CN107662946A - The preparation method of vanadium trioxide - Google Patents
The preparation method of vanadium trioxide Download PDFInfo
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- CN107662946A CN107662946A CN201710685096.3A CN201710685096A CN107662946A CN 107662946 A CN107662946 A CN 107662946A CN 201710685096 A CN201710685096 A CN 201710685096A CN 107662946 A CN107662946 A CN 107662946A
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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
- C01G31/02—Oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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
- C01P2006/40—Electric properties
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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
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a kind of preparation method of the vanadium trioxide suitable for vanadium cell, comprise the following steps：Vanadium valence carries out liquid-phase reduction for the solvate of the ammonium vanadate and oxalic acid or oxalic acid of+5 valencys in reaction dissolvent, is evaporated reaction solution, calcines, produces.This method reduces using relatively inexpensive+5 valency ammonium vanadate being easy to get as raw material through oxalic acid, calcining, you can obtain the vanadium trioxide of high purity 99%, in addition to the transfer indfficiency in production process, the yield of vanadium is without other any losses.Production technology of the present invention is easy to operate, and energy consumption is low, safety, not high to equipment requirement, is adapted to industrialization large-scale production, can significantly reduce the production cost of vanadium trioxide.
Description
Technical field
The present invention relates to the preparation method of vanadium trioxide, belong to field of chemical material synthesis.
Background technology
Vanadium trioxide is a kind of important barium oxide, be widely used in high vanadium ferroalloy and VN alloy production, sensor,
The field such as new electronic component and battery production.Wherein, vanadium trioxide is in all-vanadium redox flow battery electrolyte production process
In there is good application prospect, reason is to reduce vanadic anhydride as reducing agent using vanadium trioxide to prepare the electrolysis of 3.5 valency vanadium
The method of liquid, its simple production process, reduction effect is good, and does not bring other impurity into, has chemical reduction method and electrolysis concurrently
Advantage, it is reduced the production cost of V electrolyte, therefore, the method is once proposition i.e. by the extensive pass of relevant industries
Note.However, because the preparation cost of current vanadium trioxide is high, product purity is low, make the method for this production V electrolyte by
Limitation is arrived.
At present, vanadium trioxide is mainly made by high-valence state vfanadium compound through reducing.The method of reduction includes additional solid
Reducing agent (e.g., sulphur, carbon dust, graphite etc.) reduces, reducibility gas (e.g., H2, CO etc.) reduction, ammonium vanadate decomposes, ammonia cracking
Reduction etc..Wherein, the method simple production process for adding the reducing agents such as graphite and carbon to reduce, but required reduction temperature is high, and product
In easily residual carbon or bring other impurities into；H2Or the reducing gas such as CO reduction effect is good, product purity is high, but combustion be present
The danger such as burning, blast or release of toxic gas；Ammonium vanadate decomposes, and caused ammonia is cracked into H2And N2Reduction prepares three oxidations two
Method cleaning, the environmental protection of vanadium, without adding any reducing agent, but because ammonia cracking is incomplete, reduction is insufficient, and pair sets
It is standby to require higher.More than in addition to several main preparation methods, hydrazonium salt containing vanadium can be also calcined under the conditions of protective gas, with
And add organic reducing agent to synthesize the tiny vanadium trioxide of uniform particle sizes by the methods of Hydrothermal Synthesiss or solvent heat again, and
The shortcomings of association area obtains preferable application effect, but these methods are there is to equipment requirement height, low production efficiency, leads
Cause the production cost of vanadium trioxide higher.
The content of the invention
It is an object of the invention to provide the preparation method of vanadium trioxide, with overcome existing production technology cost it is higher,
The defects of complex operation.
The invention provides the preparation method of vanadium trioxide, comprise the following steps：Vanadium valence for+5 valencys ammonium vanadate with
The solvate of oxalic acid or oxalic acid carries out liquid-phase reduction in reaction dissolvent, is evaporated reaction solution, calcining, produces.
