CN106629846A - Method for preparing ammonium polyvanadate from sodiumizing, roasting and leaching solution - Google Patents
Method for preparing ammonium polyvanadate from sodiumizing, roasting and leaching solution Download PDFInfo
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- C01—INORGANIC CHEMISTRY
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Abstract
The invention discloses a method for preparing ammonium polyvanadate from a sodiumizing, roasting and leaching solution. The method comprises the following steps: adding an alkaline substance into the sodiumizing, roasting and leaching solution, stirring and filtering to obtain a sodium vanadate solution; adjusting the pH, then adding an impurity removing agent, stirring and filtering to obtain a sodiumizing, vanadium-extracting and purifying solution; adding a vanadium precipitating agent, adjusting the pH, heating, stirring and filtering to obtain ammonium polyvanadate crystals; washing and drying to obtain the ammonium polyvanadate. By the method, the iron content and the silicon content of the ammonium polyvanadate are greatly reduced, so that the Fe element content is reduced to 0.0038-0.0096wt% and the Si element content is reduced to 0.0032-0.0061wt%; meanwhile, the contents of other impurity elements are reduced, and requirements on low iron, low silicon and low impurity of the ammonium polyvanadate in the production of vanadium products are met. The preparation method provided by the invention is simple in process and easy to implement, and is suitable for industrial production.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of technology of preparing of ammonium poly-vanadate, more particularly to one kind is by sodium
The method that Roasting And Leaching liquid prepares ammonium poly-vanadate.
Background technology
Vanadium has numerous excellent physical properties and chemical property, and purposes is quite varied, there is the title of metal " vitamin ".With
Developing by leaps and bounds for scientific and technological level, requirement of the mankind to new material is increasingly improved, and the application of vanadium is more and more extensive, its scope
Cover the various fields such as Aero-Space, chemistry, battery, pigment, glass, optics, medicine.Vanadium content is very high in ammonium vanadate, is
The main raw material in vanadium production field.
Deng is fallen vivid et al. the containing vanadium and chromium waste residue reclaimed with vanadium products factory vanadium-containing water that have studied and prepares many vanadic acid as raw material
The technique of ammonium.The technique is will to obtain carrying out purification and impurity removal, concentration, precipitation containing vanadium solution from containing vanadium and chromium waste residue, is obtained many
Ammonium vanadate.By control condition：PH=1.8-2.2,95 DEG C of temperature, plus ammonium coefficient are 4, reach can vanadium recovery
95.77% (referring to " preparing the technical study of ammonium poly-vanadate using the vanadium and chromium-containing slag reclaimed in vanadium waste processed ", Deng falls vivid, Ye Yu
Tinkling of pieces of jade etc., Chemical Engineering Technology and exploitation, 2012,41 (4):15-17).
CN101157478 discloses a kind of preparation method of ammonium poly-vanadate of knowing clearly, and the method is first to containing addition in vanadium leachate
PH value is adjusted after calcium salt soln to alkalescence, vanadic acid calcium precipitate is obtained after heating stirring, be added to containing leaching agent after filtration, washing
In solution, heating is filtered after a period of time, and filtrate is adjusted into pH value to 1.8-2.5, at 90 DEG C under the conditions of seething with excitement, stirs 40-
Precipitation after 60min is filtrated to get ammonium poly-vanadate.
CN103952565A discloses a kind of method that vanadium slag ammonium salt leaching prepares ammonium metavanadate, and the method is by the pre- oxygen of vanadium slag
Leached with ammonium salt aqueous solution after change, crystallisation by cooling and separated after solid-liquor separation, obtain ammonium metavanadate crystal.
CN102502823A discloses a kind of preparation method of the ammonium poly-vanadate of high-tap density, adds in solution containing vanadium many
Ammonium vanadate crystal seed and ammonium sulfate, adjust and heated up after pH, and ammonium poly-vanadate is precipitated under fast stirring, after adding ammonium sulfate twice, drop
Then low mixing speed is filtered, is washed, is dried to obtain high-tap density ammonium poly-vanadate precipitating ammonium poly-vanadate.
