CN104477992A - Method for preparing vanadium pentoxide - Google Patents
Method for preparing vanadium pentoxide Download PDFInfo
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- CN104477992A CN104477992A CN201510005668.XA CN201510005668A CN104477992A CN 104477992 A CN104477992 A CN 104477992A CN 201510005668 A CN201510005668 A CN 201510005668A CN 104477992 A CN104477992 A CN 104477992A
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- C01—INORGANIC CHEMISTRY
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- C01G31/00—Compounds of vanadium
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Abstract
The invention relates to a method for preparing vanadium pentoxide and belongs to the field of fine chemical engineering. The purpose of preparation of the vanadium pentoxide is achieved. The method includes the following steps of a, re-dissolution, b, crystallization, c, water addition for dissolution, d, vanadium settlement, and e, calcination, wherein in the re-dissolution step, ammonium polyorthovanadate is dissolved in a sodium hydroxide solution, so that a re-dissolution solution is acquired; in the crystallization step, the re-dissolution solution stands still for 20 h to 40 h at the indoor temperature and filtered, filtrate is acquired and stands at the temperature from 2 DEG C to 5 DEC G so as to be crystallized, and sodium metavanadate solid is acquired; in the step of water addition for dissolution, water is added to the sodium metavanadate solid for dissolution, so that a dissolved solution is acquired; in the vanadium settlement step, ammonium sulfate or ammonium sulfate is added to the dissolved solution, a reaction is conducted at the temperature from 45 DEG C to 65 DEG C for 0.5 h to 2 h, the solution is filtered, and ammonium metavanadate solid is acquired; in the calcination step, the ammonium metavanadate solid is calcined, so that vanadium pentoxide is acquired. According to the method, the vanadium pentoxide with high purity can be obtained, the process is simple, and operation is convenient; in the preparation process, vanadium pentoxide can be prepared by adding a small amount of sodium hydroxide and ammonium salt, raw materials are saved, and the method accords with the industrial policies of energy conservation and emission reduction.
Description
Technical field
The present invention relates to the preparation method of Vanadium Pentoxide in FLAKES, belong to field of fine chemical.
Background technology
High purity vanadic anhydride refers on the basis of common Vanadium Pentoxide in FLAKES GB3283-87 standard, to reduce in vanadium the foreign matter contents such as silicon, phosphorus, iron, calcium, magnesium, chromium, aluminium, nickel, potassium, sodium and makes it lower than GB limit value (lower than 0.005%).Because country does not formulate high standard, so be high purity vanadic anhydride higher than the Vanadium Pentoxide in FLAKES of GB purity.The high purity vanadic anhydride that the present invention defines refer to purity be more than or equal to 99.9% Vanadium Pentoxide in FLAKES.
In fine chemistry industry, high purity vanadic anhydride may be used for that the catalyzer of organic synthesis, desulfurization are out of stock, sulfuric acid preparation, high-purity sulphuric acid vanadyl, high-purity sulphuric acid vanadium etc.In metallurgical, high purity vanadic anhydride can meet the purity requirement of vananum to starting material Vanadium Pentoxide in FLAKES, also can be used for producing vanadium nitrogen, vanadium iron nitrogen, ferro-vanadium.In nuclear industry: high purity vanadic anhydride may be used for producing high purity metal vanadium.In battery industry, high purity vanadic anhydride can positive electrode material, the vanadium flow battery of synthesizing lithium ion battery.Visible, the application potential of high purity vanadic anhydride is huge.
At present, the preparation method of high purity vanadic anhydride is generally following several.
First: multi-stage solvent extraction-ion exchange resin impurity removal method, this fado is used for extracting vanadium from stone coal, and the method is grey for raw material with the bone coal containing vanadium.
Second: colloidal precipitation method: with the ammonium poly-vanadate of metallurgical grade for raw material, prepare vananum high purity vanadic anhydride.This method mainly utilizes Tai-Ace S 150 in vanadium solution (pH=8 ~ 11), forms precipitation, the impurity in removing vanadium solution, mainly sila matter.The shortcoming of this method is, removes silicon, but introduces aluminium in solution, aluminium contaminant overstandard in the Vanadium Pentoxide in FLAKES causing this method to be produced.But high purity vanadic anhydride prepared by the method may be used for producing vananum, makes the method still have certain market.