Further, the Vanadium valence is that the ammonium vanadate of+5 valencys is ammonium metavanadate or ammonium poly-vanadate.
Further, the mole of vanadium and the mole ratio of oxalic acid are 1 in the ammonium vanadate：(1.5~3).
It is further preferred that the mole of vanadium and the mole ratio of oxalic acid are 1 in the ammonium vanadate：(1.5~2.5).
Further, in the ammonium vanadate vanadium mole：The volume of reaction dissolvent is 5~12mol/L.
It is further preferred that in the ammonium vanadate vanadium mole：The volume of reaction dissolvent is 8.5~10mol/L.
Further, reaction temperature is 80~100 DEG C.
It is further preferred that reaction temperature is 80~90 DEG C.
Further, calcine and carried out in protective atmosphere.
Further, the protective atmosphere be nitrogen, helium, argon gas, ammonia, CO, in gaseous alkanes one or two with
On mixture.
It is further preferred that the protective atmosphere is nitrogen.
Further, calcining heat is 700~1000 DEG C.
It is further preferred that calcining heat is 700~900 DEG C.
Further, calcination time is 1.5~5h.
It is further preferred that calcination time is 2~4h.
Further, the reaction dissolvent is water.
Further, the solvate of the oxalic acid is oxalic acid dihydrate.
Further, first it is dried before calcining；In drying process, to prevent presoma from being lumpd after drying, every 10-
20min need to carry out mechanical agitation to presoma.
The invention provides the preparation method of vanadium trioxide.This method using+5 valency ammonium vanadate cheap and easy to get as raw material,
Reduce, calcine, you can obtain the vanadium trioxide of high purity 99%, yield 100% (disregards transfer indfficiency) through oxalic acid.This hair
Open-birth production. art is easy to operate, and energy consumption is low, safety, not high to equipment requirement, is adapted to industrialization large-scale production, can significantly drop
The production cost of low vanadium trioxide.In addition, the V that this method obtains2O3Electrolyte suitable for preparing all-vanadium flow battery, will
It is 100cm that it, which is placed in effective area,2Vanadium cell in carry out charge and discharge cycles 40 times, the coulombic efficiency of battery be maintained at 96% with
On, energy efficiency is maintained at more than 80%, and coulombic efficiency and energy efficiency are almost undamped.In all-vanadium redox flow battery electrolyte
Had broad application prospects in production process.
Brief description of the drawings
Fig. 1 is vanadium trioxide production technology schematic diagram of the present invention；
Fig. 2 is that ammonium metavanadate and oxalic acid mol ratio are 1 in comparative example 1:The XRD diffraction spectras of 0.5 reaction products therefrom
Figure；
Fig. 3 is that ammonium metavanadate and oxalic acid mol ratio are 1 in comparative example 1:The XRD diffraction spectrograms of 1 reaction products therefrom；
Fig. 4 is the XRD diffraction spectrograms for calcining products therefrom in comparative example 2 in 400 DEG C；
Fig. 5 is the XRD diffraction spectrograms for calcining products therefrom in comparative example 2 in 450 DEG C；
Fig. 6 is the XRD diffraction spectrograms for calcining products therefrom in comparative example 2 in 500 DEG C；
Fig. 7 is the XRD diffraction spectrograms for calcining products therefrom in comparative example 2 in 550 DEG C；
Fig. 8 is the XRD diffraction spectrograms for calcining products therefrom in comparative example 2 in 600 DEG C；
Fig. 9 is the XRD diffraction spectrograms for calcining products therefrom in comparative example 2 in 650 DEG C；
Figure 10 is the XRD diffraction spectrograms for calcining products therefrom in comparative example 2 in 700 DEG C；
Figure 11 is battery charging and discharging coulombic efficiency and energy efficiency figure in test example 1；
Figure 12 is that ammonium metavanadate and oxalic acid mol ratio are 1 in test example 2:The XRD diffraction spectras of 1.5 reaction products therefroms
Figure；
Figure 13 is that ammonium metavanadate and oxalic acid mol ratio are 1 in test example 2:The XRD diffraction spectrograms of 2 reaction products therefroms；
Figure 14 is that ammonium metavanadate and oxalic acid mol ratio are 1 in test example 2:The XRD diffraction spectras of 2.5 reaction products therefroms
Figure；
Figure 15 is that ammonium metavanadate and oxalic acid mol ratio are 1 in test example 2:The XRD diffraction spectrograms of 3 reaction products therefroms.
