CN106395899A - Method for preparing vanadyl sulfate by use of vanadium-containing chloride solution - Google Patents
Method for preparing vanadyl sulfate by use of vanadium-containing chloride solution Download PDFInfo
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- CN106395899A CN106395899A CN201610849570.7A CN201610849570A CN106395899A CN 106395899 A CN106395899 A CN 106395899A CN 201610849570 A CN201610849570 A CN 201610849570A CN 106395899 A CN106395899 A CN 106395899A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to the field of wet-process metallurgy and particularly relates to a method for preparing vanadyl sulfate by use of a vanadium-containing chloride solution. The method comprises the following steps: 1) heating and reducing the vanadium-containing chloride solution, thereby obtaining a reduction solution; 2) regulating the pH value of the reduction solution to 0-2; 3), performing extraction, thereby obtaining a vanadium-loaded organic phase; 4) performing reverse extraction, thereby obtaining a vanadium solution; 5) regulating the pH value of the vanadium solution to 1-3; 6) extracting the solution, thereby obtaining the vanadium-loaded organic phase; 7) performing reverse extraction, thereby obtaining a vanadyl sulfate solution; and 8) absorbing the vanadyl sulfate solution by use of an adsorbent, thereby obtaining a vanadyl sulfate solution final product. According to the method, HCl leaching liquid containing vanadium resources, such as titaniferous magnetite and an SCR dead catalyst are utilized as raw materials, and an extraction-reverse extraction-deep impurity removal method is adopted, so that the method provided by the invention is capable of directly preparing high-purity anadyl sulfate from the vanadium-containing chloride solution, and has the advantages of short process and low cost.
Description
Technical field
The invention belongs to field of hydrometallurgy, in particular it relates to one kind prepares high-purity sulphuric acid from chloride solution containing vanadium
The method of vanadyl.
Background technology
All-vanadium flow redox cell (all vanadium redox flow battery) has long service life,
Charge and discharge system flexibly, can high current depth discharge and recharge, many advantages, such as no cross contamination and energy loss, can be applicable to peak regulation
Power-supply system, extensive photo-translating system, wind energy utilization system, uninterrupted power source and the aspect such as emergency power supply, electric power system,
It is considered as the green energy-storing battery of most application prospect.All-vanadium flow redox cell is mainly by electrode, electrolyte, electricity
Pond barrier film, reservoir, pile etc. form；Vanadium oxysulfate is the important component part of electrolyte, of great interest.
Traditional vanadium oxysulfate is prepared with high purity vanadic anhydride as raw material, and its technological process is：High purity vanadic anhydride sulfur
Sour dissolving → reduction → evaporative crystallization → dehydration is obtained light blue vanadium oxysulfate powder.This technical process adopts high-purity five oxidations
Two vanadium are raw material, high cost；Need to add reducing agent after high purity vanadic anhydride dissolving, introduce foreign ion, impact product is pure
Degree.
Content of the invention
It is an object of the invention to provide a kind of method preparing high-purity sulphuric acid vanadyl from chloride solution containing vanadium, the party
The selectivity efficient that method is capable of vanadium separates, and preparation process does not introduce new impurity, does not produce vanadium loss, process is simple, stream
Journey is short, vanadium extraction yield high, low cost, and extractant can recycle after back extraction.
The method preparing vanadium oxysulfate from chloride solution containing vanadium of the present invention, comprises the following steps：
1) vanadium chloride solution will be contained and be heated to 30～90 DEG C, stirring, add reducing agent to be reduced to vanadium in solution (V)
Vanadium (IV), ferrum (III) is reduced to ferrum (II), filters, and obtains reducing solution；
2) by step 1) pH value of reducing solution that obtains adjusts to 0～2, filters；
3) by step 2) solution is mixed with extractant and is extracted after the filtration that obtains, obtains load vanadium organic faciess；
4) by step 3) the load vanadium organic faciess that obtain carry out back extraction using acid solution, obtain vanadium solution；
5) by step 4) pH value of vanadium solution that obtains adjusts to 1～3, filters；
6) by step 5) solution is mixed with extractant and is extracted after the filtration that obtains, obtains load vanadium organic faciess；
7) by step 6) obtain load vanadium organic faciess carry out back extraction using acid solution, obtain oxygen vanadium sulphate solution；
8) by step 7) obtain oxygen vanadium sulphate solution and adsorbed using adsorbent, by oxygen vanadium sulphate solution surface residual
Organic matter removal, prepared oxygen vanadium sulphate solution end-product.
