (en) | 2007-12-24 | 2007-12-24 | Acidolysis oxidation conversion method for extracting vanadium from stone coal |
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| Publication Number | Publication Date |
|---|---|
| CN101210287A true CN101210287A (en) | 2008-07-02 |
Family
ID=39610541
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101927005A Pending CN101210287A (en) | 2007-12-24 | 2007-12-24 | Acidolysis oxidation conversion method for extracting vanadium from stone coal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787439A (en) * | 2010-03-02 | 2010-07-28 | 邓彤 | Method for recovering valuable metals from metallurgical waste |
| CN102912144A (en) * | 2012-09-12 | 2013-02-06 | 北京矿冶研究总院 | Method for leaching vanadium pentoxide from vanadium-containing soot |
| CN106282606A (en) * | 2016-08-30 | 2017-01-04 | 陕西华源矿业有限责任公司 | A kind of wet method process for extracting vanadium extracts preparation method and the facilities and equipments thereof of stock solution |
| CN106498157A (en) * | 2016-10-30 | 2017-03-15 | 武汉轻工大学 | A kind of large-scale kiln-burning extracts vanadium from high-calcium type Rock coal containing alum |
| CN111334675A (en) * | 2020-03-18 | 2020-06-26 | 西安西北有色地质研究院有限公司 | Method for extracting vanadium from low-grade stone coal vanadium ore |
-
2007
- 2007-12-24 CN CNA2007101927005A patent/CN101210287A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787439A (en) * | 2010-03-02 | 2010-07-28 | 邓彤 | Method for recovering valuable metals from metallurgical waste |
| CN102912144A (en) * | 2012-09-12 | 2013-02-06 | 北京矿冶研究总院 | Method for leaching vanadium pentoxide from vanadium-containing soot |
| CN106282606A (en) * | 2016-08-30 | 2017-01-04 | 陕西华源矿业有限责任公司 | A kind of wet method process for extracting vanadium extracts preparation method and the facilities and equipments thereof of stock solution |
| CN106498157A (en) * | 2016-10-30 | 2017-03-15 | 武汉轻工大学 | A kind of large-scale kiln-burning extracts vanadium from high-calcium type Rock coal containing alum |
| CN111334675A (en) * | 2020-03-18 | 2020-06-26 | 西安西北有色地质研究院有限公司 | Method for extracting vanadium from low-grade stone coal vanadium ore |
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