Embodiment
The raw material that is used in the specific embodiment of the invention, equipment are known product, are obtained by buying commercially available prod.
The invention provides the preparation method of vanadium trioxide, comprises the following steps (production technology schematic diagram is shown in Fig. 1)：
1) ammonium metavanadate or ammonium poly-vanadate mix to (mixed proportion is the mole of vanadium with oxalic acid：The mole of oxalic acid=
1：1.5~1：2.5), it is added to (the mole of vanadium in the deionized water that temperature is 80~90 DEG C：The volume of water be 8.5~
10mol/L), liquid-phase reduction is carried out；
2) after ammonium metavanadate or ammonium poly-vanadate are completely dissolved, it is heated to seething with excitement, solution concentration is evaporated, obtains forerunner
Body；
3) gained presoma is calcined 2~4h under conditions of nitrogen protection and temperature is 700~900 DEG C, and in nitrogen
Room temperature is cooled under protection, produces vanadium trioxide.
In the production technology, it is (NH to obtain main component4)2(VO)2(C2O4)3With the presoma of oxalic acid mixture, due to
Carbon content is more, and reduction effect during calcining and decomposing is good；Moreover, intermediate product resolution produces ammonia, ammonia has reduction in itself
Property, protective effect is served, intermediate product can be made preferably to be reduced.For these reasons, preparation technology tool of the present invention
There is obvious advantage：1. can high-purity, obtain vanadium trioxide in high yield, and technology stability is strong, products obtained therefrom quality
It is stable；2. gained vanadium trioxide is highly suitable for preparing V electrolyte, the efficiency for charge-discharge of battery is good, it was demonstrated that it is applied
Effect is good.
In addition, the present invention further each Parameter Conditions in preparation technology are investigated, as a result find, consumption of oxalic acid and
The mutual cooperation of calcining heat has to product to be significantly affected.When the mole of vanadium and oxalic acid proportioning is less than 1:When 1.5, it is difficult to
To vanadium trioxide；Correspondingly, under conditions of calcining heat is less than 700 DEG C, even if adjusting consumption of oxalic acid repeatedly, three oxidations two
The purity of vanadium is also difficult to reach requirement.Under both specific cooperations, most product purity is improved to more than 99%, except production at last
During transfer indfficiency outside, the yield of vanadium is without other any losses.
At present, there is not yet preparing the report of vanadium trioxide by+5 valency ammonium vanadate and oxalic acid reaction.Compared to existing system
The standby additional solid reductant of technique (e.g., sulphur, carbon dust, graphite etc.) or reducibility gas (e.g., H2, CO etc.) etc. restoring method, this
Invention has the significant advantages such as production cost is low, easy to operate, safe.
Embodiment 1 prepares vanadium trioxide using present invention process
1) pure ammonium metavanadate will be analyzed and mix that (mixed proportion is the mole of vanadium with analyzing pure two oxalic acid hydrate：Oxalic acid
Mole=1：1.5) (the mole of vanadium in the deionized water that temperature is 80 DEG C, is added portionwise：Volume=10mol/ of water
L), liquid-phase reduction is carried out；
2) after ammonium metavanadate is completely dissolved, it is heated to seething with excitement, solution concentration is evaporated, obtains presoma；
3) after gained presoma is dried at 160 DEG C, it is calcined under conditions of being 700 DEG C in nitrogen protection and temperature
2.5h, and room temperature is cooled under nitrogen protection.The purity that vanadium trioxide is finally made is 98.8%.
