CN109534399A - A kind of method that hydro-thermal reaction prepares high purity vanadic anhydride - Google Patents
A kind of method that hydro-thermal reaction prepares high purity vanadic anhydride Download PDFInfo
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- CN109534399A CN109534399A CN201910008107.3A CN201910008107A CN109534399A CN 109534399 A CN109534399 A CN 109534399A CN 201910008107 A CN201910008107 A CN 201910008107A CN 109534399 A CN109534399 A CN 109534399A
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- vanadium
- vanadic anhydride
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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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- 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 present invention relates to a kind of methods that hydro-thermal reaction prepares high purity vanadic anhydride.Its technical solution is: by urea: the mass ratio containing vanadic anhydride in vanadium solution is (1~8): 1, the urea and the vanadium solution that contains are placed in reaction kettle, 0.5~4h is stirred under the conditions of 120~300 DEG C, obtains pentavalent vanadate slurry；The pentavalent vanadate slurry is separated by solid-liquid separation, vanadate and filtrate are obtained；The vanadate is calcined into 0.5~1.5h under the conditions of 400~600 DEG C, obtains high purity vanadic anhydride.The vanadium ion containing in vanadium solution exists in the form of five valence states, and the pH value containing vanadium solution is -0.4~0 or 7~9.The present invention has the characteristics that simple process, at low cost and high production efficiency；The high purity vanadic anhydride yield prepared with this method is high and with high purity.
Description
Technical field
The invention belongs to prepare high purity vanadic anhydride technical field.High-purity five oxygen is prepared more particularly to a kind of hydro-thermal reaction
Change the method for two vanadium.
Background technique
Vanadic anhydride is the important compound of vanadium, is widely used in fields such as metallurgy, chemical industry, material and batteries.
Vanadium aluminium intermediate alloy is produced with high purity vanadic anhydride, resulting vananum is added in titanium alloy, various boats are processed into
Empty component；Electrode material of lithium battery is prepared with high purity vanadic anhydride, resulting electrode material can greatly improve lithium battery
Capacity and battery cycle life；High purity vanadic anhydride is the main source of all-vanadium redox flow battery electrolyte, all-vanadium flow battery
Have the advantages that large capacity, long-life and quick response, is the research hotspot of extensive energy storage technology.High-purity five oxygen is prepared at present
The main method for changing two vanadium is: the alkali soluble of solid containing vanadium purification and impurity removal-ammonium salt precipitation；The precipitation of ammonium salt containing vanadium solution-alkali soluble removal of impurities-is again
Precipitation.
" preparation method of high purity vanadium metal high purity vanadic anhydride " (CN201610036137.1) patented technology proposes
Vanadic anhydride is carried out alkali soluble and filtering by a kind of preparation method of high purity vanadic anhydride, and filtered liquid carries out pH
Value is adjusted, and desiliconizing agent precipitating, filtering is added, and chromium remover precipitating filtering is added in filtered liquid, then adjusts solution ph, is added
Ammonium chloride precipitation, filtration washing obtain high-purity ammonium metavanadate, and calcinations of ammonium metavanadate obtains high purity vanadic anhydride.The technique passes through
Impurity-removing precipitating several times, is obtained by filtration the lower solution of impurity content, and the mode by reprecipitation prepares high purity vanadic anhydride, work
Skill long flow path, removal of impurities and precipitation reagent consumption are high, so that high production cost and production efficiency is lower.
A kind of " high purity vanadic anhydride preparation method " (CN106430307B) patented technology, proposes acid precipitation and alkali
Property precipitation combine, hydrolysis precipitation cleans the preparation method that combines with cation exchange.First in acid condition with hydrolysis precipitation
Partial impurities are removed, resulting vanadium hydrolysate is dissolved with sodium hydroxide, are filtered to remove precipitated impurities, cation is recycled to hand over
It changes resin and removes micro metal cation impurity；It recycles liquid that ammonia-sinking is added to form sediment, washing, calcining, obtains high-purity five oxidation two
Vanadium.The invention obtains five high-purity oxygen using multiple precipitation, dissolution and resin adsorption desorption removal impurity, last ammonium salt precipitation
Change two vanadium, the process of preparation is longer, and soda acid medicament and resin consumption and energy consumption are larger, although product purity is high, production is imitated
Rate is low.