The concept that chloride solution containing vanadium of the present invention is known in the art, anions with chloride ion are mainly
Main, and in solution, contain vanadium.Chloride solution containing vanadium is mainly vanadium titano-magnetite, SCR dead catalyst etc. and contains vanadium resource through hydrochloric acid
The solution obtaining after leaching.
The method according to the invention, wherein preferably, step 1) described reducing agent is in sodium sulfite, iron powder or oxalic acid
A kind of.
The method according to the invention, wherein, step 2) according to step 1) obtain the pH value of reducing solution, from suitable substance
Adjust its pH value to 0～2.When step 2) adjust pH value used by material be alkaline matter when, described alkaline matter can select
NaOH、Na2CO3, ammonia, CaCO3Or Ca (OH)2One of；When material used by regulation pH value is acidic materials, described acid
Property material select hydrochloric acid or sulphuric acid.
The method according to the invention, wherein, step 3) mixed solvent for P204, TBP and normal heptane for the described extractant；Or
P204, TBP and the mixed solvent of kerosene；Or the mixed solvent of P507, TBP and normal heptane；Or the mixing of P507, TBP and kerosene
Solvent.
The consumption of described extractant is O/A (volume ratio)=1:6～6:1.Wherein, preferably, described P204 or
The amount ranges of P507 are 5%～40% (accounting for the volume fraction of extractant), and the amount ranges of TBP (account for extraction for 5%～15%
The volume fraction of agent), the amount ranges of kerosene or normal heptane are 55%～90% (accounting for the volume fraction of extractant).
The method according to the invention, wherein, step 4) described acid solution be mass fraction 10%～40% dilute sulfuric acid molten
Liquid, consumption is O/A (volume ratio) is 1:3～8:1.Preferably use top pure grade sulphuric acid.
The method according to the invention, wherein, step 5) material used by pH value that adjusts vanadium solution is alkaline matter, described alkali
Property material be NaOH, Na2CO3One of or ammonia.
The method according to the invention, wherein, step 6) mixed solvent for P204, TBP and normal heptane for the described extractant；Or
P204, TBP and the mixed solvent of kerosene；Or the mixed solvent of P507, TBP and normal heptane；Or the mixing of P507, TBP and kerosene
Solvent.
The consumption of described extractant is O/A (volume ratio)=1:6～6:1.Wherein, preferably, described P204 or
The amount ranges of P507 are 5%～40% (accounting for the volume fraction of extractant), and the amount ranges of TBP (account for extraction for 5%～15%
The volume fraction of agent), the amount ranges of kerosene or normal heptane are 55%～90% (accounting for the volume fraction of extractant).
The method according to the invention, wherein, step 7) described acid solution is the dilute sulfuric acid of mass fraction 10%～40%, uses
Amount is O/A (volume ratio) is 1:3～8:1.Preferably use top pure grade sulphuric acid.
The method according to the invention, wherein preferably, by step 7) be obtained oxygen vanadium sulphate solution return to step 3), repeat
Step 3) -7), carry out extracting-back extraction 4～6 times, obtain oxygen vanadium sulphate solution.
The method according to the invention, wherein, step 8) but described adsorbent can be absorption that is known in this field using
Agent, such as preferably activated carbon.
V content >=1.5mol/L in the oxygen vanadium sulphate solution that the application present invention prepares, impurity content≤200ppm, belong to
High-purity sulphuric acid vanadyl solution.