Embodiment 2 prepares vanadium trioxide using present invention process
1) pure ammonium metavanadate will be analyzed and mix that (mixed proportion is the mole of vanadium with analyzing pure two oxalic acid hydrate：Oxalic acid
Mole=1：2) (the mole of vanadium in the deionized water that temperature is 95 DEG C, is added portionwise：Volume=9mol/L of water), enter
Row liquid-phase reduction；
2) after ammonium metavanadate is completely dissolved, it is heated to seething with excitement, solution concentration is evaporated, obtains presoma；
3) gained presoma is dried at 100 DEG C, 3h is calcined under conditions of being 750 DEG C in nitrogen protection and temperature, and
Room temperature is cooled under nitrogen protection.The purity that vanadium trioxide is finally made is 99.2%.
Embodiment 3 prepares vanadium trioxide using present invention process
1) pure ammonium metavanadate will be analyzed and mix that (mixed proportion is the mole of vanadium with analyzing pure two oxalic acid hydrate：Oxalic acid
Mole=1：2.5) temperature, is added portionwise as (the mole of vanadium in 85 DEG C of deionized waters：Volume=10mol/L of water),
Carry out liquid-phase reduction；
2) after ammonium metavanadate is completely dissolved, it is heated to seething with excitement, solution concentration is evaporated, obtains presoma；
3) gained presoma is dried at 200 DEG C, 2h is calcined under conditions of being 800 DEG C in nitrogen protection and temperature, and
Room temperature is cooled under nitrogen protection.The purity that vanadium trioxide is finally made is 99.4%.
Embodiment 4 prepares vanadium trioxide using present invention process
1) pure ammonium metavanadate will be analyzed and mix that (mixed proportion is the mole of vanadium with analyzing pure two oxalic acid hydrate：Oxalic acid
Mole=1：3) (the mole of vanadium in the deionized water that temperature is 90 DEG C, is added portionwise：Volume=8.5mol/L of water),
Carry out liquid-phase reduction；
2) after ammonium metavanadate is completely dissolved, it is heated to seething with excitement, solution concentration is evaporated, obtains presoma；
3) gained presoma is dried at 180 DEG C, 3h is calcined under conditions of being 900 DEG C in nitrogen protection and temperature, and
Room temperature is cooled under nitrogen protection.The purity that vanadium trioxide is finally made is 99.0%.
Influence of the preparation technology mesoxalic acid dosage of comparative example 1 to product
This experiment is by ammonium metavanadate and oxalic acid respectively 1:0.5、1:Reacted under 1 mol ratio, the presoma prepared in
It is calcined at lower 700 DEG C of nitrogen protective condition, obtains product, concrete technology condition is the same as embodiment 1.XRD is carried out to products therefrom to spread out
Analysis is penetrated, analysis result is as shown in Figure 2,3.
Fig. 2, the analysis of 3 XRD spectrum are understood, when the mol ratio of ammonium metavanadate and oxalic acid is 1:0.5、 1:When 1, institute
The main component for obtaining product is VO2、V3O5, and not target substance V2O3。
In addition, contrast test is also in ammonium metavanadate:Oxalic acid mol ratio 1:Consumption of oxalic acid, knot are further increased on the basis of 3
Fruit on the premise of calcining heat is not improved, be calcined products therefrom in agraphitic carbon content with the increase of oxalic acid addition and
Increase, XRD diffraction occur that amorphous carbon diffraction maximum miscellaneous peak is more and more obvious, and illustrating the purity of products therefrom significantly reduces.