3rd: " alkali returns molten-acid, and heavy-alkali returns molten-precipitation-calcining " five-step approach, see patent 201210488566.The method with the ammonium poly-vanadate of metallurgical grade or ammonium meta-vanadate for raw material.The first step, alkali returns molten, is dissolved by the ammonium poly-vanadate (ammonium meta-vanadate) of solid sodium hydroxide solution, obtain containing more than vanadium (60 ~ 120g/L) containing vanadium solution.Second step, the cooling of this solution leaves standstill 24 hours, through the secondary filter of 2 to 3, is poured into by solution in dilution heat of sulfuric acid (water: vitriol oil volume ratio 3:1), obtains red many vanadic acid sodiums solid.3rd step, red many vanadic acid sodiums solid returns the molten solution obtained containing vanadium with sodium hydroxide again.Through the process of the first step and second step, this operation be all less than 5mg/L containing the content of each impurity metal ion in vanadium solution.This solution prepares high-purity non-oxidation two vanadium through precipitation, filtration, calcining process.The method complex process, introduces two steps " alkali returns molten ", needs to consume a large amount of sodium hydroxide and sulfuric acid.
Summary of the invention
The technical problem that the present invention solves is to provide the preparation method of Vanadium Pentoxide in FLAKES.
The preparation method of Vanadium Pentoxide in FLAKES of the present invention, comprises the following steps:
A, return molten: ammonium poly-vanadate is dissolved in sodium hydroxide solution, must solution be returned; In mass ratio, ammonium poly-vanadate: sodium hydroxide=1:0.8 ~ 2, the gained vanadium concentration returned in solution is 90 ~ 120g/L;
B, crystallization: will return that solution chamber is gentle and quiet puts 20 ~ 40h, filter, get filtrate, by filtrate 2 ~ 5 DEG C of standing crystallizations, obtain sodium metavanadate solid;
C, to be dissolved in water: be dissolved in water by sodium metavanadate solid, obtain lysate, the add-on of adjustment water makes the vanadium concentration in lysate be 60 ~ 90g/L;
D, precipitation: in lysate, add ammonium sulfate or ammonium chloride, 45 ~ 65 DEG C of reaction 0.5 ~ 2h, filter, obtain ammonium meta-vanadate solid, wherein, in molar ratio, vanadium ion: ammonium radical ion=1:2 ~ 4;
E, calcining: the calcining of ammonium meta-vanadate solid is obtained Vanadium Pentoxide in FLAKES.
Wherein, in a step in mass ratio, ammonium poly-vanadate: sodium hydroxide=1:1, the vanadium concentration returned in solution is 110g/L.
Wherein, will return that solution chamber is gentle and quiet puts 24h in b step, the time leaving standstill crystallization is more than 10h, and preferably knot leaves standstill the time of crystallization is 10 ~ 20h.
Wherein, in Step d, in molar ratio, vanadium ion: ammonium radical ion=1:3,60 DEG C of reaction 1h.
Further, the calcining described in step e is 500 ~ 600 DEG C of calcining 2 ~ 2.5h, preferably 550 DEG C of calcining 2 ~ 2.5h.
The inventive method can obtain highly purified Vanadium Pentoxide in FLAKES, purity can reach 99.9%, compared with prior art, the inventive method technique is simple, easy to operate, do not introduce other impurity, in preparation process, add a small amount of sodium hydroxide and ammonium salt can prepare Vanadium Pentoxide in FLAKES, only once alkali returns molten, economize in raw materials, meet energy-saving and cost-reducing industry policy.