CN103420416A discloses a kind of preparation method of ammonium metavanadate, and the method is included sodium vanadate solution and ammonium salt
Contact in acid condition, the product after contact is precipitated and isolated ammonium poly-vanadate solid, by ammonium poly-vanadate solid
Contact with water and ammonium vanadate reconstruction agent so that ammonium poly-vanadate is changed into ammonium metavanadate, and the product after contact is carried out into solid-liquid
Separate, obtain ammonium metavanadate solution.
From the foregoing, it will be observed that as the ammonium vanadate of vanadium products material, either ammonium poly-vanadate or ammonium metavanadate, the life of conventional products
Production. art is more, and according to the difference of the purposes of various vanadium products, the requirement to the product composition of ammonium vanadate is also different, its preparation side
Method also respectively has the similarities and differences.In some high-end vanadium products, such as vananum, the production process of V electrolyte product, to impurity element
Requirement it is particularly severe, it is particularly particularly strict to the content requirement of iron therein, silicon, many vanadic acid of extraordinary requirement are related at present
In ammonium product, low iron, the production technology of low silicon ammonium poly-vanadate are not yet seen in report.
The content of the invention
Not enough for more than, the present invention provides a kind of method for preparing ammonium poly-vanadate by sodium roasting leachate, obtains
The content of Fe elements is down to 0.0038-0.0096wt%, and the content of Si elements is down to 0.0032-0.0061wt%, other impurities
The ammonium poly-vanadate product that the content of element is also greatly reduced.
To reach above-mentioned purpose, the present invention provides technical scheme below：
The present invention provides a kind of method for preparing ammonium poly-vanadate by sodium roasting leachate, and methods described includes following step
Suddenly：
(1) alkaline matter is added in sodium roasting leachate, is filtered after stirring, obtain sodium vanadate solution；
(2) pH of regulating step (1) sodium vanadate solution, is subsequently adding cleaner, sodium is obtained after agitation and filtration and is carried
Vanadium scavenging solution；
(3) precipitation agent is added in step (2) the sodium vanadium extraction scavenging solution, pH is adjusted, heating stirring is obtained after filtration
Ammonium poly-vanadate crystal；
(4) step (3) the ammonium poly-vanadate crystal is washed with water, after being dried ammonium poly-vanadate is obtained.
Sodium roasting leachate of the present invention refers to vanadium slag with the leachate obtained after sodium carbonate, sodium chloride roasting.It is logical
Sodium roasting is carried out to vanadium slag after first, removes a part of impurity element, obtain the sodium roasting that v element obtains preliminary purification
Leachate, then it is processed through the preparation method for providing of the invention, you can obtain low iron, the ammonium poly-vanadate of low silicon is produced
Product.When sodium roasting leachate is processed, iron and silicon contains the preparation method that the present invention is provided in the ammonium poly-vanadate product of acquisition
Amount well below directly with this method directly process vanadium slag or other contain vanadium leachate.
Heretofore described stirring is carried out from this area conventional technique means, and particular determination is not done to this.It is exemplary
Ground, the stirring can be mechanical agitation；For the time of stirring does not equally limit, stirring is until there is no longer precipitation appearance i.e.
Can.
Heretofore described filtration is carried out from this area conventional technique means, and particular determination is not done to this.It is exemplary
Ground, described filtration selects vacuum cycle pump to carry out.
According to the present invention, the concentration of vanadium is 15-40g/L in step (1) the sodium roasting leachate, for example, can be
15g/L, 18g/L, 20g/L, 23g/L, 25g/L, 28g/L, 30g/L, 32g/L, 35g/L, 38g/L or 40g/L, and above-mentioned number
Concrete point value between value, as space is limited and for simple and clear consideration, the present invention tool that no longer scope described in exclusive list includes
Body point value.
According to the present invention, the temperature of step (1) the sodium roasting leachate is 30-100 DEG C, for example can be 30 DEG C,
35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C or 100 DEG C, and
Concrete point value between above-mentioned numerical value, as space is limited and for simple and clear consideration, scope bag no longer described in exclusive list of the invention
The concrete point value for including.The temperature of the sodium roasting leachate is preferably 60-80 DEG C.
The temperature of step (1) the sodium roasting leachate is to obtain after sodium roasting in actual production process in the present invention
The temperature that leachate is taken out of, therefore it need not again be heated.
