CN106319214B - It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution - Google Patents
It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution Download PDFInfo
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- CN106319214B CN106319214B CN201610837361.0A CN201610837361A CN106319214B CN 106319214 B CN106319214 B CN 106319214B CN 201610837361 A CN201610837361 A CN 201610837361A CN 106319214 B CN106319214 B CN 106319214B
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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
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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
- 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
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Abstract
The present invention relates to a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution.Its technical solution is：First oxidant is added in containing in vanadium solution, is aoxidized to get vanadium solution after oxidation；The addition of oxidant is fully oxidized to 1.0 ~ 2.5 times of oxidant theoretical molar amount needed for pentavalent vanadium for the vanadium of middle or low price containing vanadium solution.Urea is pressed again: the mass ratio of vanadic anhydride is that (3 ~ 20) ︰ 1 add in urea after aoxidizing in vanadium solution, and stirring, separation of solid and liquid is to get ammonium poly-vanadate and deposition vanadium mother liquid in vanadium solution after oxidation.Then ammonium poly-vanadate under the conditions of 450 ~ 650 DEG C is calcined into 0.5 ~ 3.0h, vanadic anhydride is made.The chemical composition containing vanadium solution is：Vanadium concentration is more than 6g/L, and aluminum concentration is less than 20g/L, and concentration of iron is less than 1.0g/L, and na concn is less than 30g/L, and potassium concn is less than 2.0g/L, and calcium concentration is less than 1.0g/L；PH value containing vanadium solution is less than 0.5.The present invention has the advantages that technological process is short, precipitation rate is high and vanadic anhydride product purity is high.
Description
Technical field
The invention belongs to contain vanadium solution precipitation technical field.More particularly to one kind from acid more impurity containing direct in vanadium solution
The method of precipitation.
Background technology
From containing vanadium solution precipitation be using the method for precipitation and separation of solid and liquid by vanadium and separation of foreign elements with obtain compared with
The process of the pure product containing vanadium.The primary chemical intermediate processing of vanadium has hydrolysis precipitation, molysite precipitation, calcium salt precipitation and ammonium salt to sink
Vanadium：Ammonium salt precipitation is divided into as the precipitation of alkalescent ammonium salt, the precipitation of faintly acid ammonium salt and acid ammonium salt precipitation；It is that will purify to hydrolyze precipitation
The pH value of treated vanadic acid or sodium vanadate solution is adjusted to 1.5 ~ 3.0, and more vanadic acid and more are settled out under conditions of heating stirring
The mixture of sodium vanadate, but obtained final products purity of vanadium pentoxide is less than 90%；What calcium salt precipitation and molysite precipitation obtained
Product can not be used directly to production vanadic anhydride generally as the intermediate products of Vanadium Concentrationin and the raw material of smelting ferrovanadium.
Alkalescent ammonium salt precipitation is first to adjust the pH value containing vanadium solution to 8.0 ~ 9.0, adds in excessive ammonium salt, at room temperature
Ammonium metavanadate crystal is generated, in order to improve precipitation rate and purity of vanadium pentoxide, does not require nothing more than the concentration of vanadium containing vanadium solution height, and need
It first passes through purified treatment and to add in excessive ammonium salt.Faintly acid ammonium salt precipitation is by the pH value containing vanadium solution after purified treatment
4.0 ~ 6.0 are adjusted to, ammonium salt is added in, ammonium poly-vanadate is settled out under conditions of heating stirring, gained ammonium poly-vanadate is in hot water
Dissolving, precipitation under conditions of being 2.0 in pH value, precipitation technological process is long, and ammonium salt consumption is big.Acid ammonium salt precipitation is at purification
Containing after reason adds in suitable ammonium salt in vanadium solution, adjust pH value to 2.0 ~ 3.0, more vanadium are settled out under conditions of heating stirring
Sour ammonium, but for acid polymictic precipitation containing vanadium solution, there are purified treatment process flow it is long the problem of.