Embodiment
The preparation method of Vanadium Pentoxide in FLAKES of the present invention, comprises the following steps:
A, return molten: ammonium poly-vanadate is dissolved in sodium hydroxide solution, must solution be returned; In mass ratio, ammonium poly-vanadate: sodium hydroxide=1:0.8 ~ 2, the gained vanadium concentration returned in solution is 90 ~ 120g/L, and now, can record the pH value returning solution is 11 ~ 13;
B, crystallization: will return that solution chamber is gentle and quiet puts 20 ~ 40h, filter, get filtrate, by filtrate 2 ~ 5 DEG C of standing crystallizations, obtain sodium metavanadate solid;
C, to be dissolved in water: be dissolved in water by sodium metavanadate solid, obtain lysate, the add-on of adjustment water makes the vanadium concentration in lysate be 60 ~ 90g/L, and now, the pH value of lysate is 11 ~ 13;
D, precipitation: in lysate, add ammonium sulfate or ammonium chloride, 45 ~ 65 DEG C of reaction 0.5 ~ 2h, filter, obtain ammonium meta-vanadate solid, wherein, in molar ratio, vanadium ion: ammonium radical ion=1:2 ~ 4;
E, calcining: the calcining of ammonium meta-vanadate solid is obtained Vanadium Pentoxide in FLAKES.
Ammonium poly-vanadate complicated component of the present invention, can use general formula NH
4v
xo
yrepresent.Containing various impurity in ammonium poly-vanadate, the impurity content exceeding indexs such as its chromium, silicon, calcium, magnesium, manganese, aluminium.
In a step, containing various impurity metal ion and nonmetallic ion impurity in ammonium poly-vanadate, adding sodium hydroxide can generate precipitation of hydroxide with metallic cation impurity wherein, introduces sodium ion simultaneously, ensure that the generation of sodium metavanadate.In order to ensure the effect of sedimentation removal of impurities, ammonium poly-vanadate: sodium hydroxide mass ratio is preferably 1:1, and regulate the vanadium ion concentration returned in solution to be to ensure carrying out smoothly of later crystallization, the vanadium concentration preferably returned in solution is 110g/L.Vanadium ion concentration is relevant to the crystallization time that is also long-pending and b step of Na ion concentration, vanadium ion concentration and Na ion concentration long-pending larger, crystallization time is shorter, but this value can not be excessive, excessive will in the process of " thick ammonium poly-vanadate returns molten ", direct formation supersaturated solution, do not filter and separate out solid with regard to direct crystallization, now impurity can be wrapped in this crystalline solid.
In b step, in order to make the abundant sedimentation of impurity, need refilter crystallization after returning solution left standstill 20 ~ 40h, in order to raise the efficiency, time of repose is preferably 24h.To return solution filter after, filter residue can return vanadium extraction operation recycling, filtrate 2 ~ 5 DEG C leave standstill, will adularescent sodium metavanadate solid separate out, solid-liquid separation, can obtain sodium metavanadate solid.In order to make crystallization complete, the time that b step leaves standstill crystallization is more than 10h, in order to save time, raises the efficiency meanwhile, and preferred crystallization time is 10 ~ 20h.
In step c, sodium metavanadate solid crystallization obtained is soluble in water, the ratio of adjustment solid and water, ensures that in lysate, vanadium concentration is 60 ~ 90g/L, and solution ph, in 11 ~ 13 scopes, is conducive to next step precipitation operation.In order to avoid introducing impurity as much as possible, described water is preferably deionized water.
In Step d, can add ammonium salt and carry out precipitation in lysate, described ammonium salt can be ammonium chloride or ammonium sulfate, is preferably ammonium sulfate.The add-on of ammonium salt calculates by the vanadium in lysate, in molar ratio, vanadium ion: ammonium radical ion=1:2 ~ 5, be preferably vanadium ion: ammonium radical ion=1:3, after adding ammonium sulfate, the pH value of solution is 8 ~ 9,45 ~ 65 DEG C of reaction 0.5 ~ 2h, the ammonium meta-vanadate solid of a large amount of white is separated out, in order to improve reaction efficiency, and preferably 60 DEG C of reaction 1h.