According to the present invention, step (1) alkaline matter be in piece alkali, liquid caustic soda or ammonia any one or at least two
Combination, for example, can be any one in piece alkali, liquid caustic soda or ammonia, example but non-limiting be combined as piece alkali and liquid caustic soda, piece
Alkali and ammonia, liquid caustic soda and ammonia, piece alkali, liquid caustic soda and ammonia.
According to the present invention, pH >=12 of sodium roasting leachate after step (1) the addition alkaline matter for example can be
12nd, the concrete point value between 12.2,12.4,12.6,12.8,13,13.2,13.4,13.6,13.8 or 14, and above-mentioned numerical value,
As space is limited and for simple and clear consideration, the present invention concrete point value that no longer scope described in exclusive list includes.The addition alkali
Afterwards the pH of sodium roasting leachate is preferably 12.
From the temperature and pH of above-mentioned preferred sodium roasting leachate, impurity element can be further removed, it is right to reach
The effect of leachate purification.
According to the present invention, the temperature of step (2) sodium vanadate solution is 30-100 DEG C, for example can be 30 DEG C, 35 DEG C,
40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C or 100 DEG C, and above-mentioned number
Concrete point value between value, as space is limited and for simple and clear consideration, the present invention tool that no longer scope described in exclusive list includes
Body point value.The temperature of the sodium roasting leachate is preferably 60-80 DEG C.
The temperature of step (2) sodium vanadate solution is previous step to remaining after the process of sodium roasting leachate in the present invention
Temperature, it is not necessary to it is heated again.
According to the present invention, the pH described in step (2) is 7-9.5, for example can be 7,7.2,7.5,7.8,8,8.3,8.5,
8.7th, the concrete point value between 9,9.5,9.3 or 9.5, and above-mentioned numerical value, as space is limited and for simple and clear consideration, the present invention
The concrete point value that no longer scope described in exclusive list includes.PH described in step (2) is preferably 9.2.
According to the present invention, step (2) the regulation pH sulfuric acid or hydrochloric acid are adjusted, preferably sulfuric acid.
According to the present invention, the cleaner described in step (2) be aluminum sulfate, sodium metaaluminate, aluminium chloride any one or at least
Two kinds of combination, for example, can be any one in aluminum sulfate, sodium metaaluminate, aluminium chloride, typical but non-limiting combination
For aluminum sulfate and sodium metaaluminate, aluminum sulfate and aluminium chloride, sodium metaaluminate and aluminium chloride, aluminum sulfate, sodium metaaluminate and aluminium chloride.Step
Suddenly the cleaner described in (2) is preferably aluminum sulfate.
According to the present invention, Al elements and the mol ratio of sodium vanadate solution Si elements are (1- in step (2) cleaner
1.5):1, for example can be 1:1、1.1:1、1.2:1、1.3:1、1.4:1 or 1.5:It is specific between 1, and above-mentioned numerical value
Value, as space is limited and for simple and clear consideration, the present invention concrete point value that no longer scope described in exclusive list includes.
Temperature, pH from above-mentioned preferred sodium vanadate solution and removed as cleaner and from above-mentioned from aluminum sulfate
Miscellaneous dose of addition, can play facilitation to removal of impurities reaction, make cleaner give play to the effect of maximum, especially first to Si
Element is swept off, and further realizes removing the purpose of impurity element.
According to the present invention, the precipitation agent described in step (3) is any one in ammonium sulfate, ammonium chloride, ammonium acetate, ammonium carbonate
Kind or at least two combination, for example, can be any one in ammonium sulfate, ammonium chloride, ammonium acetate, ammonium carbonate, typical but non-
It is determinate to be combined as ammonium sulfate and ammonium chloride, ammonium acetate and ammonium carbonate, ammonium sulfate and ammonium acetate, ammonium sulfate and ammonium carbonate, chlorine
Change ammonium and ammonium acetate, ammonium chloride and ammonium carbonate, ammonium sulfate, ammonium chloride, ammonium acetate and ammonium carbonate etc..Precipitation described in step (3)
Agent is preferably ammonium sulfate.