" a method of V electrolyte high purity vanadic anhydride is prepared with sodium vanadium vanadium extraction liquid " (CN106145188A)
Patented technology proposes a kind of method that high purity vanadic anhydride is prepared from sodium vanadium solution.Sulphur is added into sodium vanadium liquid
Sour ammonium, then sodium vanadate is obtained by filtration with sulphur acid for adjusting pH precipitating, it is redissolved sodium vanadate, when pH is 7~11, is added and contains ammonium or ammonia
Medium, precipitated crystal obtain ammonium metavanadate, then hot water dissolving's ammonium metavanadate and carry out again repeat precipitated crystal process, obtain
Ammonium metavanadate obtains high purity vanadic anhydride by calcining.The invention is using multiple precipitating course of dissolution come purified solution enrichment
Vanadium consumes a large amount of soda acid, and process flow is long, high production cost, and energy consumption is high and production efficiency is low.
" a method of from acid more impurity containing precipitation direct in vanadium solution " (CN106319214B) patented technology, it proposes
A kind of method of precipitation direct from containing vanadium solution.It is directly in mass ratio (3~20) to more impurity acid solutions containing vanadium: 1
Urea is added, stirs 1.0~6.0h, precipitating under the conditions of 40~70 DEG C, product calcines 0.5 under the conditions of 450~650 DEG C~
3.0h obtains high-purity vanadium pentoxide.The technology is compared with other high purity vanadic anhydride technologies of preparing, though reduce removal of impurities
Process and process is shortened, high-purity vanadium pentoxide directly is made from containing one step of vanadium solution.But precipitation time longest reaches
6h, the time is longer, and the consumption of urea is up to 20: 1, and reagent consumption is still higher, and purity of vanadium pentoxide is only capable of
Reach 99%.
From the prior art, the technology of preparing of vanadic anhydride is mostly molten with ammonium metavanadate, vanadic anhydride at present
Liquid is raw material containing vanadium solution, is cleaned by alkali soluble removal of impurities-ammonium salt precipitation or vanadium solution purification and impurity removal-ammonium salt precipitating-alkali soluble
The method of precipitation again, its shortcoming is that complex process is tediously long, reagent consumption is big；Or from " one kind contains vanadium solution from acid more impurity
In direct precipitation method " from the point of view of (CN106319214B) patented technology, urea precipitation is directlyed adopt under normal pressure, there is the times
The problem of long (for up to 6h), reagent consumption high (ammonium coefficient is added to be 20) and purity relatively low (being only capable of reaching 99%).To sum up institute
State, existing high purity vanadic anhydride preparation method there is complex process, long flow path, reagent cost is big, energy consumption is high, production effect
The problem of rate is low and product purity is low.
Summary of the invention
The present invention is directed to overcome the deficiencies of existing technologies, and it is an object of the present invention to provide a kind of simple process, at low cost, production efficiency
The method that high hydro-thermal reaction prepares high purity vanadic anhydride；The high purity vanadic anhydride yield height and purity prepared with this method
It is high.
To achieve the above object, steps are as follows for the technical solution adopted by the present invention:
Step 1: pressing urea: the mass ratio containing vanadic anhydride in vanadium solution is (1~8): 1, by the urea and described
It is placed in reaction kettle containing vanadium solution, 0.5~4h is stirred under the conditions of 120~300 DEG C, obtains pentavalent vanadate slurry.
Step 2: the pentavalent vanadate slurry is separated by solid-liquid separation, vanadate and filtrate are obtained.
Step 3: the vanadate is calcined 0.5~1.5h under the conditions of 400~600 DEG C, high-purity five oxidation two is obtained
Vanadium.