Above result of the test shows that consumption of oxalic acid can be produced to finished product and significantly affected, and is determined in preparation technology of the present invention
Amount ranges in, i.e., the mole of vanadium and the mole ratio of oxalic acid are 1 in ammonium vanadate：, can be in high yield when (1.5~3)
The target product V of high-purity is prepared in ground2O3。
Influence of the calcining heat to product in the preparation technology of comparative example 2
Presoma is prepared according to embodiment 1, by presoma as in tube furnace, be passed through nitrogen protection, respectively at 400 DEG C,
450 DEG C, 500 DEG C, 550 DEG C, 600 DEG C, 650 DEG C, 700 DEG C of roasting 4h, after the completion of roasting, continue logical nitrogen, until furnace temperature drops to
Room temperature.XRD diffraction analysis is carried out to products therefrom, analysis result is as shown in Fig. 4~10.
From Fig. 4~10 as can be seen that with the continuous rise of sintering temperature, V2O3Diffraction maximum it is more and more obvious, miscellaneous peak is got over
Come weaker.Illustrating when less than 700 DEG C of roasting temperatures, presoma decomposes not exclusively, and the content of amorphous carbon is more in product,
Product purity is not high；When calcining heat is higher than 700 DEG C, presoma complete decomposition, carbon therein is stronger to the reducing power of vanadium, energy
Access the V of high-purity2O3。
Beneficial effects of the present invention are proved below by way of test example.
Test example 1 prepares vanadium cell using vanadium trioxide of the present invention as raw material
It is 4.2 in molar ratio by vanadic anhydride and according to embodiments of the present invention 1 vanadium trioxide prepared:1 ratio
Mixing, add 6mol/L sulfuric acid, react 120min at 90 DEG C, after being cooled to room temperature, filtering, determine filtrate in trivalent vanadium and
Content (the V of pentavalent vanadium+3：V+5=1.04:1) H in deionized water regulation solution, is added2SO4Concentration is 3mol/L, total V density
For 2mol/L.Taking the equivalent electrolyte to be respectively placed in the both positive and negative polarity fluid reservoir of vanadium cell, (effective area of vanadium cell is
100cm2), with 40mA/cm2Current density carry out constant current charge-discharge circulate 40 times, the energy efficiency and coulombic efficiency of battery are such as
Shown in Figure 11.
It can be seen from figure 11 that the coulombic efficiency of battery is maintained at more than 96%, energy efficiency is maintained at more than 80%, and
Coulombic efficiency and energy efficiency are almost undamped, illustrate the functional of the electrolyte.
Above result of the test shows, the V prepared using the inventive method2O3Electricity suitable for preparing all-vanadium flow battery
Solve liquid, its purity can reach the requirement for preparing vanadium cell, and production cost substantially reduces in addition, be advantageous to using vanadium trioxide as
The method that reducing agent reduction vanadic anhydride prepares 3.5 valency V electrolytes obtains further genralrlization application.
The checking test of 2 preparation technology of the present invention of test example
Ammonium metavanadate is with oxalic acid respectively 1:1.5、1:2、1:2.5、1:Reacted under 3 mol ratios, the presoma prepared
It is calcined at lower 700 DEG C of nitrogen protective condition, obtains reduzate, process conditions are the same as embodiment 1.Products therefrom carries out XRD and spread out
Analysis is penetrated, analysis result is as shown in Figure 12~15.
XRD spectrum analysis to Figure 12~15 understands that the main component of this several product is V2O3。
Above result of the test shows that stable preparation process of the present invention is reliable, products obtained therefrom steady quality.
Claims (10)
1. the preparation method of vanadium trioxide, it is characterized in that：Comprise the following steps：Vanadium valence for+5 valencys ammonium vanadate and oxalic acid or
The solvate of oxalic acid carries out liquid-phase reduction in reaction dissolvent, is evaporated reaction solution, calcining, produces.
2. preparation method as claimed in claim 1, it is characterized in that：The Vanadium valence be+5 valencys ammonium vanadate be ammonium metavanadate or
Ammonium poly-vanadate.
3. preparation method as claimed in claim 1 or 2, it is characterized in that：The mole of vanadium and oxalic acid rubs in the ammonium vanadate
Your amount ratio is 1：(1.5~3)；Preferably 1：(1.5~2.5).