According to the present invention, step (3) pH is 1.9-3.0, for example can be 1.9,2.0,2.1,2.2,2.3,2.4,
2.5th, the concrete point value between 2.6,2.7,2.8,2.9 or 3.0, and above-mentioned numerical value, as space is limited and for simple and clear consideration,
The present invention concrete point value that no longer scope described in exclusive list includes.Step (3) pH is preferably 2.8；
According to the present invention, step (3) the regulation pH sulfuric acid or hydrochloric acid are adjusted, preferably sulfuric acid.
According to the present invention, NH in step (3) the precipitation agent4 +With the mol ratio of V element in the sodium vanadium extraction scavenging solution
For (1-2):3, for example can be 1:3、1.1:3、1.2:3、1.3:3、1.4:3、1.5:3、1.6:3、1.7:3、1.8:3、1.9:3
Or 2:Concrete point value between 3, and above-mentioned numerical value, as space is limited and for simple and clear consideration, the present invention no longer exclusive list
The concrete point value that the scope includes.NH in step (3) the precipitation agent4 +Rub with V element in the sodium vanadium extraction scavenging solution
That ratio preferably 1.8:3.
According to the present invention, the temperature of step (3) heating is 95-100 DEG C, for example can be 95 DEG C, 96 DEG C, 97 DEG C,
Concrete point value between 98 DEG C, 99 DEG C or 100 DEG C, and above-mentioned numerical value, as space is limited and for simple and clear consideration, the present invention is not
The concrete point value that again scope described in exclusive list includes.The temperature of step (3) heating is preferably 98 DEG C.
From above-mentioned preferred pH and temperature, preferred precipitation agent and its addition can be such that precipitation more smoothly carries out,
Simultaneously impurity element is effectively avoided, the especially incorporation of iron and silicon, and then obtain the ammonium poly-vanadate crystalline substance of low iron, low silicon
Body.
According to the present invention, the temperature that step (4) is described when washing with water is 30-80 DEG C, for example can be 30 DEG C, 35 DEG C,
Concrete point value between 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C or 80 DEG C, and above-mentioned numerical value, is limited to
Length and for simple and clear consideration, the present invention concrete point value that no longer scope described in exclusive list includes.Step (4) is described to use water
Temperature during washing is preferably 60 DEG C.
When being washed at 60 DEG C, ammonium poly-vanadate crystal surface treatment it is cleaner, impurity element residual it is less.
Exemplarily, the method for preparing ammonium poly-vanadate by sodium roasting leachate of the present invention is comprised the following steps：
(1) sodium roasting leachate is measured, temperature is 30-100 DEG C, and with alkaline matter pH value of solution >=12, stirring are adjusted
Filter after 30min, obtain sodium vanadate solution；
(2) the sodium vanadate solution sulphur acid for adjusting pH for obtaining step (1) is 7-9.5, and temperature is 30-100 DEG C, Ran Houjia
Enter cleaner stirring, filter, obtain sodium vanadium extraction scavenging solution；
(3) the sodium vanadium extraction scavenging solution obtained to step (2) adds precipitation agent, and it is 1.9-3.0 to adjust pH with the concentrated sulfuric acid, plus
Heat is filtered to 95-100 DEG C after stirring, standing, obtains ammonium poly-vanadate crystal；
(4) gained ammonium poly-vanadate in step (3) is obtained into high-purity ammonium poly-vanadate with 30-80 DEG C of water washing.
Compared with prior art, the present invention at least has the advantages that：
(1) content of iron and silicon in ammonium poly-vanadate is significantly reduced so that the content of Fe elements is down to 0.0038-
The content of 0.0096wt%, Si element is down to 0.0032-0.0061wt%, while the content of other impurities element is reduced, it is full
In sufficient vanadium production of articles to the low iron of ammonium poly-vanadate, low silicon, low impurity requirement.
(2) preparation method process is simple provided by the present invention, it is easy to accomplish, it is adaptable to industrial production.
Specific embodiment
For ease of understanding, it is as follows that the present invention enumerates embodiment.It will be understood to those of skill in the art that following examples are only
The preferred embodiments of the present invention, are only used for help and understand the present invention, thus should not be taken as limiting the scope of the invention.