The calcining of ammonium meta-vanadate solid can obtain Vanadium Pentoxide in FLAKES, and for ensureing that calcining completely, improves Vanadium Pentoxide in FLAKES yield, preferably 500 ~ 600 DEG C of calcining 2 ~ 2.5h, more preferably at 550 DEG C of calcining 2 ~ 2.5h.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1
A, weighing 200g ammonium poly-vanadate are placed in A beaker, weigh 200g sodium hydroxide and are dissolved in the B beaker filling 930ml water.Slowly pour sodium hydroxide solution into A beaker, stir, room temperature reaction 30 minutes, dissolves completely to solid.Now, the vanadium concentration in solution is 110g/L, and pH value is 12.
The cooling of b, room temperature, standing 24h, filter three times with filter plants such as Büchner funnels.Filtrate is positioned in climatic chamber, and temperature is adjusted to 2 ~ 5 DEG C, leaves standstill more than 10h, treats that the sodium metavanadate solid of white is separated out.Solid-liquid separation, weighing solid is 150g.
C, be dissolved in the deionized water of 840ml by the solid of b step gained, add 487g ammonium sulfate, 60 DEG C of water-bath 1h separate out to a large amount of white solids.
D, by step c gained solid filtering, dry, last 550 DEG C calcining 2.5h obtain high purity vanadic anhydride.After testing, the purity of gained Vanadium Pentoxide in FLAKES is 99.9%.
Embodiment 2
A, weighing 200g ammonium poly-vanadate are placed in A beaker, weigh 400g sodium hydroxide and are dissolved in the B beaker filling 1030ml water.Slowly pour sodium hydroxide solution into A beaker, stir, room temperature reaction 30 minutes, dissolves completely to solid.Now, the vanadium concentration in solution is 100g/L, and pH value is 13.
The cooling of b, room temperature, standing 40h, filter three times with filter plants such as Büchner funnels.Filtrate is positioned in climatic chamber, and temperature is adjusted to 2 ~ 5 DEG C, leaves standstill 12h, treats that the sodium metavanadate solid of white is separated out.Solid-liquid separation, weighing solid is 153g.
C, be dissolved in the deionized water of 1000ml by the solid of b step gained, add 717g ammonium chloride, 65 DEG C of water-bath 0.5h separate out to a large amount of white solids.
D, by step c gained solid filtering, dry, last 600 DEG C calcining 2.5h obtain high purity vanadic anhydride.After testing, the purity of gained Vanadium Pentoxide in FLAKES is 99.0%.
Embodiment 3
A, weighing 200g ammonium poly-vanadate are placed in A beaker, weigh 160g sodium hydroxide and are dissolved in the B beaker filling 850ml water.Slowly pour sodium hydroxide solution into A beaker, stir, room temperature reaction 30 minutes, dissolves completely to solid.Now, the vanadium concentration in solution is 120g/L, and pH value is 11.
The cooling of b, room temperature, standing 20h, filter three times with filter plants such as Büchner funnels.Filtrate is positioned in climatic chamber, and temperature is adjusted to 2 ~ 5 DEG C, leaves standstill 20h, treats that the sodium metavanadate solid of white is separated out.Solid-liquid separation, weighing solid is 147g.
C, be dissolved in the deionized water of 700ml by the solid of b step gained, add 318g ammonium sulfate, 45 DEG C of water-bath 2h separate out to a large amount of white solids.
D, by step c gained solid filtering, dry, last 500 DEG C calcining 2.5h obtain high purity vanadic anhydride.After testing, the purity of gained Vanadium Pentoxide in FLAKES is 99.5%.
