CN118062893A - Method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate - Google Patents
Method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate Download PDFInfo
- Publication number
- CN118062893A CN118062893A CN202410234597.XA CN202410234597A CN118062893A CN 118062893 A CN118062893 A CN 118062893A CN 202410234597 A CN202410234597 A CN 202410234597A CN 118062893 A CN118062893 A CN 118062893A
- Authority
- CN
- China
- Prior art keywords
- ammonium
- ammonium metavanadate
- reaction
- temperature
- finished
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 38
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 6
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 125000000129 anionic group Chemical group 0.000 claims abstract description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 3
- 230000009615 deamination Effects 0.000 claims abstract description 3
- 238000006481 deamination reaction Methods 0.000 claims abstract description 3
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate provided by the invention comprises the following steps: s1: adding an industrial ammonium metavanadate raw material into pure water, heating, stirring, dissolving, adding NaOH, standing and filtering after the reaction is finished to obtain an upper layer solution; s2: adjusting the PH of the solution to 9-10, adding an anionic flocculant, adding magnesium sulfate or magnesium chloride, and filtering after the reaction is finished to obtain a secondary purifying solution; s3: adjusting the pH value of the secondary purifying liquid to 8-9, adopting a weak alkaline ammonium salt precipitation method, adding ammonium chloride or ammonium sulfate into the heated secondary purifying liquid, cooling to room temperature after the reaction is finished, and drying to obtain ammonium metavanadate; s4: deamination and calcination are carried out on the dried ammonium metavanadate in a muffle furnace to obtain high-purity vanadium pentoxide; the invention adopts a sectional impurity removal chemical purification method to purify ammonium metavanadate, the whole process is carried out under alkaline or weak alkaline conditions, no acid is consumed, the impurity removal rate is high, and no new impurities are introduced.
Description
Technical Field
The invention relates to the technical field of alloy preparation, in particular to a method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate.
Background
Ammonium metavanadate (NH 4VO3) is white crystalline powder with a molecular weight of 116.98, is insoluble in water, hot water and ammonia water, and is insoluble in ethanol, ether and ammonium chloride, and is burnt in air to become vanadium pentoxide.
The high-purity vanadium pentoxide is mainly used in the fields of aerospace, all-vanadium redox flow battery energy storage, luminescent materials, vanadium-based hydrogen storage alloy, nano catalysis and the like, along with the industrialization of all-vanadium redox flow battery energy storage and some high-end technical products, the high-purity vanadium pentoxide has higher requirements on purity and quality, and the high-purity vanadium pentoxide is mainly imported in China at present, so that the high-purity vanadium pentoxide has a very large market gap, and the industrial development of the high-purity vanadium pentoxide in China is rapidly accelerated. Most of impurities in the vanadium product are metal elements, silicon and phosphorus, and the large use amount of the extractant and the ion exchange resin in the process of purifying the vanadium pentoxide by a solvent extraction method and an ion exchange method at present leads to high production cost and small application of industrial production; the chemical purification method has the advantages of complex impurity removal process, longer process flow, large acid consumption, easy introduction of new impurities and the like, and the purity of the vanadium pentoxide is difficult to improve.
