CN108315572A - A method of the Leaching Vanadium chromium from containing vanadium and chromium solid material - Google Patents
A method of the Leaching Vanadium chromium from containing vanadium and chromium solid material Download PDFInfo
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- CN108315572A CN108315572A CN201810119952.3A CN201810119952A CN108315572A CN 108315572 A CN108315572 A CN 108315572A CN 201810119952 A CN201810119952 A CN 201810119952A CN 108315572 A CN108315572 A CN 108315572A
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- Prior art keywords
- chromium
- vanadium
- leaching
- solid material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
-
- 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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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
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Abstract
The invention belongs to technical field of non-ferrous metallurgy, and in particular to a method of the Leaching Vanadium chromium from containing vanadium and chromium solid material, the characteristics of this method be will include V2O5Containing vanadium and chromium solid material, reducing agent and acid solution carry out reducing leaching reaction, obtain containing vanadium and chromium leachate through being separated by solid-liquid separation after；The present invention dexterously utilizes V2O4Compare V2O5More easily with the characteristic reacted of acid, meticulous selective reduction agent, in leaching process by V existing for surface layer in containing vanadium and chromium solid material2O5Selective reduction is at V2O4And it is reacted into solution with acid, to eliminate direct Ore Leaching process because of surface layer V2O5Presence hinder particle inside vanadium leaching, obtain faster reaction rate and higher V leaching rate；Cr (OH) simultaneously3Also it is reacted with Cr with acid3+Form enter solution, and the substances such as silicon then remain in leached mud.The present invention has technological process short, easy to operate, and vanadium chromium leaching rate is high, and advantages of environment protection is suitable for industrial applications.
Description
Technical field
The present invention relates to a kind of methods of Leaching Vanadium chromium in solid material from containing vanadium and chromium, belong to technical field of non-ferrous metallurgy.
Background technology
Vanadium is similar with chromium property, nature they preservation is in mineral usually in a manner of symbiosis, wherein v-ti magnetite
Mine is exactly the Typical Representative of this kind of mineral.The slag containing chrome alum that v-bearing titanomagnetite smelting process generates is the master for producing vanadic anhydride
Want raw material.The precipitation that will produce V containing low concentration (V) and Cr (VI) that a large amount of pH are 1.5~3.0 after this Leaching of Vanadium from Vanadium slag containing chromium is female
Reducing agent is added using the mode of reduction-neutralization in liquid, at present deposition vanadium mother liquid processing into waste water first, will be with VO2 +With
H2V10O28 4-(V) ions of V existing for form and with Cr2O7 2-Cr existing for form (VI) ion reduction is VO2+And Cr3+, mistake herein
Journey part vanadium can also be reduced to V3+, Low Valent Vanadium and chromium Precipitation are then obtained by vanadium chromium reducing slag by neutralisation treatment.Just
Vanadium is mainly with V in the vanadium chromium reducing slag of precipitation2O4Form exists, on a small quantity with Na3V(SO4)3Form exists, and chromium is mainly with Cr (OH)3
Form exist, also contain Na in slag in addition2SO4、Na2SiO3、NaNH4SO4(H2O)2With the substances such as NaCl.Phosphorous chemical industry enterprise, stone
Oily chemical enterprise etc. also will produce similar vanadium chromium reducing slag.
Patent CN106048240A discloses a kind of method of the direct Leaching Vanadium chromium reducing slag of acid solution, this method processing
New vanadium chromium reducing slag can obtain good vanadium chromium leaching rate, but for having stored up the leaching of vanadium chromium reducing slag vanadium for a long time
It is undesirable to go out effect.Hydrogen peroxide, ozone, oxygen etc. are oxidant can be oxidized to Low Valent Vanadium pentavalent vanadium simultaneously in alkaline solution
Realize the leaching of vanadium, but alkali oxide leaching process Cr (III) can also be aoxidized, vanadium chromium inferior separating effect.Vanadium chromium reducing slag its
Its mineral decomposition method has sodium roasting method, calcification baking method, sub-molten salt method etc., the common ground of these methods be all first by vanadium and
Chromium simultaneous oxidation is V (V) and Cr (VI), then separation and Extraction pentavalent vanadium and Cr VI from aqueous solution again.Due to V in solution
(V) ion is similar with Cr (VI) ionic natures, although solvent extraction, ion-exchange and electronation theoretically may be used
Precipitation method etc. carry out separation and Extraction, but no matter which kind of method all has of high cost, long flow path.