Claims (5)
1. the preparation method of Vanadium Pentoxide in FLAKES, is characterized in that comprising the following steps:
A, return molten: ammonium poly-vanadate is dissolved in sodium hydroxide solution, must solution be returned; In mass ratio, ammonium poly-vanadate: sodium hydroxide=1:0.8 ~ 2, the gained vanadium concentration returned in solution is 90 ~ 120g/L;
B, crystallization: will return that solution chamber is gentle and quiet puts 20 ~ 40h, filter, get filtrate, by filtrate 2 ~ 5 DEG C of standing crystallizations, obtain sodium metavanadate solid;
C, to be dissolved in water: be dissolved in water by sodium metavanadate solid, obtain lysate, the add-on of adjustment water makes the vanadium concentration in lysate be 60 ~ 90g/L;
D, precipitation: in lysate, add ammonium sulfate or ammonium chloride, 45 ~ 65 DEG C of reaction 0.5 ~ 2h, filter, obtain ammonium meta-vanadate solid, wherein, in molar ratio, vanadium ion: ammonium radical ion=1:2 ~ 4;
E, calcining: the calcining of ammonium meta-vanadate solid is obtained Vanadium Pentoxide in FLAKES.
2. the preparation method of Vanadium Pentoxide in FLAKES according to claim 1, is characterized in that: in a step in mass ratio, ammonium poly-vanadate: sodium hydroxide=1:1, and the vanadium concentration returned in solution is 110g/L.
3. the preparation method of Vanadium Pentoxide in FLAKES according to claim 1, is characterized in that: will return in b step that solution chamber is gentle and quiet puts 24h, and the time leaving standstill crystallization is more than 10h, and preferably knot leaves standstill the time of crystallization is 10 ~ 20h.
4. the preparation method of Vanadium Pentoxide in FLAKES according to claim 1, is characterized in that: in Step d, in molar ratio, and vanadium ion: ammonium radical ion=1:3,60 DEG C of reaction 1h.
5. the preparation method of Vanadium Pentoxide in FLAKES according to claim 1, is characterized in that: the calcining described in step e is 500 ~ 600 DEG C of calcining 2 ~ 2.5h, preferably 550 DEG C of calcining 2 ~ 2.5h.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105314678A (en) * | 2015-11-19 | 2016-02-10 | 攀钢集团西昌钢钒有限公司 | Vanadium pentoxide preparation method |
| CN106145188A (en) * | 2016-07-05 | 2016-11-23 | 河北钢铁股份有限公司承德分公司 | A kind of method that sodium vanadium extraction liquid prepares V electrolyte high purity vanadic anhydride |
| CN106241872A (en) * | 2016-07-29 | 2016-12-21 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN106399786A (en) * | 2016-11-25 | 2017-02-15 | 南通汉瑞新材料科技有限公司 | Novel method for preparing vanadium-nitrogen alloy |
| CN106430305A (en) * | 2016-08-31 | 2017-02-22 | 大连博融新材料股份有限公司 | Production method of high-density ammonium metavanadate |
| CN106785101A (en) * | 2016-12-12 | 2017-05-31 | 东莞市佳乾新材料科技有限公司 | A kind of solid state battery based on high-purity vanadium pentoxide and preparation method thereof |
| CN107285381A (en) * | 2017-08-17 | 2017-10-24 | 芜湖人本合金有限责任公司 | Ammonium metavanadate and preparation method thereof |
| CN107324387A (en) * | 2017-08-17 | 2017-11-07 | 芜湖人本合金有限责任公司 | The preparation method of vanadic anhydride |
| CN110467222A (en) * | 2019-09-06 | 2019-11-19 | 洪江市钒盛钒业科技有限公司 | A method of preparing vanadic anhydride |
| CN110723750A (en) * | 2019-10-24 | 2020-01-24 | 成都先进金属材料产业技术研究院有限公司 | Direct preparation of high-purity V from alkaline vanadium-containing leaching solution2O5Method (2) |
| CN111302396A (en) * | 2020-04-20 | 2020-06-19 | 承德燕北冶金材料有限公司 | Preparation method of vanadium pentoxide |
| CN111748702A (en) * | 2020-07-06 | 2020-10-09 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide and circulating sodium and ammonium by using vanadium solution |