4. the preparation method as described in claims 1 to 3 any one, it is characterized in that：The mole of vanadium in the ammonium vanadate：Instead
The volume for answering solvent is 5~12mol/L；Preferably 8.5~10mol/L.
5. preparation method as claimed in claim 1, it is characterized in that：The temperature of liquid-phase reduction is 80~100 DEG C；Preferably 80~
90℃。
6. preparation method as claimed in claim 1, it is characterized in that：Calcining is carried out in protective atmosphere.
7. preparation method as claimed in claim 6, it is characterized in that：The protective atmosphere be nitrogen, helium, argon gas, ammonia,
One or more kinds of mixture in CO, gaseous alkanes；Preferably nitrogen.
8. the preparation method as described in claim 1,6 or 7 any one, it is characterized in that：Calcining heat is 700~1000 DEG C；
Preferably 700~900 DEG C.
9. the preparation method as described in any one of claim 1 or 6~8, it is characterized in that：Calcination time is 1.5~5h；It is preferred that
For 2~4h.
10. preparation method as claimed in claim 1, it is characterized in that：The reaction dissolvent is water.
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| CN108314083A (en) * | 2018-04-04 | 2018-07-24 | 河钢股份有限公司承德分公司 | A method of by preparing vanadium trioxide containing vanadium solution |
| 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 |
| CN110581284A (en) * | 2019-09-30 | 2019-12-17 | 陕西科技大学 | Electrocatalysis function V2O3Preparation method and application of @ Co |
| CN110857222A (en) * | 2018-08-23 | 2020-03-03 | 南京理工大学 | Preparation method of vanadium trioxide powder |
| CN110857223A (en) * | 2018-08-23 | 2020-03-03 | 南京理工大学 | Preparation method of high-purity vanadium trioxide powder |
| CN112408478A (en) * | 2020-12-02 | 2021-02-26 | 中国科学院过程工程研究所 | Preparation method of vanadium trioxide |
| CN114293321A (en) * | 2021-12-30 | 2022-04-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Low-cost room-temperature rapid batch preparation method and equipment for special-shaped vanadium oxide nanofibers and aggregates thereof |
| CN114684854A (en) * | 2022-03-30 | 2022-07-01 | 东风汽车集团股份有限公司 | Preparation method of nano vanadium trioxide |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108314083A (en) * | 2018-04-04 | 2018-07-24 | 河钢股份有限公司承德分公司 | A method of by preparing vanadium trioxide containing vanadium solution |
| CN108314083B (en) * | 2018-04-04 | 2020-11-03 | 河钢股份有限公司承德分公司 | Method for preparing vanadium trioxide from vanadium-containing solution |
| 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 |
| CN110857222A (en) * | 2018-08-23 | 2020-03-03 | 南京理工大学 | Preparation method of vanadium trioxide powder |
| CN110857223A (en) * | 2018-08-23 | 2020-03-03 | 南京理工大学 | Preparation method of high-purity vanadium trioxide powder |
| CN110581284A (en) * | 2019-09-30 | 2019-12-17 | 陕西科技大学 | Electrocatalysis function V2O3Preparation method and application of @ Co |
| CN110581284B (en) * | 2019-09-30 | 2020-12-08 | 陕西科技大学 | Electrocatalysis function V2O3Preparation method and application of @ Co |
| CN112408478A (en) * | 2020-12-02 | 2021-02-26 | 中国科学院过程工程研究所 | Preparation method of vanadium trioxide |
| CN114293321A (en) * | 2021-12-30 | 2022-04-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Low-cost room-temperature rapid batch preparation method and equipment for special-shaped vanadium oxide nanofibers and aggregates thereof |
| CN114293321B (en) * | 2021-12-30 | 2023-02-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Low-cost room-temperature rapid batch preparation method and equipment for special-shaped vanadium oxide nanofibers and aggregates thereof |
| CN114684854A (en) * | 2022-03-30 | 2022-07-01 | 东风汽车集团股份有限公司 | Preparation method of nano vanadium trioxide |
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