" method that wet method recycles vanadium from vanadium ore containing high silicon and high carbon "（CN101914695A）Patented technology, for high silicon and high carbon
And the low-grade navajoite containing impurity such as aluminium, sulphur, Determinations, it leaches-P204 extractions-sulfuric acid by sulfuric acid oxidation and is stripped
Taking technique is obtained containing vanadium solution, sodium chlorate is added in containing in vanadium solution, stirring oxidation 1.0h, is cooled to room temperature under the conditions of 60 DEG C
Afterwards, adjust pH value to 2.5 ~ 3.0 with ammonium hydroxide, heating is boiled, and stirs 1.0 ~ 2.0h, obtains ammonium poly-vanadate precipitation, precipitation rate for 95 ~
99%, 5.0h is calcined under the conditions of being deposited in 550 ~ 650 DEG C, obtains the vanadic anhydride that purity is more than 98%.The technique precipitation rate and
Purity of vanadium pentoxide is low.
Wu Haiying etc.（Wu Haiying, Dai Zilin, danger is green, and precipitation technique is ground in Li Guiying bone coal navajoite Whote-wet method vanadium extraction technologies
Study carefully [J] mining metallurgical engineerings, 2012,32 (5):90-93.）Rock coal containing alum is directly leached to-P204 extractions-sulfuric acid back extraction through persulfuric acid
Taking technique is obtained containing vanadium solution, and sodium chlorate oxidation is added under 60 DEG C of water bath conditions, with 15% ammonium hydroxide adjust pH value 0.5 with
It is interior, 1.0h is stirred under the conditions of 95 DEG C, this section of precipitation rate is 85%, and product purity of vanadium pentoxide is 99.23%；Second segment precipitation
It is then to adjust above-mentioned filtrate under the conditions of pH value is 2.0,95 DEG C with ammonium hydroxide to stir 2.0h, filters, obtain precipitation product, Xiang Chen
30% sodium hydroxide solution is added in vanadium product, with sulphur acid for adjusting pH value to 5.0 ~ 5.5, adds in ammonium sulfate, then with sulphur acid for adjusting pH
Be worth be 2.0,90 DEG C under the conditions of stir 2.0h, final products purity of vanadium pentoxide is 99.12%.By alkali after second segment precipitation
Molten-sulfuric acid tune pH value-ammonium salt precipitation, purified treatment process flow are long.
" a kind of from method of the high alumina containing precipitation in vanadium solution "（CN104131180A）Patented technology contains vanadium for high alumina
Solution, first plus ammonium hydroxide adjusts pH value to 2.0 ~ 4.0h of stirring, crystallization under the conditions of 1.5 ~ 2.0,5 ~ 30 DEG C and ammonia-alum is precipitated, and crystallizes tail
Liquid adds sodium chlorate oxidizing lower vanadium ion, and ammonium hydroxide is added after oxidation and adjusts pH value to stirring under the conditions of 2.3 ~ 2.5,92 ~ 95 DEG C
2.0 ~ 3.0h obtains red vanadium, smart vanadium product is obtained after red vanadium drying and calcining.Technique needs are carried out to containing vanadium solution at purification
Reason, process flow are long.
In conclusion the existing technology of precipitation containing vanadium solution is primarily present, technological process is long, precipitation rate is low and five oxidations two
The shortcomings such as vanadium product purity is low.
Invention content
The present invention is directed to overcome prior art defect, it is therefore an objective to provide that a kind of technological process is short, precipitation rate is high and five oxidations
Two vanadium product purities are high from acid more methods of the impurity containing precipitation direct in vanadium solution.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that：
Step 1: oxidation
Oxidant is added in containing vanadium solution after 0.2 ~ 1.0h in vanadium solution, is aoxidized under the conditions of 40 ~ 70 DEG C to get oxidation；
The addition of the oxidant is fully oxidized to 1.0 of oxidant theoretical molar amount needed for pentavalent vanadium for the vanadium of middle or low price containing vanadium solution
~ 2.5 times.