Disclosure of Invention
In view of the above drawbacks, the present invention provides a method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate, comprising the following steps:
S1: adding an industrial ammonium metavanadate raw material into pure water, wherein the mass ratio of the raw material to the pure water is 1 (5-6), heating, stirring and dissolving, adding NaOH, wherein the mass ratio of the raw material to the NaOH is 1:0.3, stirring and reacting at constant temperature and constant speed for 2 hours, and standing and filtering after the reaction is finished at the temperature of 90 ℃ at the rotating speed of 500r/min to obtain an upper-layer solution;
S2: adjusting the PH of the solution to 9-10, firstly adding an anionic flocculant (polyacrylamide), wherein the mass ratio of the raw materials to the dosage of the anionic flocculant is 100:0.01, then adding magnesium sulfate or magnesium chloride, wherein the mass ratio of the raw materials to the magnesium sulfate or magnesium chloride is 100:4, carrying out constant-temperature constant-speed reaction for 0.5h, carrying out temperature 50 ℃ and rotating speed 500r/min, and filtering after the reaction is finished to obtain a secondary purifying liquid;
S3: adjusting the pH of the secondary purifying liquid to 8-9, adopting a weak alkaline ammonium salt precipitation method, heating the secondary purifying liquid in a water bath, adding ammonium chloride or ammonium sulfate into the heated secondary purifying liquid, reacting at a constant temperature and a constant speed for 1h, wherein the ammonium addition coefficient is 1.5, the temperature is 90 ℃, the rotating speed is 300r/min, cooling to the room temperature after the reaction is finished, filtering, washing with pure water, filtering for 3 times, and drying in a constant temperature drying oven at 60 ℃ to obtain ammonium metavanadate;
s4: deamination and calcination are carried out on the dried ammonium metavanadate in a muffle furnace, wherein the calcination temperature is 550 ℃, and the calcination time is 2.5h, so that the high-purity vanadium pentoxide is obtained.
The invention adopts a sectional impurity removal chemical purification method to purify ammonium metavanadate, and uses the prepared high-purity ammonium metavanadate to calcine to obtain high-purity vanadium pentoxide, the whole process is carried out under alkaline or weak alkaline conditions, no acid consumption is caused, the impurity removal rate is high, and no new impurity is introduced.
Detailed Description
Examples
Step one: 100g of ammonium metavanadate is added into 500ml of pure water, the mixture is heated to 90 ℃ by using a water bath pot, 200ml of 15% NaOH solution is added, the mixture is stirred at a constant speed of 500r/min at a constant temperature of 90 ℃ for 2h, and after the reaction is finished, the mixture is stood and filtered to obtain an upper layer solution.
Step two: and (3) regulating the pH of the solution obtained in the step one to 9.5, adding 1ml of 1% polyacrylamide, then adding 20ml of 20% magnesium sulfate, stirring at a constant temperature of 50 ℃ for reaction for 0.5h at a constant speed of 500r/min, standing and filtering after the reaction is finished to obtain a secondary purified solution (V 2O5:95.5 g/L).
Step three: heating the secondary purifying liquid in the second step in a water bath, adding ammonium sulfate into the heated secondary purifying liquid, reacting at a constant temperature and a constant speed for 1h, wherein the ammonium addition coefficient is 1.5, the temperature is 90 ℃, the rotating speed is 300r/min, cooling to room temperature after the reaction is finished, filtering, washing with pure water for 3 times, and drying in a constant temperature drying oven at 60 ℃ to obtain ammonium metavanadate;
step four: and (3) deaminizing and calcining the dried ammonium metavanadate in the step (III) in a muffle furnace, wherein the calcining temperature is 550 ℃, and the calcining time is 2.5h, so that the high-purity vanadium pentoxide (99.82%) is obtained.
