CN102730757A - Method for preparing high purity vanadium pentoxide through using ammonium metavanadate - Google Patents
Method for preparing high purity vanadium pentoxide through using ammonium metavanadate Download PDFInfo
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- CN102730757A CN102730757A CN2011100897418A CN201110089741A CN102730757A CN 102730757 A CN102730757 A CN 102730757A CN 2011100897418 A CN2011100897418 A CN 2011100897418A CN 201110089741 A CN201110089741 A CN 201110089741A CN 102730757 A CN102730757 A CN 102730757A
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Abstract
The invention which relates to a method for preparing high purity vanadium pentoxide through using ammonium metavanadate belongs to the wet metallurgy field. The method comprises the following steps: heating and dissolving crude ammonium metavanadate in water, adjusting the pH value to 8-10 with an alkali after dissolving, adding an impurity removing agent to remove impurities, filtering to obtain a sodium metavanadate solution, adding ammonia water or an ammonium salt to the sodium metavanadate solution to precipitate to obtain an ammonium metavanadate precipitate, dehydrating the ammonium metavanadate precipitate, carrying out water washing on the precipitate through using a dilute ammonium salt solution, dehydrating after the wash washing, and roasting to obtain the high purity vanadium pentoxide. Vanadium pentoxide produced through adopting the method of the invention has the advantages of high purity and less impurities, and completely satisfies production requirements of high-end products; and the method of the invention has the advantages of short process flow, simple equipment, low cost and high benefit, and is suitable for the large-scale industrial production.
Description
Technical field
The present invention relates to a kind ofly prepare the method for high purity vanadic anhydride, belong to the hydrometallurgy category with ammonium meta-vanadate.
Background technology
The high purity vanadic anhydride vanadium is meant that on the basis of common Vanadium Pentoxide in FLAKES GB3283-87 standard foreign matter contents such as silicon, phosphorus, iron make it to be lower than the GB limit value in the reduction vanadium.Because country does not formulate high standard, be high purity vanadic anhydride so be higher than the Vanadium Pentoxide in FLAKES of GB purity.
Along with the continuous progress of science and technology, Flos Bombacis Malabarici has been developed microalloy heat and has been pricked rail, and X52 level pipe, line steel and microalloy automobile beam have steel plate.Many simultaneously local new vananum, vanadium nitride, vanadium carbide, vanadium metal, vanadium silk, 80 vanadium iron gone up.Vanadium cell also will come out.These products all need be produced with high purity vanadic anhydride.Existing GB purity vanadium is difficult to satisfy the requirement of these high-end products with vanadium.As: aluminium is less than 0.1% in the vanadium carbide requirement vanadium, and silicon is less than 0.1%, and phosphorus is less than 0.05%; Vanadium nitride requires silicon 0.07% in the vanadium, phosphorus 0.01%, and X52 level pipe line steel silicon 0.15-0.35%, phosphorus is less than 0.02%; Vanadium metal and vanadium silk also require nitrogen and carbon content all less than 10 * 10
-4%
The production of high purity vanadic anhydride, present domestic cleaners such as Tai-Ace S 150, calcium chloride, oxalic acid, sulphosalicylic acid that mostly adopt, the content of silicon, phosphorus, iron in the decline vanadium in different pH values respectively.Its technical process is long, and the consumption worker is many, and production cost is high, and the Vanadium Pentoxide in FLAKES product purity does not all reach the requirement of some high-end products with vanadium mostly.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare the method for high purity vanadic anhydride, produce the highly purified Vanadium Pentoxide in FLAKES that can satisfy some high-end products with the vanadium requirement with ammonium meta-vanadate.
The objective of the invention is to realize: a kind of method for preparing high purity vanadic anhydride with ammonium meta-vanadate through following technical scheme; It is characterized in that: at first with thick ammonium meta-vanadate heating for dissolving in water; PH value is regulated to 8-10 with alkali in the dissolving back; Add the cleaner removal of impurities again, get sodium metavanadate solution after the filtration, in sodium metavanadate solution, add ammoniacal liquor or ammonium salt and precipitate to such an extent that ammonium meta-vanadate precipitates; The ammonium meta-vanadate deposition with the dilute ammonium salt solution washing, gets high purity vanadic anhydride through dehydration, roasting after the washing again after dehydration.