The vanadium ion containing in vanadium solution exists in the form of five valence states.
The vanadium solution that contains is one of following two kinds of solution:
The chemical component of the first solution is: vanadium ion concentration is 8~50g/L, and iron concentration is less than 2g/L, aluminium
Ion concentration is less than 25g/L, and calcium ion concentration is less than 1g/L, and silicon ion concentration is less than 0.1g/L, and phosphate ion concentration is less than 0.1g/
L；The pH value containing vanadium solution is -0.4~0.
The chemical component of second of the solution is: vanadium ion concentration is 8~50g/L, and iron concentration is less than 0.1g/L,
Aluminium ion concentration is less than 1g/L, and silicon ion concentration is less than 2g/L, and phosphate ion concentration is less than 2g/L；The pH value containing vanadium solution is
7~9.
Due to using the above method, the present invention has the positive effect that compared with prior art:
1, high purity vanadic anhydride is made using one step of hydro-thermal reaction due to the present invention, eliminates and is sunk by ammonium salt containing vanadium solution
Shallow lake prepares the processes such as intermediate products and alkali soluble purification and impurity removal, simplifies technique, shortens process.
2, it since the present invention is that high purity vanadic anhydride is made from containing a step in vanadium solution, saves Partial cleansing except general labourer
Skill reduces the consumption of soda acid and other removal of impurities medicaments, with it is existing " it is a kind of from acid more impurity containing directly heavy in vanadium solution
The method of vanadium " (CN106319214B) (hereinafter referred to as " direct precipitation technology ") patented technology is compared, and the calcination process stage forges
Burning temperature reduces 50~150 DEG C, reduces energy consumption, reduces production cost.
3, the present invention is compared with " direct precipitation technology ": the consumption of urea of the invention is only the three of " direct precipitation technology "
2/1 mono- to five, the production time is the half of " direct precipitation technology " production time to 2/3rds.The present invention
The production time is also reduced while reducing reagent consumption, greatly reduces energy consumption.
4, the prior art is shown, after purity of vanadium pentoxide reaches 99%, if purity improves 0.2~0.5% again, is needed again
By the process of three to five alkali soluble removal of impurities reprecipitations.Precipitation rate of the invention is 99.2% or more, product purity 99.5%
More than, hence it is evident that it is higher than " direct precipitation technology " (precipitation rate is 98.5%, purity 99%).Product purity and life i.e. of the invention
It produces efficiency and is significantly better than the prior art.
Therefore, the present invention has the characteristics that simple process, at low cost and high production efficiency；High-purity five prepared with this method
V 2 O yield is high and with high purity.
Specific embodiment
The present invention will be further described With reference to embodiment, not to the limitation of its protection scope:
Embodiment 1
A kind of method that hydro-thermal reaction prepares high purity vanadic anhydride.The present embodiment the method comprises the concrete steps that:
Step 1: pressing urea: the mass ratio containing vanadic anhydride in vanadium solution is (1~3): 1, by the urea and described
It is placed in reaction kettle containing vanadium solution, 0.5~1.5 is stirred under the conditions of 120~200 DEG C, obtains pentavalent vanadate slurry.
Step 2: the pentavalent vanadate slurry is separated by solid-liquid separation, vanadate and filtrate are obtained.
Step 3: the vanadate is calcined 1.0~1.5h under the conditions of 400~450 DEG C, high-purity five oxidation two is obtained
Vanadium.
The vanadium ion containing in vanadium solution exists in the form of five valence states.
The chemical component containing vanadium solution are as follows: 8~30g/L of vanadium ion concentration, iron concentration are less than 2g/L, aluminium ion
Concentration is less than 25g/L, and calcium ion concentration is less than 1g/L, and silicon ion concentration is less than 0.1g/L, and phosphate ion concentration is less than 0.1g/L；Institute
Stating the pH value containing vanadium solution is -0.4~-0.2.
The yield of vanadic anhydride is greater than 99.2% in the present embodiment；Purity of vanadium pentoxide obtained is greater than 99.8%.