Claims (1)
1. The method for preparing the high-purity vanadium pentoxide by purifying the ammonium metavanadate is characterized by comprising the following steps of:
S1: adding an industrial ammonium metavanadate raw material into pure water, wherein the mass ratio of the raw material to the pure water is 1 (5-6), heating, stirring and dissolving, adding NaOH, wherein the mass ratio of the raw material to the NaOH is 1:0.3, stirring and reacting at constant temperature and constant speed for 2 hours, and standing and filtering after the reaction is finished at the temperature of 90 ℃ at the rotating speed of 500r/min to obtain an upper-layer solution;
S2: adjusting the PH of the solution to 9-10, firstly adding an anionic flocculant, wherein the mass ratio of the raw materials to the dosage of the anionic flocculant is 100:0.01, then adding magnesium sulfate or magnesium chloride, wherein the mass ratio of the raw materials to the magnesium sulfate or magnesium chloride is 100:4, carrying out constant temperature and constant speed reaction for 0.5h, carrying out temperature 50 ℃ and rotating speed 500r/min, and filtering after the reaction is finished to obtain a secondary purifying liquid;
S3: adjusting the pH of the secondary purifying liquid to 8-9, adopting a weak alkaline ammonium salt precipitation method, heating the secondary purifying liquid in a water bath, adding ammonium chloride or ammonium sulfate into the heated secondary purifying liquid, reacting at a constant temperature and a constant speed for 1h, wherein the ammonium addition coefficient is 1.5, the temperature is 90 ℃, the rotating speed is 300r/min, cooling to the room temperature after the reaction is finished, filtering, washing with pure water, filtering for 3 times, and drying in a constant temperature drying oven at 60 ℃ to obtain ammonium metavanadate;
s4: deamination and calcination are carried out on the dried ammonium metavanadate in a muffle furnace, wherein the calcination temperature is 550 ℃, and the calcination time is 2.5h, so that the high-purity vanadium pentoxide is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410234597.XA CN118062893A (en) | 2024-03-01 | 2024-03-01 | Method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410234597.XA CN118062893A (en) | 2024-03-01 | 2024-03-01 | Method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118062893A true CN118062893A (en) | 2024-05-24 |
Family
ID=91110687
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410234597.XA Pending CN118062893A (en) | 2024-03-01 | 2024-03-01 | Method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118062893A (en) |
-
2024
- 2024-03-01 CN CN202410234597.XA patent/CN118062893A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102603000B (en) | Process for preparing high-purity vanadium pentoxide by adopting ammonium metavanadate as raw material | |
| CN103420416B (en) | Ammonium metavanadate preparation method | |
| CN114772569B (en) | Method for preparing ferric phosphate by two-step hydrochloric acid dissolution of pyrite cinder | |
| KR101348524B1 (en) | Process for preparing ammonium metatungstate | |
| CN108754186A (en) | The method for preparing vfanadium compound containing vanadium solution | |
| CN111994952A (en) | Method for preparing high-purity vanadium pentoxide by vacuum sublimation of metallurgical-grade vanadium pentoxide | |
| CN107117654B (en) | A method of vanadium dioxide is prepared from containing vanadium solution | |
| CN113025833A (en) | Method for precipitating vanadium from high-concentration vanadium solution | |
| CN102924380B (en) | Preparation method of imidocarb | |
| CN115403019A (en) | Preparation method of iron phosphate | |
| CN101955233B (en) | Method for producing ferrous sulphate monohydrate | |
| CN110331297B (en) | Method for preparing vanadium pentoxide from vanadium slag in short process | |
| CN101920994A (en) | Method for preparing vanadyl sulfate | |
| CN118062893A (en) | Method for preparing high-purity vanadium pentoxide by purifying ammonium metavanadate | |
| CN103449482B (en) | A kind of method utilizing serpentine to prepare magnesium oxide, nickel, cobalt and white carbon black | |
| CN114524771A (en) | Preparation method of 6-hydroxy-2,4,5-triaminopyrimidine sulfate | |
| CN108640162B (en) | Alkali circulation iron-containing solid waste iron oxide pigment production equipment system | |
| CN116259811A (en) | Method for preparing vanadium electrolyte from sodium vanadate solution | |
| CN105585045A (en) | Method for preparing titanyl sulfate | |
| CN113044862B (en) | Method for dehydrating different ammonium carnallite materials by utilizing synergistic coupling effect of different ammonium carnallite materials | |
| CN112574043B (en) | Production process of basic red intermediate 3-ethylamino-p-methylphenol | |
| CN101774651B (en) | Method for preparing reagent cobalt chloride hexahydrate | |
| CN109336151B (en) | Method for preparing aluminum chloride by using fly ash | |
| CN102826601A (en) | Method for preparing high-purity zirconium oxide through purifying silicon removed zirconium | |
| CN102618064B (en) | Synthesizing process of Janus green B |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |