CN110317961A - The method for preparing vanadic anhydride containing vanadium solution - Google Patents
The method for preparing vanadic anhydride containing vanadium solution Download PDFInfo
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- CN110317961A CN110317961A CN201910726248.9A CN201910726248A CN110317961A CN 110317961 A CN110317961 A CN 110317961A CN 201910726248 A CN201910726248 A CN 201910726248A CN 110317961 A CN110317961 A CN 110317961A
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- solution
- vanadic anhydride
- containing vanadium
- vanadium
- vanadium solution
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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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention belongs to technical field of wet metallurgy, and in particular to the method for preparing vanadic anhydride containing vanadium solution.Technical problem to be solved by the invention is to provide one kind to eliminate ammonia nitrogen waste water from source, and can guarantee the method for preparing vanadic anhydride containing vanadium solution of product purity.This method comprises the following steps: a, adjusting the pH value containing vanadium solution to 2.0~2.8, is heated to 30 DEG C~60 DEG C, is passed through SO2Gas contains vanadium solution after being restored；B, the pH value containing vanadium solution is 3~7 after adjusting reduction, and reaction, separation of solid and liquid obtains deposition vanadium mother liquid and precipitation solid, and precipitation solid is calcined to obtain vanadic anhydride.The rate of recovery of the method for the present invention vanadium is up to 98% or more, and the purity for the vanadic anhydride being prepared is up to 99% or more.
Description
Technical field
The invention belongs to technical field of wet metallurgy, and in particular to the method for preparing vanadic anhydride containing vanadium solution.
Background technique
Vanadium is widely used, and it is of crucial importance to be applied to fields, the strategic positions such as metallurgy, chemical industry, aerospace.Domestic and international vanadium extraction
Raw material is containing vanadium slag, bone coal, Petroleum Ash, dead catalyst etc., and acquisition is molten containing vanadium after these generally go through roasting, leaching containing vanadium raw materials
Liquid obtains high concentration vanadium liquid after purification enrichment containing vanadium solution, obtains five oxidations two after oxidation after acid ammonium salt precipitation, calcining
Vanadium.The technique can generate a large amount of ammonia nitrogen waste water during ammonium salt precipitation, and ammonia nitrogen waste water pollutes environment, and processing cost
It is high, it has also become the bottleneck of limitation vanadium industry development.
Patent document CN106241871A discloses high concentration vanadium liquid acid ammonium salt precipitation method, and this method is first to configure
Certain density ammonium salt solution adjusts pH value to 2~3, slowly ammonium salt solution is added into high concentration vanadium liquid, while acid adding is protected
Holding system pH is 2~3, and ammonium poly-vanadate is obtained by filtration to after precipitating completely in sustained response.Although this method can be effectively reduced
Vanadium wastewater amount, and have the advantages that precipitation rate height and product purity are high, still, it is useless that this method can not eliminate ammonia nitrogen from source
Water causes later period ammonia nitrogen waste water processing cost high.
Patent document CN106337135A discloses a kind of method of novel no ammonia-sinking vanadium production vanadic anhydride, this method
It is to guarantee that vanadium is pentavalent in solution using high concentration vanadium liquid as raw material by oxidation, sulfuric acid is added or sodium carbonate adjusts solution to acid
Property, the supersaturated system of pentavalent vanadium is formed, poly vanadic acid precipitating is crystallized out, continues to reduce acidity, forms vanadic anhydride hydration
Object precipitating, calcining obtain vanadic anhydride precipitating.Although this method eliminates ammonia nitrogen waste water from source, this method substantially belongs to
In the hydrolytic precipitation of pentavalent vanadium, the consumption of sulfuric acid or sodium carbonate is larger, is difficult to ensure the purity of product.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to eliminate ammonia nitrogen waste water from source, and can guarantee
The method for preparing vanadic anhydride containing vanadium solution of product purity.
The present invention solves above-mentioned technical problem and prepares vanadic anhydride containing vanadium solution the technical solution adopted is that providing
Method, this method comprises the following steps:
A, the pH value containing vanadium solution is adjusted to 2.0~2.8, is heated to 30 DEG C~60 DEG C, is passed through SO2After gas obtains reduction
Containing vanadium solution；
B, the pH value containing vanadium solution is 3~7 after adjusting reduction, and reaction, separation of solid and liquid obtains deposition vanadium mother liquid and precipitation solid,
Precipitation solid is calcined to obtain vanadic anhydride.
Further, in step a, the sulphur for adjusting pH value containing vanadium solution and being 30%~50% using volume fraction
Acid solution.
Further, described to be passed through SO in step a2The rate of gas is 30~50L/min；Every cubic metre containing vanadium it is molten
Liquid duration of ventilation is 30~70min.
Further, in step a, described containing V in vanadium solution is 30~60g/L；Vanadium valence is+5 valences；PH value is 7~11.