The present invention with hydrochloric acid leachate containing vanadium resource such as vanadium titano-magnetite, SCR dead catalyst as raw material, using extraction-anti-
The method of extraction-deep impurity-removing, the method direct preparation of high-purity vanadium oxysulfate from chloride solution containing vanadium, it is short to have a flow process, becomes
This low advantage.
It is an advantage of the current invention that：
(1) method that high-purity sulphuric acid vanadyl is prepared in present invention proposition from chloride solution containing vanadium, it is to avoid traditional preparation
The problems such as high-purity sulphuric acid vanadyl process high energy consumption, three-waste pollution are serious, vanadium recovery is not high, product quality is high.
(2) method preparing high-purity sulphuric acid vanadyl proposed by the present invention, the response rate of vanadium is high, product quality is high, and impurity contains
Amount is low.
Brief description
Fig. 1 prepares the process chart of the method for vanadium oxysulfate from chloride solution containing vanadium for the present invention.
Specific embodiment
The present invention is expanded on further by the following examples, these embodiments are only used for the purpose illustrating, not
Limit the scope of the present invention.The test method of unreceipted actual conditions in the following example, generally according to normal condition.
Embodiment 1
Main component containing vanadium chloride solution is：V content is 8.3g/L, and Fe content is 78.7g/L, and Ca content is
17.4g/L, Mg content is 1.1g/L, and Al content is 9.4g/L；
1) solution is heated to 30 DEG C, stirring, add iron powder reducing, V in solution (V) is reduced to V (IV), Fe (III)
It is reduced to Fe (II), filters, obtain reducing solution；
2) by step 1) obtain reducing solution and utilize Na2CO3Adjust reducing solution pH value to 0.5, filter；
3) by step 2) obtain the mixing extraction of solution and P507, TBP and kerosene (volume ratio is respectively 5%, 5%, 90%)
Agent mixing is taken to be extracted, O/A=2:1, obtain load vanadium organic faciess；
4) by step 3) obtain load vanadium organic faciess carry out back extraction, O/A=1 using 10% sulfuric acid solution:1, obtain vanadium molten
Liquid；
5) by step 4) vanadium solution that obtains utilizes ammonia to adjust vanadium solution pH value to 1.2, filters；
6) by step 5) solution and P507, TBP and kerosene (volume ratio is respectively 5%, 5%, 90%) after the filtration that obtains
Mixed extractant mixing extracted, O/A=1:4, obtain load vanadium organic faciess；
7) by step 6) obtain load vanadium organic faciess carry out back extraction, O/A=5 using 20% sulfuric acid solution:1, obtain vanadium molten
Liquid, by vanadium solution return to step 3), repeat step 3) -7), such extracting-back extraction 4 times, complete extraction process；
8) by step 7) obtain the organic faciess that oxygen vanadium sulphate solution utilizes activated carbon adsorption oxygen vanadium sulphate solution surface residual,
Preparation becomes high-purity oxygen vanadium sulphate solution, wherein V content 75g/L, Fe content 8.4mg/L, Al content 7.3mg/L, Ca content
5.6mg/L.