Said thick ammonium meta-vanadate heating for dissolving temperature in water is 90-95 ℃, and the weight ratio of thick ammonium meta-vanadate and water is 1: 3-4.5.
It is sodium hydroxide, yellow soda ash or its mixture that said pH value is regulated alkali.
The weight ratio of ammonium salt and water is 1-5 in the said dilute ammonium salt solution: 100.
Said ammonium salt is ammonium chloride or bicarbonate of ammonia.
Said filtration operation adopts the filter press filter to filter, and dehydration procedure adopts centrifuge dewatering.
The invention has the beneficial effects as follows: the Vanadium Pentoxide in FLAKES purity of 1, producing is high, impurity is few, meets the production requirement of some high-end products fully; 2, technical process is short, equipment is simple, cost is low, high efficiency, is fit to the industrial production of mass-producing.
Embodiment
Below in conjunction with embodiment the present invention is described further:
Embodiment 1
Thick ammonium meta-vanadate is added in the entry with 1: 4 ratio of weight ratio; Speed with 120r/min is heated to 90 ℃ while stirring, keeps ammonium meta-vanadate being dissolved fully in 20-30 minute, and pH value to 9 is regulated with sheet alkali in the dissolving back; Add the magnesium chloride removal of impurities again; With getting sodium metavanadate solution after the filtration of filter press filter, in sodium metavanadate solution, add chloride precipitation and get the ammonium meta-vanadate deposition, ammonium meta-vanadate precipitates behind centrifuge dewatering; Rare ammonium chloride solution with 1% is directly washing in whizzer, washes after 10 minutes and gets high purity vanadic anhydride through dehydration, roasting again.Can reach 99.9% through analyzing Vanadium Pentoxide in FLAKES purity.
Embodiment 2
Thick ammonium meta-vanadate is added in the entry with 1: 4 ratio of weight ratio; Speed with 120r/min is heated to 95 ℃ while stirring, keeps ammonium meta-vanadate being dissolved fully in 20-30 minute, and pH value to 10 is regulated with sheet alkali in the dissolving back; Add the sal epsom removal of impurities again; With getting sodium metavanadate solution after the filtration of filter press filter, in sodium metavanadate solution, add chloride precipitation and get the ammonium meta-vanadate deposition, ammonium meta-vanadate precipitates behind centrifuge dewatering; Rare ammonium chloride solution with 5% is directly washing in whizzer, washes after 15 minutes and gets high purity vanadic anhydride through dehydration, roasting again.Can reach 99.9% through analyzing Vanadium Pentoxide in FLAKES purity.
Embodiment 3
Thick ammonium meta-vanadate is added in the entry with 1: 4 ratio of weight ratio; Speed with 120r/min is heated to 95 ℃ while stirring, keeps ammonium meta-vanadate being dissolved fully in 20-30 minute, and pH value to 9 is regulated with the mixture of sheet alkali and yellow soda ash in the dissolving back; Add the sal epsom removal of impurities again; With getting sodium metavanadate solution after the filtration of filter press filter, in sodium metavanadate solution, add chloride precipitation and get the ammonium meta-vanadate deposition, ammonium meta-vanadate precipitates behind centrifuge dewatering; Rare ammonium bicarbonate soln with 1% is directly washing in whizzer, washes after 10 minutes and gets high purity vanadic anhydride through dehydration, roasting again.Can reach 99.9% through analyzing Vanadium Pentoxide in FLAKES purity.
Embodiment 4
Thick ammonium meta-vanadate is added in the entry with 1: 4 ratio of weight ratio; Speed with 120r/min is heated to 95 ℃ while stirring, keeps ammonium meta-vanadate being dissolved fully in 20-30 minute, and pH value to 10 is regulated with the mixture of sheet alkali and yellow soda ash in the dissolving back; Add the sal epsom removal of impurities again; With getting sodium metavanadate solution after the filtration of filter press filter, in sodium metavanadate solution, add chloride precipitation and get the ammonium meta-vanadate deposition, ammonium meta-vanadate precipitates behind centrifuge dewatering; Rare ammonium bicarbonate soln with 5% is directly washing in whizzer, washes after 15 minutes and gets high purity vanadic anhydride through dehydration, roasting again.Can reach 99.9% through analyzing Vanadium Pentoxide in FLAKES purity.