Since cost-effective Land use systems, current this containing vanadium and chromium solid material can only store up processing not yet.It is this
Autoxidation can occur in the presence of air for the Low Valent Vanadium in weakly acidic pH solid material, cause in containing vanadium and chromium solid material
Vanadium can be simultaneously with V2O5、V2O4And Na3V(SO4)3Form exist, surface layer is mainly V2O5Inside is V2O4And Na3V(SO4)3And with
The extension V of time2O5Content it is more and more.Recycling for vanadium chromium in this containing vanadium and chromium solid material, leaching process
Often one of key link only obtains high vanadium chromium leaching rate in leaching process, could be that subsequent extraction separation obtains
Necessary condition.
Invention content
Defect existing for various leaching-out techniques in for the above-mentioned prior art to the containing vanadium and chromium solid material stored up,
The purpose of the present invention is to provide a kind of method of Leaching Vanadium chromium in solid material from containing vanadium and chromium, principle is gone back based on selectivity
Original leaches vanadium chromium in containing vanadium and chromium solid material in conjunction with acid solution, and this method has vanadium chromium leaching rate height, easy to operate, at
This is low, the features such as disclosure satisfy that industrialization production requirements.
A method of the Leaching Vanadium chromium from containing vanadium and chromium solid material, which is characterized in that will include V2O5Containing vanadium and chromium solid
Material, reducing agent and acid solution carry out reducing leaching reaction, and containing vanadium and chromium leachate is obtained through being separated by solid-liquid separation after；
The reducing agent is at least one of sulfur dioxide, sulphite, thiosulfate, pyrosulfite.
The reducing leaching refer to reducing leaching reaction temperature be room temperature to 115 DEG C；The time of reducing leaching reaction
For 2~8h.
For containing V2O5Containing vanadium and chromium solid material, the present invention provides a kind of completely new leaching thinkings, i.e., described
Under reducing agent, by V in containing vanadium and chromium solid material2O5Selective reduction is at V2O4, then pass through V2O4Ore Leaching, promoted leach effect
Fruit.And the vanadium in leachate is all with VO2+And V3+Form exists, and chromium is all with Cr3+Form exists, the vanadium in this leachate
Chromium can be easy to carry out the separation and extraction of vanadium chromium.
Preferably, the containing vanadium and chromium solid material, which is superficial deposit, V2O5Vanadium chromium reducing slag.
Preferably, the containing vanadium and chromium solid material is in vanadium chromium reducing slag stacking process, surface layer Low Valent Vanadium material warp
Air oxidation is at V2O5Material.
The method of the present invention is applicable to any V2O5The containing vanadium and chromium solid material of content, especially suitable for V2O5Content is higher
Containing vanadium and chromium solid material.
Preferably, in containing vanadium and chromium solid material, V2O5Content is not less than 1.6wt%；Further preferably 1.6~
3.8wt%.
The present invention dexterously utilizes V2O4Compare V2O5The characteristic more easily reacted with acid is being leached by the reducing agent
Process is by V existing for surface layer in containing vanadium and chromium solid material2O5Selective reduction is at V2O4And it is reacted into solution with acid, to disappear
Except direct Ore Leaching process because of surface layer V2O5Presence hinder the leaching of vanadium inside particle, obtain faster reaction rate and more
High V leaching rate.
In industrial applications, sulphite is preferably sodium sulfite, and thiosulfate is preferably sodium thiosulfate, Jiao Ya
Sulfate is preferably sodium pyrosulfite.
Preferably, the reducing agent addition amount is V in containing vanadium and chromium solid material2O5It is reduced to V2O4The 1 of theoretical amount~
2.0 again.
Preferably, the acid solution is the solution of a concentration of 5~12mol/L of H+.
Preferably, the H+ in the acid solution is provided by least one of sulfuric acid, hydrochloric acid, phosphoric acid.
Add according to 1: 1.1~6g/mL of solid-to-liquid ratio preferably, the acid solution addition is containing vanadium and chromium solid material and acid solution
Enter acid solution.
The present invention compared with the prior art has the following advantages and effect：
V2O5It is a kind of amphoteric oxide, but based on acidity, is soluble in alkali, is difficult then dissolving in an acidic solution.It is right
In surface layer with V2O5Based on vanadium chromium reducing slag hinder V inside solid particle in Ore Leaching process2O4With acid react and
Na3V(SO4)3Dissolution.V2O4It is also amphiprotic substance, but it is soluble in bronsted lowry acids and bases bronsted lowry simultaneously, the present invention is exactly dexterously to utilize
V2O4Compare V2O5More easily with the characteristic reacted of acid, meticulous selective reduction agent, leaching process will be in containing vanadium and chromium solid material
V2O5Selective reduction is at V2O4And it is reacted into solution with acid；Cr (OH) simultaneously3Also it is reacted with Cr with acid3+Form enter it is molten
Liquid, and the substances such as silicon then remain in leached mud.The present invention has technological process short, easy to operate, and vanadium chromium leaching rate is high, environment
The advantages that friendly, is suitable for industrial applications.