Embodiment 2
Main component containing vanadium chloride solution is：V content is 15.3g/L, and Fe content is 14.7g/L, and Ca content is
5.3g/L, Mg content is 4.1g/L, and Al content is 3.4g/L；
1) solution is heated to 90 DEG C, stirring, add sodium sulfite reduction, V in solution (V) is reduced to V (IV), Fe
(III) it is reduced to Fe (II), filters, obtain reducing solution；
2) by step 1) obtain reducing solution using hydrochloric acid material regulation reducing solution pH value to 1.1；
3) by step 2) filtered after solution and P507, TBP and normal heptane (volume ratio is respectively 25%, 15%,
60%) mixed extractant mixing is extracted, O/A=1:2, obtain load vanadium organic faciess；
4) by step 3) obtain load vanadium organic faciess carry out back extraction, O/A=1 using 20% sulfuric acid solution:1, obtain vanadium molten
Liquid；
5) by step 4) vanadium solution that obtains utilizes ammonia to adjust vanadium solution pH value to 2.4, filters；
6) by step 5) solution and P507, TBP and normal heptane after the filtration that obtains (volume ratio is respectively 25%, 15%,
60%) mixed extractant mixing is extracted, O/A=2:1, obtain load vanadium organic faciess；
7) by step 6) obtain load vanadium organic faciess carry out back extraction, O/A=5 using 20% sulfuric acid solution:1, obtain vanadium molten
Liquid, by vanadium solution return to step 3), repeat step 3) -7), such extracting-back extraction 5 times, complete extraction process；
8) by step 7) obtain the organic faciess that oxygen vanadium sulphate solution utilizes activated carbon adsorption oxygen vanadium sulphate solution surface residual,
Preparation becomes high-purity oxygen vanadium sulphate solution, wherein V content 68g/L, Fe content 5.1mg/L, Al content 4.3mg/L.
Embodiment 3
Main component containing vanadium chloride solution is：V content is 3.5g/L, and Fe content is 0.3g/L, and Ca content is 3.1g/
L, Al content is 2.7g/L；
1) vanadium chloride solution will be contained and be heated to 60 DEG C, stirring, add sodium sulfite reduction, V in solution (V) is reduced
For V (IV), Fe (III) is reduced to Fe (II), filters, and obtains reducing solution；
2) by step 1) obtain reducing solution using Calcium Carbonate regulation reducing solution pH value to 2；
3) by step 2) filtered after solution and P204, TBP and normal heptane (volume ratio is respectively 40%, 5%, 55%)
Mixed extractant mixing extracted, O/A=1:4, obtain load vanadium organic faciess；
4) by step 3) obtain load vanadium organic faciess carry out back extraction, O/A=1 using 40% sulfuric acid solution:1, obtain vanadium molten
Liquid；
5) by step 4) vanadium solution that obtains utilizes ammonia to adjust vanadium solution pH value to 3, filters；
6) by step 5) solution and P204, TBP and normal heptane after the filtration that obtains (volume ratio is respectively 40%, 5%,
55%) mixed extractant mixing is extracted, O/A=1:1, obtain load vanadium organic faciess；
7) by step 6) obtain load vanadium organic faciess carry out back extraction, O/A=6 using 40% sulfuric acid solution:1, obtain vanadium molten
Liquid, by vanadium solution return to step 3), repeat step 3) -7), such extracting-back extraction 6 times, complete extraction process；
8) by step 7) obtain the organic faciess that oxygen vanadium sulphate solution utilizes activated carbon adsorption oxygen vanadium sulphate solution surface residual,
Preparation becomes high-purity oxygen vanadium sulphate solution, wherein V content 80g/L, Fe content 4.6mg/L, Al content 3.1mg/L.
Certainly, the present invention can also have various embodiments, in the case of without departing substantially from present invention spirit and its essence, is familiar with
Those skilled in the art can according to disclosure of the invention make various corresponding change and deform, but these corresponding change and
Deformation all should belong to the scope of the claims of the present invention.
Claims (10)
1. a kind of method preparing vanadium oxysulfate from chloride solution containing vanadium, comprises the following steps：
1) vanadium chloride solution will be contained and be heated to 30～90 DEG C, and add reducing agent that vanadium in solution (V) is reduced to vanadium (IV), ferrum
(III) it is reduced to ferrum (II), filters, obtain reducing solution；
2) by step 1) pH value of reducing solution that obtains adjusts to 0～2, filters；
3) by step 2) solution is mixed with extractant and is extracted after the filtration that obtains, obtains load vanadium organic faciess；
4) by step 3) the load vanadium organic faciess that obtain carry out back extraction using acid solution, obtain vanadium solution；
5) by step 4) pH value of vanadium solution that obtains adjusts to 1～3, filters；
6) by step 5) solution is mixed with extractant and is extracted after the filtration that obtains, obtains load vanadium organic faciess；
7) by step 6) obtain load vanadium organic faciess carry out back extraction using acid solution, obtain oxygen vanadium sulphate solution；
8) by step 7) obtain oxygen vanadium sulphate solution and adsorbed using adsorbent, oxygen vanadium sulphate solution surface residual is organic
Thing removes, prepared oxygen vanadium sulphate solution end-product.