| CN111979431A (en) * | 2019-10-11 | 2020-11-24 | 成都秦脉科技有限公司 | Production method of ammonium vanadate |
| CN114180624A (en) * | 2021-12-23 | 2022-03-15 | 大连博融新材料有限公司 | Method for preparing high-purity vanadium by separating vanadium and ammonium serving as ammonium metavanadate raw materials |
| CN115196676A (en) * | 2022-07-13 | 2022-10-18 | 湖南省银峰新能源有限公司 | Preparation method of high-purity vanadium pentoxide suitable for vanadium electrolyte |
| CN116040681A (en) * | 2023-01-31 | 2023-05-02 | 承德天大钒业有限责任公司 | Three-dimensional porous vanadium pentoxide, and preparation method and application thereof |
| CN116177601A (en) * | 2021-11-29 | 2023-05-30 | 中国科学院过程工程研究所 | Method for preparing high-purity vanadium pentoxide from ammonium polyvanadate |
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| CN105314678A (en) * | 2015-11-19 | 2016-02-10 | 攀钢集团西昌钢钒有限公司 | Vanadium pentoxide preparation method |
| CN106145188A (en) * | 2016-07-05 | 2016-11-23 | 河北钢铁股份有限公司承德分公司 | A kind of method that sodium vanadium extraction liquid prepares V electrolyte high purity vanadic anhydride |
| CN106241872A (en) * | 2016-07-29 | 2016-12-21 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN106241872B (en) * | 2016-07-29 | 2018-05-18 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN106430305A (en) * | 2016-08-31 | 2017-02-22 | 大连博融新材料股份有限公司 | Production method of high-density ammonium metavanadate |
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| CN106399786A (en) * | 2016-11-25 | 2017-02-15 | 南通汉瑞新材料科技有限公司 | Novel method for preparing vanadium-nitrogen alloy |
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| CN107285381A (en) * | 2017-08-17 | 2017-10-24 | 芜湖人本合金有限责任公司 | Ammonium metavanadate and preparation method thereof |
| CN107324387A (en) * | 2017-08-17 | 2017-11-07 | 芜湖人本合金有限责任公司 | The preparation method of vanadic anhydride |
| CN110467222A (en) * | 2019-09-06 | 2019-11-19 | 洪江市钒盛钒业科技有限公司 | A method of preparing vanadic anhydride |
| CN110467222B (en) * | 2019-09-06 | 2021-11-23 | 洪江市钒盛钒业科技有限公司 | Method for preparing vanadium pentoxide |
| CN111979431A (en) * | 2019-10-11 | 2020-11-24 | 成都秦脉科技有限公司 | Production method of ammonium vanadate |
| CN110723750A (en) * | 2019-10-24 | 2020-01-24 | 成都先进金属材料产业技术研究院有限公司 | Direct preparation of high-purity V from alkaline vanadium-containing leaching solution2O5Method (2) |
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| CN111748702A (en) * | 2020-07-06 | 2020-10-09 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide and circulating sodium and ammonium by using vanadium solution |
| CN116177601A (en) * | 2021-11-29 | 2023-05-30 | 中国科学院过程工程研究所 | Method for preparing high-purity vanadium pentoxide from ammonium polyvanadate |
| CN114180624A (en) * | 2021-12-23 | 2022-03-15 | 大连博融新材料有限公司 | Method for preparing high-purity vanadium by separating vanadium and ammonium serving as ammonium metavanadate raw materials |
| CN114180624B (en) * | 2021-12-23 | 2024-01-23 | 大连融科储能集团股份有限公司 | Method for preparing high-purity vanadium by separating ammonium metavanadate raw material vanadium and ammonium |
| CN115196676A (en) * | 2022-07-13 | 2022-10-18 | 湖南省银峰新能源有限公司 | Preparation method of high-purity vanadium pentoxide suitable for vanadium electrolyte |
| CN115196676B (en) * | 2022-07-13 | 2024-01-23 | 湖南省银峰新能源有限公司 | Preparation method of high-purity vanadium pentoxide suitable for vanadium electrolyte |
| CN116040681A (en) * | 2023-01-31 | 2023-05-02 | 承德天大钒业有限责任公司 | Three-dimensional porous vanadium pentoxide, and preparation method and application thereof |
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| CN104477992B (en) | 2017-02-22 |
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