Further, in step b, contain vanadium solution using alkaline solution after adjusting reduction.
Preferably, the alkaline solution is the NaOH or Na of 1~2mol/L2CO3At least one of solution.
Further, in step b, the time of the reaction is 60~120min.
Further, in step b, the temperature of the calcining is 400 DEG C~600 DEG C；The time of calcining is 30~90min.
The present invention provides a kind of normal pressures without ammonia-sinking vanadium method, is tetravalence vanadium solution by that will contain pentavalent vanadium solution reduction
Afterwards, then through hydrolysis precipitation, calcining vanadic anhydride is obtained.The method of the present invention eliminates ammonia nitrogen waste water from source, and has saved ammonia
The processing cost of nitrogen waste water, and problem of environmental pollution caused by ammonium salt precipitation is eliminated from source.The method of the present invention vanadium returns
Yield is up to 98% or more, and the purity for the vanadic anhydride being prepared is up to 99% or more.The method of the present invention dosing is few,
It is environmental-friendly, simple process, at low cost, it has broad application prospects.
Specific embodiment
Raw material, equipment used in the specific embodiment of the invention are known product, are obtained by purchase commercial product.
The present invention provides the methods for preparing vanadic anhydride containing vanadium solution, and this method comprises the following steps:
A, the pH value containing vanadium solution is adjusted to 2.0~2.8, is heated to 30 DEG C~60 DEG C, is passed through SO2After gas obtains reduction
Containing vanadium solution；
B, the pH value containing vanadium solution is 3~7 after adjusting reduction, and reaction, separation of solid and liquid obtains deposition vanadium mother liquid and precipitation solid,
Precipitation solid is calcined to obtain vanadic anhydride.
What the present invention used is obtained by vanadium slag sodium roasting-water logging containing vanadium solution, is 30~60g/L containing V in vanadium solution；
Vanadium valence is+5 valences；PH value is 7~11.
The purpose of step a of the present invention is that the pentavalent vanadium contained in vanadium solution is reduced to tetravalence vanadium.Containing vanadium in vanadium solution with five
Valence vanadium form exists, including VO3 -、V3O9 3-、V4O12 4-Deng using the sulfuric acid solution that volume fraction is 30%~50% to adjust containing vanadium
The pH value of solution is to make to utilize H in acidity containing vanadium solution to 2.0~2.8+Guarantee going on smoothly for reduction process；It will contain
After vanadium solution is adjusted to acidity, after being heated to 30 DEG C~60 DEG C, it is passed through SO2Gas participates in reduction reaction, SO2The speed of gas
Rate is 30~50L/min；Every cubic metre of duration of ventilation containing vanadium solution is 30~70min.In order to guarantee higher reduction reaction
Efficiency will contain vanadium solution and be continuously maintained in 30 DEG C~60 DEG C, vanadium solution containing tetravalence is obtained after reduction.
The purpose of step b of the present invention is will to contain tetravalence vanadium solution precipitation to obtain vanadium dioxide, by vanadium dioxide oxidizing roasting
For vanadic anhydride.Specifically, step b is reacted using the pH value containing vanadium solution after alkaline solution adjusting reduction to 3~7,
It is in order to make the vanadium in solution be converted into vanadium dioxide precipitating, to reach precipitation purpose.Alkaline solution is the NaOH of 1~2mol/L
Or Na2CO3At least one of solution.Reaction is to carry out under normal temperature conditions, reacts 60~120min, and separation of solid and liquid is sunk
Vanadium mother liquid and precipitation solid, the calcining of precipitation solid, the temperature of calcining are 400 DEG C~600 DEG C, and 30~90min of calcining is up to five oxygen
Change two vanadium.
The present invention will further be elaborated by specific embodiment below.
In the following embodiments of the present invention containing vanadium solution obtained by vanadium slag sodium roasting-water logging.
Embodiment 1
The present embodiment is 55g/L containing V in vanadium solution；Vanadium valence is+5 valences；PH value is 7.2.
It uses volumetric concentration to adjust the pH value containing vanadium solution to 2.6 for 36% sulfuric acid solution, is heated to 45 DEG C, is passed through
SO2Gas, SO2The rate of gas is 46L/min, and every cubic metre of duration of ventilation containing vanadium solution is 56min, is contained after being restored
Vanadium solution；
Using 1.0mol/LNaOH and 0.5mol/LNa2CO3Mixed-alkali solution adjust reduction after the pH value containing vanadium solution
It is 4.5, after reacting 100min under normal temperature condition, separation of solid and liquid obtains deposition vanadium mother liquid and solid, and solid is calcined at 450 DEG C
60min obtains vanadic anhydride.After measured, the rate of recovery of vanadium reaches 98.7%, product V2O5Purity reaches 98.6%.