V2O5+2e+2H+→V2O4+H2O
V2O4+4H+→2VO2++2H2O
Cr(OH)3+3H+→Cr3++3H2O
Na3V(SO4)3→3Na++V3++3SO4 2-
Na2SO4→2Na++SO4 2-
Na2SiO3+2H+→2Na++H2SiO3↓
NaNH4SO4(H2O)2→Na++NH4 ++SO4 2-+2H2O
NaCl→Na++C1-
The study found that the leaching thinking innovated using the present invention, V leaching rate is higher than 99%；Especially for five oxidations two
The higher containing vanadium and chromium solid material of content of vanadium, effect become apparent from；Leaching rate can lift up to 20% or more, be led in nonferrous smelting
Domain, effect protrude.
Specific implementation mode
With reference to embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than it is right
The present invention's further limits.
Embodiment 1
Take (the wherein V containing 6.3wt%V2O5Content is 3.8wt%) and 28.2wt%Cr (OH)3Containing vanadium and chromium solid material
The H of 2.5mol/L is added by solid-to-liquid ratio 1: 6g/ml by 500g2SO4Solution is reduced to four according to pentavalent vanadium in containing vanadium and chromium solid material
1.2 times of valence vanadium theoretical amount addition sodium sulfites, leaching 4h at 100 DEG C, solid-liquor separation.V leaching rate is 99.5%, chromium
Leaching rate is 99.7%.
Comparative example 1
Relative to embodiment 1, this comparative example is inquired into, do not use the present invention claims reducing leaching technique, it is specific as follows：
Take (the wherein V containing 6.3wt%V2O5Content is 3.8wt%) and 28.2wt%Cr (OH)3Containing vanadium and chromium solid material
The H of 2.5mol/L is added by solid-to-liquid ratio 1: 6g/ml by 500g2SO4Solution, leaching 4h at 100 DEG C, solid-liquor separation.Vanadium leaches
Rate is 78.2%, and chromium leaching rate is 99.8%.
Embodiment 2
Take (the wherein V containing 4.1wt%V2O5Content is 1.6wt%) and 20.0wt%Cr (OH)3Containing vanadium and chromium solid material
The HCl solution of 6mol/L is added by solid-to-liquid ratio 1: 5g/mL, tetravalence is reduced to according to pentavalent vanadium in containing vanadium and chromium solid material by 1000g
1.5 times of vanadium theoretical amount addition sodium thiosulfate, leaching 5h at 105 DEG C, solid-liquor separation.V leaching rate is 99.1%, chromium
Leaching rate is 99.6%.
Comparative example 2
Relative to embodiment 2, this comparative example is inquired into, do not use the present invention claims reducing leaching technique, it is specific as follows：
Take (the wherein V containing 4.1wt%V2O5Content is 1.6wt%) and 20.0wt%Cr (OH)3Containing vanadium and chromium solid material
The HCl solution of 6mol/L is added by solid-to-liquid ratio 1: 5g/mL by 1000g, leaching 5h at 105 DEG C, solid-liquor separation.V leaching rate
It is 89.5%, chromium leaching rate is 99.5%.
Embodiment 3
Take (the wherein V containing 7.1wt%V2O5Content is 2.9wt%) and 3.57wt%Cr (OH)3Containing vanadium and chromium solid material
The H of 6mol/L is added by solid-to-liquid ratio 1: 4g/mL by 500g2SO4Solution is reduced to tetravalence according to pentavalent vanadium in containing vanadium and chromium solid material
1.3 times of vanadium theoretical amount addition sodium pyrosulfites, leaching 6h at 105 DEG C, solid-liquor separation.V leaching rate is 99.3%, chromium
Leaching rate is 98.8%.
Embodiment 4
Take (the wherein V containing 7.1wt%V2O5Content is 2.9wt%) and 3.57wt%Cr (OH)3Containing vanadium and chromium solid material
The H of 6mol/L is added by solid-to-liquid ratio 1: 4g/mL by 500g2SO4Solution is reduced to tetravalence according to pentavalent vanadium in containing vanadium and chromium solid material
1.1 times of vanadium theoretical amount are passed through sulfur dioxide, at room temperature leaching 2h, solid-liquor separation.V leaching rate is 99.2%, and chromium leaches
Rate is 98.5%.