Embodiment 2
A kind of method that hydro-thermal reaction prepares high purity vanadic anhydride.The present embodiment the method comprises the concrete steps that:
Step 1: pressing urea: the mass ratio containing vanadic anhydride in vanadium solution is (3~5): 1, by the urea and described
It is placed in reaction kettle containing vanadium solution, 1~2h is stirred under the conditions of 200~250 DEG C, obtains pentavalent vanadate slurry.
Step 2: the pentavalent vanadate slurry is separated by solid-liquid separation, vanadate and filtrate are obtained.
Step 3: the vanadate is calcined 0.5~1.0h under the conditions of 450~500 DEG C, high-purity five oxidation two is obtained
Vanadium.
Described exists in the form of five valence states containing the vanadium ion in vanadium solution.
The chemical component containing vanadium solution are as follows: 30~50g/L of vanadium ion concentration, iron concentration be less than 2g/L, aluminium from
Sub- concentration is less than 25g/L, and calcium ion concentration is less than 1g/L, and silicon ion concentration is less than 0.1g/L, and phosphate ion concentration is less than 0.1g/L；
The pH value containing vanadium solution is -0.2~0.
The yield of vanadic anhydride is greater than 99.5% in the present embodiment；Purity of vanadium pentoxide obtained is greater than 99.7%.
Embodiment 3
A kind of method that hydro-thermal reaction prepares high purity vanadic anhydride.The present embodiment the method comprises the concrete steps that:
Step 1: pressing urea: the mass ratio containing vanadic anhydride in vanadium solution is (4~6): 1, by the urea and described
It is placed in reaction kettle containing vanadium solution, 3~4h is stirred under the conditions of 250~300 DEG C, obtains pentavalent vanadate slurry.
Step 2: the pentavalent vanadate slurry is separated by solid-liquid separation, vanadate and filtrate are obtained.
Step 3: the vanadate is calcined 0.5~1.0h under the conditions of 550~600 DEG C, high-purity five oxidation two is obtained
Vanadium.
Described exists in the form of five valence states containing the vanadium ion in vanadium solution.
The chemical component containing vanadium solution are as follows: 8~35g/L of vanadium ion concentration, iron concentration be less than 0.1g/L, aluminium from
Sub- concentration be less than 1g/L, silicon ion concentration be less than 2g/L, phosphate ion concentration be less than 2g/L, the pH value containing vanadium solution be 7~
8。
The yield of vanadic anhydride is greater than 99.3% in the present embodiment；Purity of vanadium pentoxide obtained is greater than 99.5%.
Embodiment 4
A kind of method that hydro-thermal reaction prepares high purity vanadic anhydride.The present embodiment the method comprises the concrete steps that:
Step 1: pressing urea: the mass ratio containing vanadic anhydride in vanadium solution is (6~8): 1, by the urea and described
It is placed in reaction kettle containing vanadium solution, 2~3h is stirred under the conditions of 240~280 DEG C, obtains pentavalent vanadate slurry.
Step 2: the pentavalent vanadate slurry is separated by solid-liquid separation, vanadate and filtrate are obtained.
Step 3: the vanadate is calcined 1.0~1.5h under the conditions of 500~550 DEG C, high-purity five oxidation two is obtained
Vanadium.
Described exists in the form of five valence states containing the vanadium ion in vanadium solution.
The chemical component containing vanadium solution is: vanadium ion concentration is 8~50g/L, and iron concentration is less than 0.1g/L, aluminium
Ion concentration is less than 1g/L, and silicon ion concentration is less than 2g/L, and phosphate ion concentration is less than 2g/L；The pH value containing vanadium solution is 8
~9.
The yield of vanadic anhydride is greater than 99.8% in the present embodiment；Purity of vanadium pentoxide obtained is greater than 99.7%.
Present embodiment has the positive effect that compared with prior art:
1, high purity vanadic anhydride is made using one step of hydro-thermal reaction due to present embodiment, eliminated by molten containing vanadium
Liquid ammonium salt precipitating prepares the processes such as intermediate products and alkali soluble purification and impurity removal, simplifies technique, shortens process.