Embodiment 2
The present embodiment is 32g/L containing V in vanadium solution；Vanadium valence is+5 valences；PH value is 10.
It uses volumetric concentration to adjust the pH value containing vanadium solution to 2.1 for 48% sulfuric acid solution, is heated to 35 DEG C, is passed through
SO2Gas, SO2The rate of gas is 38L/min, and every cubic metre of duration of ventilation containing vanadium solution is 68min, is contained after being restored
Vanadium solution；
The pH value containing vanadium solution reacts 90min under normal temperature condition for 6.4 after using 1.6mol/LNaOH solution to adjust reduction
Afterwards, it is separated by solid-liquid separation and obtains deposition vanadium mother liquid and solid, solid is obtained into vanadic anhydride in 500 DEG C of calcining 60min.After measured, vanadium
The rate of recovery reach 98.9%, product V2O5Purity reaches 99.2%.
Embodiment 3
The present embodiment is 48g/L containing V in vanadium solution；Vanadium valence is+5 valences；PH value is 9.2.
It uses volumetric concentration to adjust the pH value containing vanadium solution to 2.3 for 44% sulfuric acid solution, is heated to 45 DEG C, is passed through
SO2Gas, SO2The rate of gas is 50L/min, and every cubic metre of duration of ventilation containing vanadium solution is 52min, is contained after being restored
Vanadium solution；
Using 2mol/LNa2CO3The pH value containing vanadium solution is 7 after solution adjusts reduction, after reacting 90min under normal temperature condition,
Separation of solid and liquid obtains deposition vanadium mother liquid and solid, and solid is obtained vanadic anhydride in 480 DEG C of calcining 80min.After measured, time of vanadium
Yield reaches 98.3%, product V2O5Purity reaches 98.5%.
By Examples 1 to 3 it is found that making the rate of recovery of vanadium up to 98% or more using the method for the present invention, five be prepared
The purity of V 2 O is up to 99% or more.Ammonia nitrogen waste water is eliminated from source, and has saved the processing cost of ammonia nitrogen waste water, and
And problem of environmental pollution caused by ammonium salt precipitation is eliminated from source.
Claims (8)
1. the method for preparing vanadic anhydride containing vanadium solution, characterized by the following steps:
A, the pH value containing vanadium solution is adjusted to 2.0~2.8, is heated to 30 DEG C~60 DEG C, is passed through SO2Gas contains vanadium after being restored
Solution；
B, the pH value containing vanadium solution is 3~7 after adjusting reduction, and reaction, separation of solid and liquid obtains deposition vanadium mother liquid and precipitation solid, precipitation
Solid is calcined to obtain vanadic anhydride.
2. the method according to claim 1 for preparing vanadic anhydride containing vanadium solution, it is characterised in that: described in step a
Adjust the sulfuric acid solution that pH value containing vanadium solution is 30%~50% using volume fraction.
3. the method according to claim 1 or 2 for preparing vanadic anhydride containing vanadium solution, it is characterised in that: in step a,
It is described to be passed through SO2The rate of gas is 30~50L/min；Every cubic metre of duration of ventilation containing vanadium solution is 30~70min.
4. described in any item methods for preparing vanadic anhydride containing vanadium solution according to claim 1~3, it is characterised in that: step
In rapid a, described containing V in vanadium solution is 30~60g/L；Vanadium valence is+5 valences；PH value is 7~11.
5. the method according to any one of claims 1 to 4 for preparing vanadic anhydride containing vanadium solution, it is characterised in that: step
In rapid b, contain vanadium solution using alkaline solution after adjusting reduction.
6. the method according to claim 5 for preparing vanadic anhydride containing vanadium solution, it is characterised in that: the alkaline solution
For the NaOH or Na of 1~2mol/L2CO3At least one of solution.
7. described in any item methods for preparing vanadic anhydride containing vanadium solution according to claim 1~6, it is characterised in that: step
In rapid b, the time of the reaction is 60~120min.
8. described in any item methods for preparing vanadic anhydride containing vanadium solution according to claim 1~7, it is characterised in that: step
In rapid b, the temperature of the calcining is 400 DEG C~600 DEG C；The time of calcining is 30~90min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114408971A (en) * | 2022-02-28 | 2022-04-29 | 武汉科技大学 | Method for cleanly and efficiently preparing 99-grade vanadium pentoxide |
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Patent Citations (8)
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| CN102219257A (en) * | 2011-04-01 | 2011-10-19 | 中国恩菲工程技术有限公司 | Method for preparing vanadium pentoxide |
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| CN103602819A (en) * | 2013-11-29 | 2014-02-26 | 中南大学 | Comprehensive recovery method of vanadate-chromate-containing solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114408971A (en) * | 2022-02-28 | 2022-04-29 | 武汉科技大学 | Method for cleanly and efficiently preparing 99-grade vanadium pentoxide |
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