Embodiment 1
(1) the sodium roasting leachate that 3L vanadium concentration is 40g/L is measured, temperature is 100 DEG C, adjusts pH value with liquid caustic soda and be
13, filter after stirring 30min, obtain sodium vanadate solution；
(2) the sodium vanadate solution sulfuric acid regulation pH=8.5 obtained by step (1) is filtered, temperature is 30 DEG C, is subsequently adding
27.5g aluminum sulfate is stirred, and is filtered, and obtains sodium vanadium extraction scavenging solution；
(3) 135g ammonium sulfate is added to the sodium vanadium extraction scavenging solution obtained by step (2), with the concentrated sulfuric acid pH=3.0 is adjusted, plus
Heat is filtered to 95 DEG C after stirring, standing, obtains ammonium poly-vanadate crystal；
(4) gained ammonium poly-vanadate in step (3) is obtained into high-purity ammonium poly-vanadate with 50 DEG C of water washings.
Embodiment 2
(1) the sodium roasting leachate that 3L vanadium concentration is 30g/L is measured, temperature is 30 DEG C, being passed through ammonia regulation pH value is
14, filter after stirring 30min, obtain sodium vanadate solution；
(2) the sodium vanadate solution sulfuric acid regulation pH=9.5 obtained by step (1) is filtered, temperature is 100 DEG C, Ran Houjia
Enter the stirring of 30g aluminum sulfate, filter, obtain sodium vanadium extraction scavenging solution；
(3) 140g ammonium sulfate is added to the sodium vanadium extraction scavenging solution obtained by step (2), with the concentrated sulfuric acid pH=3, heating is adjusted
To 100 DEG C, filter after stirring, standing, obtain ammonium poly-vanadate crystal；
(4) gained ammonium poly-vanadate in step (3) is obtained into high-purity ammonium poly-vanadate with 40 DEG C of water washings.
Embodiment 3
(1) the sodium roasting leachate that 3L vanadium concentration is 25g/L is measured, temperature is 80 DEG C, it is 13 to adjust pH value with piece alkali,
Filter after stirring 30min, obtain sodium vanadate solution；
(2) the sodium vanadate solution sulfuric acid regulation pH=7 obtained by step (1) is filtered, temperature is 60 DEG C, is subsequently adding
32.5g aluminum sulfate is stirred, and is filtered, and obtains sodium vanadium extraction scavenging solution；
(3) 113g ammonium sulfate is added to the sodium vanadium extraction scavenging solution obtained by step (2), with the concentrated sulfuric acid pH=2.1 is adjusted, plus
Heat is filtered to 95 DEG C after stirring, standing, obtains ammonium poly-vanadate crystal；
(4) gained ammonium poly-vanadate in step (3) is obtained into high-purity ammonium poly-vanadate with 80 DEG C of water washings.
Embodiment 4
(1) the sodium roasting leachate that 3L vanadium concentration is 25g/L is measured, temperature is 60 DEG C, adjusts pH value with piece alkali and be
12.5, filter after stirring 30min, obtain sodium vanadate solution；
(2) the sodium vanadate solution sulfuric acid regulation pH=8.5 obtained by step (1) is filtered, temperature is 80 DEG C, is subsequently adding
26.3g aluminum sulfate is stirred, and is filtered, and obtains sodium vanadium extraction scavenging solution；
(3) 127g ammonium sulfate is added to the sodium vanadium extraction scavenging solution obtained by step (2), with the concentrated sulfuric acid pH=1.9 is adjusted, plus
Heat is filtered to 100 DEG C after stirring, standing, obtains ammonium poly-vanadate crystal；
(4) gained ammonium poly-vanadate in step (3) is obtained into high-purity ammonium poly-vanadate with 30 DEG C of water washings.
Embodiment 5
(1) the sodium roasting leachate that 3L vanadium concentration is 20g/L is measured, temperature is 75 DEG C, it is 12 to adjust pH value with piece alkali,
Filter after stirring 30min, obtain sodium vanadate solution；
(2) the sodium vanadate solution sulfuric acid regulation pH=9.2 obtained by step (1) is filtered, temperature is 75 DEG C, is subsequently adding
28.7g aluminum sulfate is stirred, and is filtered, and obtains sodium vanadium extraction scavenging solution；
(3) 120g ammonium sulfate is added to the sodium vanadium extraction scavenging solution obtained by step (2), with the concentrated sulfuric acid pH=2.8 is adjusted, plus
Heat is filtered to 98 DEG C after stirring, standing, obtains ammonium poly-vanadate crystal；
(4) gained ammonium poly-vanadate in step (3) is obtained into high-purity ammonium poly-vanadate with 60 DEG C of water washings.