2. method according to claim 1 is it is characterised in that step 1) described reducing agent is sodium sulfite, iron powder or grass
One of acid.
3. method according to claim 1 is it is characterised in that step 2) to adjust material used by pH value be alkaline matter, institute
Stating alkaline matter is NaOH, Na2CO3, ammonia, CaCO3Or Ca (OH)2One of；Or, adjusting material used by pH value is acid
Property material, described acidic materials be hydrochloric acid or sulphuric acid.
4. method according to claim 1 is it is characterised in that step 3) described extractant is P204, TBP and normal heptane
Mixed solvent；Or the mixed solvent of P204, TBP and kerosene；Or the mixed solvent of P507, TBP and normal heptane；Or P507, TBP and
The mixed solvent of kerosene；Preferably, the consumption of extractant is O/A=1:6～6:1.
5. method according to claim 1 is it is characterised in that step 4) described acid solution is dilution heat of sulfuric acid, as excellent
Selection of land, the addition of described dilution heat of sulfuric acid is O/A=1:3～8:1.
6. method according to claim 1 is it is characterised in that step 5) material used by pH value that adjusts vanadium solution is alkalescence
Material, described alkaline matter is NaOH, Na2CO3One of or ammonia.
7. method according to claim 1 is it is characterised in that step 6) described extractant is P204, TBP and normal heptane
Mixed solvent；Or the mixed solvent of P204, TBP and kerosene；Or the mixed solvent of P507, TBP and normal heptane；Or P507, TBP and
The mixed solvent of kerosene；Preferably, the consumption of extractant is O/A=1:6～6:1.
8. method according to claim 1 is it is characterised in that step 7) described acid solution is dilution heat of sulfuric acid, as excellent
Selection of land, the addition of described dilution heat of sulfuric acid is O/A=1:3～8:1.
9. according to the arbitrary described method of claim 1-8 it is characterised in that by step 7) oxygen vanadium sulphate solution that is obtained returns
Step 3), repeat step 3) -7), carry out extracting-back extraction 4～6 times, obtain oxygen vanadium sulphate solution.
10. method according to claim 1 is it is characterised in that step 8) described adsorbent is activated carbon.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108211420A (en) * | 2018-01-17 | 2018-06-29 | 大连博融新材料有限公司 | The extraction preparation process of high-purity sulphuric acid vanadyl solution |
| CN108217726A (en) * | 2018-04-12 | 2018-06-29 | 四川星明能源环保科技有限公司 | A kind of high-purity ammonium vanadate and preparation method thereof |
| CN108314082A (en) * | 2018-02-07 | 2018-07-24 | 四川星明能源环保科技有限公司 | A method of high-purity sulphuric acid vanadyl solution is prepared based on raw material containing vanadium leachate |
| CN108336426A (en) * | 2018-02-07 | 2018-07-27 | 四川星明能源环保科技有限公司 | The preparation method and its oxygen vanadium sulfate crystals obtained of a kind of vanadic sulfate |
| CN108394934A (en) * | 2018-04-12 | 2018-08-14 | 四川星明能源环保科技有限公司 | A kind of V electrolyte high-purity oxyvanadium compound and preparation method thereof |
| CN108423712A (en) * | 2018-04-12 | 2018-08-21 | 四川星明能源环保科技有限公司 | Vanadium trioxide and preparation method thereof |
| CN110066929A (en) * | 2019-04-26 | 2019-07-30 | 广东省稀有金属研究所 | A kind of preparation method of oxygen vanadium sulphate solution |
| CN113186395A (en) * | 2021-04-13 | 2021-07-30 | 四川星明能源环保科技有限公司 | Method for preparing vanadyl sulfate from vanadium-containing solution |