2, it since present embodiment is that high purity vanadic anhydride is made from containing a step in vanadium solution, saves Partial cleansing
Impurity removal process reduces the consumption of soda acid and other removal of impurities medicaments, with it is existing " it is a kind of from acid more impurity containing in vanadium solution
The method of direct precipitation " (CN106319214B) (hereinafter referred to as " direct precipitation technology ") patented technology is compared, calcination process rank
The calcination temperature of section reduces 50~150 DEG C, reduces energy consumption, reduces production cost.
3, present embodiment is compared with " direct precipitation technology ": the consumption of the urea of present embodiment is only
For the one third of " direct precipitation technology " to 2/5ths, the production time is the half of " direct precipitation technology " production time
To 2/3rds.Present embodiment also reduces the production time while reducing reagent consumption, greatly reduces energy
Consumption.
4, the prior art is shown, after purity of vanadium pentoxide reaches 99%, if purity improves 0.2%~0.5% again, is needed
Using the process of three to five alkali soluble removal of impurities reprecipitations.For the precipitation rate of present embodiment 99.2% or more, product is pure
Degree is 99.5% or more, hence it is evident that is higher than the prior art (precipitation rate is 98.5%, purity 99%).That is present embodiment
Product purity and production efficiency are significantly better than the prior art and " direct precipitation technology ".
Therefore, present embodiment has the characteristics that simple process, at low cost and high production efficiency；It is prepared with this method
High purity vanadic anhydride yield is high and purity is high.
Claims (2)
1. a kind of method that hydro-thermal reaction prepares high purity vanadic anhydride, it is characterised in that specific step is as follows for the method:
Step 1: press urea: the mass ratio containing vanadic anhydride in vanadium solution be (1~8): 1, by the urea and it is described contain vanadium
Solution is placed in reaction kettle, and 0.5~4h is stirred under the conditions of 120~300 DEG C, obtains pentavalent vanadate slurry；
Step 2: the pentavalent vanadate slurry is separated by solid-liquid separation, vanadate and filtrate are obtained；
Step 3: the vanadate is calcined 0.5~1.5h under the conditions of 400~600 DEG C, high purity vanadic anhydride is obtained；
The vanadium ion containing in vanadium solution exists in the form of five valence states.
2. the method that hydro-thermal reaction according to claim 1 prepares high purity vanadic anhydride, it is characterised in that described to contain vanadium
Solution is one of following two kinds of solution:
The chemical component of the first solution is: vanadium ion concentration is 8~50g/L, and iron concentration is less than 2g/L, aluminium ion
Concentration is less than 25g/L, and calcium ion concentration is less than 1g/L, and silicon ion concentration is less than 0.1g/L, and phosphate ion concentration is less than 0.1g/L；Institute
Stating the pH value containing vanadium solution is -0.4~0；
The chemical component of second of the solution is: vanadium ion concentration be 8~50g/L, iron concentration be less than 0.1g/L, aluminium from
Sub- concentration is less than 1g/L, and silicon ion concentration is less than 2g/L, and phosphate ion concentration is less than 2g/L；The pH value containing vanadium solution be 7~
9。
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Cited By (2)
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| CN110416535A (en) * | 2019-07-25 | 2019-11-05 | 三峡大学 | A kind of preparation method of self-supporting NaxV2O5 nano wire sodium-ion battery array material |
| CN114291846A (en) * | 2021-11-19 | 2022-04-08 | 攀钢集团研究院有限公司 | Preparation method of nano vanadium pentoxide cathode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110416535A (en) * | 2019-07-25 | 2019-11-05 | 三峡大学 | A kind of preparation method of self-supporting NaxV2O5 nano wire sodium-ion battery array material |
| CN114291846A (en) * | 2021-11-19 | 2022-04-08 | 攀钢集团研究院有限公司 | Preparation method of nano vanadium pentoxide cathode material |
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