Claims (6)
1. method for preparing high purity vanadic anhydride with ammonium meta-vanadate; It is characterized in that: at first with thick ammonium meta-vanadate heating for dissolving in water, pH value is regulated to 8-10 with alkali in the dissolving back, adds the cleaner removal of impurities again; Get sodium metavanadate solution after the filtration; In sodium metavanadate solution, add ammoniacal liquor or ammonium salt precipitate the ammonium meta-vanadate deposition, with the dilute ammonium salt solution washing, warp dewaters the ammonium meta-vanadate deposition again after the washing, roasting gets high purity vanadic anhydride through the dehydration back.
2. a kind ofly prepare the method for high purity vanadic anhydride with ammonium meta-vanadate according to claim 1 is said, it is characterized in that: thick ammonium meta-vanadate heating for dissolving temperature in water is 90-95 ℃, and the weight ratio of thick ammonium meta-vanadate and water is 1: 3-4.5.
3. a kind ofly prepare the method for high purity vanadic anhydride with ammonium meta-vanadate according to claim 1 is said, it is characterized in that: it is sodium hydroxide, yellow soda ash or its mixture that said pH value is regulated alkali.
4. a kind ofly prepare the method for high purity vanadic anhydride with ammonium meta-vanadate according to claim 1 is said, it is characterized in that: the weight ratio of ammonium salt and water is 1-5 in the said dilute ammonium salt solution: 100.
5. said a kind ofly prepare the method for high purity vanadic anhydride with ammonium meta-vanadate according to claim 1 with 4, it is characterized in that: said ammonium salt is ammonium chloride or bicarbonate of ammonia.
6. a kind ofly prepare the method for high purity vanadic anhydride with ammonium meta-vanadate according to claim 1 is said, it is characterized in that: filter operation and adopt the filter press filter to filter, dehydration procedure adopts centrifuge dewatering.
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923776A (en) * | 2012-12-03 | 2013-02-13 | 张春雨 | Method for producing high-purity vanadium pentoxide |
| CN103601241A (en) * | 2013-11-13 | 2014-02-26 | 河北钢铁股份有限公司承德分公司 | Preparation method of high-purity powder vanadium pentoxide |
| CN103708553A (en) * | 2013-12-26 | 2014-04-09 | 国药集团化学试剂有限公司 | Method for improving industrial-grade ammonium vanadate quality |
| CN104477992A (en) * | 2015-01-07 | 2015-04-01 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
| CN104495927A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
| CN106241873A (en) * | 2016-08-26 | 2016-12-21 | 陕西华源矿业有限责任公司 | The preparation method of high-purity vanadium pentoxide |
| CN106986383A (en) * | 2016-01-20 | 2017-07-28 | 陕西五洲矿业股份有限公司 | The preparation method of high purity vanadic anhydride used for all-vanadium redox flow battery |
| 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 |
| CN107285382A (en) * | 2017-08-17 | 2017-10-24 | 芜湖人本合金有限责任公司 | The preparation method of high purity vanadic anhydride |
| CN107304068A (en) * | 2016-04-22 | 2017-10-31 | 陕西五洲矿业股份有限公司 | The preparation method of high purity vanadium metal high purity vanadic anhydride |
| 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 |
| US10053371B2 (en) | 2015-01-30 | 2018-08-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for preparing high-purity vanadium pentoxide powder |
| US10099939B2 (en) | 2015-01-30 | 2018-10-16 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium pentoxide powder |
| US10112846B2 (en) | 2015-01-30 | 2018-10-30 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium tetraoxide powder |
| US10125024B2 (en) | 2015-01-30 | 2018-11-13 | Institute Of Procees Engineering Chinese Academy Of Sciences | System and method for purifying and preparing high-purity vanadium pentoxide powder |
| CN109607613A (en) * | 2018-12-11 | 2019-04-12 | 中南大学 | A method of with deionized water clean manufacturing high purity vanadic anhydride |
| US10294118B2 (en) | 2015-01-30 | 2019-05-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for purifying vanadium pentoxide |