| CN114349048A (en) * | 2021-11-25 | 2022-04-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadyl sulfate solution by recycling titanium tetrachloride refining tailings |
| CN115477326A (en) * | 2022-09-02 | 2022-12-16 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadyl sulfate solution from industrial vanadium slag calcification roasting pickle liquor |
| RU2807979C1 (en) * | 2021-11-25 | 2023-11-21 | Паньган Груп Паньчжихуа Айрон & Стил Рисерч Инститьют Ко., Лтд. | Method of preparing highly purific solution of vanadyl sulphate from purified titanium tetrachloride sludge |
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| CN105428681A (en) * | 2015-12-30 | 2016-03-23 | 王晓伟 | Remelting type reduction preparation method for vanadyl sulfate electrolyte |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105428681A (en) * | 2015-12-30 | 2016-03-23 | 王晓伟 | Remelting type reduction preparation method for vanadyl sulfate electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108211420B (en) * | 2018-01-17 | 2020-06-16 | 大连博融新材料有限公司 | Extraction preparation process of high-purity vanadyl sulfate solution |
| CN108211420A (en) * | 2018-01-17 | 2018-06-29 | 大连博融新材料有限公司 | The extraction preparation process of high-purity sulphuric acid vanadyl solution |
| CN108314082A (en) * | 2018-02-07 | 2018-07-24 | 四川星明能源环保科技有限公司 | A method of high-purity sulphuric acid vanadyl solution is prepared based on raw material containing vanadium leachate |
| CN108336426A (en) * | 2018-02-07 | 2018-07-27 | 四川星明能源环保科技有限公司 | The preparation method and its oxygen vanadium sulfate crystals obtained of a kind of vanadic sulfate |
| CN108217726A (en) * | 2018-04-12 | 2018-06-29 | 四川星明能源环保科技有限公司 | A kind of high-purity ammonium vanadate and preparation method thereof |
| CN108394934A (en) * | 2018-04-12 | 2018-08-14 | 四川星明能源环保科技有限公司 | A kind of V electrolyte high-purity oxyvanadium compound and preparation method thereof |
| CN108423712A (en) * | 2018-04-12 | 2018-08-21 | 四川星明能源环保科技有限公司 | Vanadium trioxide and preparation method thereof |
| CN110066929A (en) * | 2019-04-26 | 2019-07-30 | 广东省稀有金属研究所 | A kind of preparation method of oxygen vanadium sulphate solution |
| CN113186395A (en) * | 2021-04-13 | 2021-07-30 | 四川星明能源环保科技有限公司 | Method for preparing vanadyl sulfate from vanadium-containing solution |
| CN114349048A (en) * | 2021-11-25 | 2022-04-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadyl sulfate solution by recycling titanium tetrachloride refining tailings |
| WO2023093046A1 (en) * | 2021-11-25 | 2023-06-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadyl sulfate solution from recovered titanium tetrachloride refining tailings |
| RU2807979C1 (en) * | 2021-11-25 | 2023-11-21 | Паньган Груп Паньчжихуа Айрон & Стил Рисерч Инститьют Ко., Лтд. | Method of preparing highly purific solution of vanadyl sulphate from purified titanium tetrachloride sludge |
| CN114349048B (en) * | 2021-11-25 | 2024-03-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadyl sulfate solution by recycling titanium tetrachloride refined tailings |
| CN115477326A (en) * | 2022-09-02 | 2022-12-16 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadyl sulfate solution from industrial vanadium slag calcification roasting pickle liquor |
| CN115477326B (en) * | 2022-09-02 | 2024-01-26 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadyl sulfate solution by industrial vanadium slag calcification roasting pickle liquor |
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