To sum up embodiment and comparative example is found, is carried out reducing leaching reaction using technical solution of the present invention, can be obviously improved
The leaching rate of vanadium chromium can effectively solve containing vanadium and chromium solid material because surface autoxidation forms V2O5Caused by V leaching rate
The leaching rate of vanadium can be promoted to 99% or more, to containing vanadium and chromium solid by low technical problem, technical solution through the invention
The solid wastes recycling of material utilizes and field of environment protection is in solid waste resource reclaim, field of environment protection, has broad prospect of application.
Claims (10)
1. a kind of method of Leaching Vanadium chromium in solid material from containing vanadium and chromium, which is characterized in that will include V2O5Containing vanadium and chromium solids
Material, reducing agent and acid solution carry out reducing leaching reaction, and containing vanadium and chromium leachate is obtained through being separated by solid-liquid separation after；
The reducing agent is at least one of sulfur dioxide, sulphite, thiosulfate, pyrosulfite.
2. as described in claim 1 from containing vanadium and chromium solid material Leaching Vanadium chromium method, which is characterized in that it is described to contain vanadium
Chromium solid material, which is superficial deposit, V2O5Vanadium chromium reducing slag.
3. as claimed in claim 1 or 2 from containing vanadium and chromium solid material Leaching Vanadium chromium method, which is characterized in that containing vanadium and chromium
In material, V2O5Content is not less than 1.6wt%.
4. as described in claim 1 from containing vanadium and chromium solid material Leaching Vanadium chromium method, which is characterized in that the sulfurous
Hydrochlorate is sodium sulfite；
The thiosulfate is sodium thiosulfate；
The pyrosulfite is sodium pyrosulfite.
5. the method for Leaching Vanadium chromium in the solid material as described in claim 1 or 4 from containing vanadium and chromium, which is characterized in that described to go back
Former agent addition is V in containing vanadium and chromium solid material2OsIt is reduced to V2O41~2.0 times of theoretical amount.
6. as described in claim 1 from containing vanadium and chromium solid material Leaching Vanadium chromium method, which is characterized in that the acid solution is
H+The solution of a concentration of 5~12mol/L.
7. as claimed in claim 6 from containing vanadium and chromium solid material Leaching Vanadium chromium method, which is characterized in that in the acid solution
H+It is provided by least one of sulfuric acid, hydrochloric acid, phosphoric acid.
8. the method for Leaching Vanadium chromium in slave containing vanadium and chromium solid material as claimed in claims 6 or 7, which is characterized in that the acid
Liquid addition is that acid solution is added according to 1: 1.1~6g/mL of solid-to-liquid ratio in containing vanadium and chromium solid material and acid solution.
9. as described in claim 1 from containing vanadium and chromium solid material Leaching Vanadium chromium method, which is characterized in that reducing leaching is anti-
The temperature answered is room temperature to 115 DEG C.
10. as claimed in claim 9 from containing vanadium and chromium solid material Leaching Vanadium chromium method, which is characterized in that reducing leaching
The time of reaction is 2~8h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810119952.3A CN108315572A (en) | 2018-02-05 | 2018-02-05 | A method of the Leaching Vanadium chromium from containing vanadium and chromium solid material |
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| CN201810119952.3A CN108315572A (en) | 2018-02-05 | 2018-02-05 | A method of the Leaching Vanadium chromium from containing vanadium and chromium solid material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358920A (en) * | 2019-07-31 | 2019-10-22 | 武汉科技大学 | A method of separating vanadium from vanadium chromium waste residue |
| CN111876615A (en) * | 2020-07-10 | 2020-11-03 | 武汉科技大学 | Method for separating vanadium and molybdenum from high-chromium waste residue |
| CN114231732A (en) * | 2021-12-20 | 2022-03-25 | 攀枝花市阳润科技有限公司 | Method for deeply extracting vanadium from vanadium-containing slurry |
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| CN111876615A (en) * | 2020-07-10 | 2020-11-03 | 武汉科技大学 | Method for separating vanadium and molybdenum from high-chromium waste residue |
| CN111876615B (en) * | 2020-07-10 | 2022-07-05 | 武汉科技大学 | Method for separating vanadium and molybdenum from high-chromium waste residue |
| CN114231732A (en) * | 2021-12-20 | 2022-03-25 | 攀枝花市阳润科技有限公司 | Method for deeply extracting vanadium from vanadium-containing slurry |
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