| 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) |
| CN112408479A (en) * | 2020-12-13 | 2021-02-26 | 湖南众鑫新材料科技股份有限公司 | Process for preparing low-valence vanadium from ammonium metavanadate |
| CN112591795A (en) * | 2020-12-28 | 2021-04-02 | 湖南众鑫新材料科技股份有限公司 | Method for treating tail gas generated in preparation of low-valence vanadium from ammonium metavanadate |
| CN115010176A (en) * | 2022-05-26 | 2022-09-06 | 湖南省银峰新能源有限公司 | Preparation method of high-purity vanadium pentoxide |
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Cited By (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923776A (en) * | 2012-12-03 | 2013-02-13 | 张春雨 | Method for producing high-purity vanadium pentoxide |
| CN102923776B (en) * | 2012-12-03 | 2013-07-03 | 张春雨 | Method for producing high-purity vanadium pentoxide |
| CN103601241A (en) * | 2013-11-13 | 2014-02-26 | 河北钢铁股份有限公司承德分公司 | Preparation method of high-purity powder vanadium pentoxide |
| CN103708553B (en) * | 2013-12-26 | 2016-01-06 | 国药集团化学试剂有限公司 | A kind of method promoting technical grade ammonium meta-vanadate quality |
| CN103708553A (en) * | 2013-12-26 | 2014-04-09 | 国药集团化学试剂有限公司 | Method for improving industrial-grade ammonium vanadate quality |
| CN104477992A (en) * | 2015-01-07 | 2015-04-01 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
| CN104495927A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
| CN104495927B (en) * | 2015-01-07 | 2016-03-30 | 攀钢集团研究院有限公司 | Prepare the method for Vanadium Pentoxide in FLAKES |
| US10099939B2 (en) | 2015-01-30 | 2018-10-16 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium pentoxide powder |
| US10294118B2 (en) | 2015-01-30 | 2019-05-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for purifying vanadium pentoxide |
| US10125024B2 (en) | 2015-01-30 | 2018-11-13 | Institute Of Procees Engineering Chinese Academy Of Sciences | System and method for purifying and preparing high-purity vanadium pentoxide powder |
| US10112846B2 (en) | 2015-01-30 | 2018-10-30 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for producing high-purity vanadium tetraoxide powder |
| US10053371B2 (en) | 2015-01-30 | 2018-08-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for preparing high-purity vanadium pentoxide powder |
| CN106986383B (en) * | 2016-01-20 | 2021-07-30 | 陕西五洲矿业股份有限公司 | Preparation method of high-purity vanadium pentoxide for all-vanadium flow battery |
| CN106986383A (en) * | 2016-01-20 | 2017-07-28 | 陕西五洲矿业股份有限公司 | The preparation method of high purity vanadic anhydride used for all-vanadium redox flow battery |
| CN107304068A (en) * | 2016-04-22 | 2017-10-31 | 陕西五洲矿业股份有限公司 | The preparation method of high purity vanadium metal high purity vanadic anhydride |
| CN106241873A (en) * | 2016-08-26 | 2016-12-21 | 陕西华源矿业有限责任公司 | The preparation method of high-purity vanadium pentoxide |
| 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 |
| CN107285382A (en) * | 2017-08-17 | 2017-10-24 | 芜湖人本合金有限责任公司 | The preparation method of high purity vanadic anhydride |
| 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 |
| CN109607613A (en) * | 2018-12-11 | 2019-04-12 | 中南大学 | A method of with deionized water clean manufacturing high purity 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) |
| CN112408479A (en) * | 2020-12-13 | 2021-02-26 | 湖南众鑫新材料科技股份有限公司 | Process for preparing low-valence vanadium from ammonium metavanadate |
| CN112591795A (en) * | 2020-12-28 | 2021-04-02 | 湖南众鑫新材料科技股份有限公司 | Method for treating tail gas generated in preparation of low-valence vanadium from ammonium metavanadate |
| CN112591795B (en) * | 2020-12-28 | 2023-09-12 | 湖南众鑫新材料科技股份有限公司 | Treatment method for tail gas of low-valence vanadium prepared from ammonium metavanadate |
| CN115010176A (en) * | 2022-05-26 | 2022-09-06 | 湖南省银峰新能源有限公司 | Preparation method of high-purity vanadium pentoxide |
| CN115010176B (en) * | 2022-05-26 | 2024-06-07 | 湖南省银峰新能源有限公司 | Preparation method of high-purity vanadium pentoxide |
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Application publication date: 20121017 |