The content of impurity element in the ammonium poly-vanadate that embodiment 1-5 is obtained is determined, the data of acquisition are as shown in table 1.
Table 1
From data in upper table：The content of each impurity element is equal in the ammonium poly-vanadate that the method that the present invention is provided is prepared
Very low, the content of wherein Fe elements is down to 0.0038-0.0096wt%, and the content of Si elements is down to 0.0032-0.0061wt%；
When the condition in from embodiment 5 prepares ammonium poly-vanadate, Fe elements are 0.0038wt%, and the content of Si elements is
0.0032wt%, the two content is minimum, while the content of other impurities element is also maintained at reduced levels, therefore embodiment
Condition in 5 is optimum preparation condition of the invention.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of embodiments of the present invention, as long as it is without prejudice to this
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of method that ammonium poly-vanadate is prepared by sodium roasting leachate, it is characterised in that the method comprising the steps of：
(1) alkaline matter is added in sodium roasting leachate, is filtered after stirring, obtain sodium vanadate solution；
(2) pH of regulating step (1) sodium vanadate solution, is subsequently adding cleaner, sodium vanadium extraction is obtained after agitation and filtration net
Change liquid；
(3) precipitation agent is added in step (2) the sodium vanadium extraction scavenging solution, pH is adjusted, heating stirring obtains many vanadium after filtration
Sour ammonium crystal；
(4) step (3) the ammonium poly-vanadate crystal is washed with water, after being dried ammonium poly-vanadate is obtained.
2. the method for claim 1, it is characterised in that the concentration of vanadium is in step (1) the sodium roasting leachate
15-40g/L；
Preferably, the temperature of the sodium roasting leachate is 30-100 DEG C, preferably 60-80 DEG C.
3. method as claimed in claim 1 or 2, it is characterised in that step (1) alkaline matter is piece alkali, liquid caustic soda or ammonia
In gas any one or at least two combination；
Preferably, step (1) it is described add alkaline matter after sodium roasting leachate pH >=12, preferably 12；
Preferably, the temperature of step (2) sodium vanadate solution is 30-100 DEG C, preferably 60-80 DEG C.
4. the method as described in any one of claim 1-3, it is characterised in that the pH described in step (2) is 7-9.5, preferably
9.2；
Preferably, step (2) the regulation pH sulfuric acid or hydrochloric acid are adjusted, preferably sulfuric acid.
5. the method as described in any one of claim 1-4, it is characterised in that the cleaner described in step (2) is aluminum sulfate, partially
In sodium aluminate, aluminium chloride any one or at least two combination, preferably aluminum sulfate；
Preferably, Al elements and the mol ratio of sodium vanadate solution Si elements are (1-1.5) in step (2) cleaner:1.
6. the method as described in any one of claim 1-5, it is characterised in that the precipitation agent described in step (3) is ammonium sulfate, chlorine
Change ammonium, ammonium acetate, in ammonium carbonate any one or at least two combination, preferably ammonium sulfate.
7. the method as described in any one of claim 1-6, it is characterised in that step (3) pH is 1.9-3.0, preferably
2.8；
Preferably, step (3) the regulation pH sulfuric acid or hydrochloric acid are adjusted, preferably sulfuric acid.
8. the method as described in any one of claim 1-7, it is characterised in that NH in step (3) the precipitation agent4 +With the sodium
The mol ratio for changing V element in vanadium extraction scavenging solution is (1-2):3, preferably 1.8:3.
9. the method as described in any one of claim 1-8, it is characterised in that the temperature of step (3) heating is 95-100
DEG C, preferably 98 DEG C.
10. the method as described in any one of claim 1-9, it is characterised in that the temperature that step (4) is described when washing with water is
30-80 DEG C, preferably 60 DEG C.
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| CN108085517A (en) * | 2017-12-15 | 2018-05-29 | 河钢股份有限公司承德分公司 | A kind of preparation method of aerospace grade tablet vanadic anhydride |
| CN108439467A (en) * | 2018-06-27 | 2018-08-24 | 攀钢集团研究院有限公司 | The continuous washing purification process of ammonium poly-vanadate |
| CN108517424A (en) * | 2018-04-08 | 2018-09-11 | 河钢股份有限公司承德分公司 | A method of being ultrasonically treated precipitation |
| CN110092419A (en) * | 2019-06-03 | 2019-08-06 | 承德燕北冶金材料有限公司 | A method of preparing high-purity ammonium poly-vanadate |
| CN114058880A (en) * | 2021-10-15 | 2022-02-18 | 河钢承德钒钛新材料有限公司 | Method for purifying sodium vanadate solution |
| 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 |
| CN114314660A (en) * | 2021-12-16 | 2022-04-12 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing low-silicon ammonium polyvanadate by reducing, precipitating and desiliconizing vanadium |
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| CN114436329A (en) * | 2021-12-16 | 2022-05-06 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadium pentoxide by sodium-vanadium solution two-step method |
| CN114477285A (en) * | 2021-12-16 | 2022-05-13 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by method |
| CN114480844A (en) * | 2021-12-16 | 2022-05-13 | 成都先进金属材料产业技术研究院股份有限公司 | Method for deeply removing silicon from alkaline vanadium-containing solution |
| CN115010177A (en) * | 2022-07-27 | 2022-09-06 | 中国科学院过程工程研究所 | Method for preparing vanadium pentoxide under mild condition |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899582A (en) * | 2010-07-30 | 2010-12-01 | 四川省川威集团有限公司 | Method for extracting vanadium pentoxide from vanadium slag |
| CN102251113A (en) * | 2011-07-12 | 2011-11-23 | 河北钢铁股份有限公司承德分公司 | Method for purifying vanadium leaching solution |
| CN102251119A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院过程工程研究所 | Method for recycling vanadium extraction tailings |
| CN104388683A (en) * | 2014-12-08 | 2015-03-04 | 中南大学 | Method for separating and recycling vanadium and chromium from vanadium and chromium-containing material |
-
2016
- 2016-11-18 CN CN201611019909.7A patent/CN106629846A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899582A (en) * | 2010-07-30 | 2010-12-01 | 四川省川威集团有限公司 | Method for extracting vanadium pentoxide from vanadium slag |
| CN102251119A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院过程工程研究所 | Method for recycling vanadium extraction tailings |
| CN102251113A (en) * | 2011-07-12 | 2011-11-23 | 河北钢铁股份有限公司承德分公司 | Method for purifying vanadium leaching solution |
| CN104388683A (en) * | 2014-12-08 | 2015-03-04 | 中南大学 | Method for separating and recycling vanadium and chromium from vanadium and chromium-containing material |
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| CN110092419A (en) * | 2019-06-03 | 2019-08-06 | 承德燕北冶金材料有限公司 | A method of preparing high-purity ammonium poly-vanadate |
| CN110092419B (en) * | 2019-06-03 | 2021-12-17 | 承德燕北冶金材料有限公司 | Method for preparing high-purity ammonium polyvanadate |
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| CN114477285A (en) * | 2021-12-16 | 2022-05-13 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing ammonium chromium polyvanadate by reducing acidic precipitated vanadium and ammonium chromium polyvanadate prepared by method |
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| CN114394619B (en) * | 2021-12-16 | 2024-06-04 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing low-silicon ammonium sodium polyvanadate through reduction and vanadium precipitation desilication |
| CN114436329B (en) * | 2021-12-16 | 2024-04-30 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing high-purity vanadium pentoxide by sodium vanadium solution two-step method |
| CN114314660A (en) * | 2021-12-16 | 2022-04-12 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing low-silicon ammonium polyvanadate by reducing, precipitating and desiliconizing vanadium |
| CN114480844B (en) * | 2021-12-16 | 2024-03-26 | 成都先进金属材料产业技术研究院股份有限公司 | Method for deeply removing silicon from alkaline vanadium-containing solution |
| 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 |
| 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 |
| CN115010177B (en) * | 2022-07-27 | 2023-08-29 | 中国科学院过程工程研究所 | Method for preparing vanadium pentoxide under mild condition |
| CN115010177A (en) * | 2022-07-27 | 2022-09-06 | 中国科学院过程工程研究所 | Method for preparing vanadium pentoxide under mild condition |
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Application publication date: 20170510 |