Step 2: homogeneous precipitation
By urea: the mass ratio of vanadic anhydride is that (3 ~ 20) ︰ 1, the urea is added in vanadium solution after the oxidation
After the oxidation in vanadium solution, 1.0 ~ 6.0h is stirred under the conditions of 70 ~ 100 DEG C, separation of solid and liquid is female to get ammonium poly-vanadate and precipitation
Liquid.
Step 3: calcining
The ammonium poly-vanadate under the conditions of 450 ~ 650 DEG C is calcined into 0.5 ~ 3.0h, vanadic anhydride is made.
The chemical composition containing vanadium solution is：Vanadium concentration is more than 6g/L；Aluminum concentration is less than 20g/L；Concentration of iron is less than
1.0g/L；Na concn is less than 30g/L；Potassium concn is less than 2.0g/L；Calcium concentration is less than 1.0g/L.The pH value containing vanadium solution is small
In 0.5.
The oxidant is one or more of hydrogen peroxide, sodium chlorate, sodium hypochlorite.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art：
1st, the present invention does not need to be how miscellaneous to the acidity from acid more impurity containing urea is directly added into during precipitation in vanadium solution
Matter carries out purified treatment containing vanadium solution.In a heated condition, urea, which slowly decomposes generation ammonia and carbon dioxide, ammonia, makes the pH of solution
Value gradually rises and generates ammonium ion, avoids generating local over-concentration phenomenon, slowly generating ammonium poly-vanadate in containing vanadium solution sinks
It forms sediment, precipitation rate is more than 98.5%.
2nd, homogeneous precipitation can effectively prevent co-precipitation in the present invention, and the ammonium poly-vanadate crystal form of generation is complete, particle is equal
It is even, impurity content is few, it is no longer necessary to alkali soluble removal of impurities-sulfuric acid tune pH value-ammonium salt precipitation, by ammonium poly-vanadate calcine up to five oxidation two
Vanadium.Obtained purity of vanadium pentoxide is more than 99.0%.
Therefore, the present invention has the advantages that technological process is short, precipitation rate is high and vanadic anhydride product purity is high.
Specific embodiment
The present invention will be further described With reference to embodiment, not to the limitation of its protection domain.
The chemical composition containing vanadium solution is described in the present embodiment：Vanadium concentration is more than 6g/L；Aluminum concentration is less than 20g/L；Iron is dense
Degree is less than 1.0g/L；Na concn is less than 30g/L；Potassium concn is less than 2.0g/L；Calcium concentration is less than 1.0g/L.It is described containing vanadium solution
PH value is less than 0.5.
It is repeated no more in embodiment.
Embodiment 1
It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution.The specific steps of the present embodiment the method
It is：
Step 1: oxidation
Oxidant is added in containing vanadium solution after 0.2 ~ 0.6h in vanadium solution, is aoxidized under the conditions of 40 ~ 50 DEG C to get oxidation；
The addition of the oxidant is fully oxidized to 1.0 of oxidant theoretical molar amount needed for pentavalent vanadium for the vanadium of middle or low price containing vanadium solution
~ 1.5 times.
Step 2: homogeneous precipitation
By urea: the mass ratio of vanadic anhydride is that (12 ~ 20) ︰ 1, the urea is added in vanadium solution after the oxidation
After the oxidation in vanadium solution, 1.0 ~ 4.0h is stirred under the conditions of 70 ~ 90 DEG C, separation of solid and liquid is female to get ammonium poly-vanadate and precipitation
Liquid.
Step 3: calcining
The ammonium poly-vanadate under the conditions of 450 ~ 550 DEG C is calcined into 0.5 ~ 2.0h, vanadic anhydride is made.
The oxidant is hydrogen peroxide.
Embodiment 2
It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution.The present embodiment is hydrogen peroxide except the oxidant
Outside the mixture of sodium chlorate, remaining is the same as embodiment 1.
Embodiment 3
It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution.The specific steps of the present embodiment the method
It is：
Step 1: oxidation
Oxidant is added in containing vanadium solution after 0.4 ~ 0.8h in vanadium solution, is aoxidized under the conditions of 50 ~ 60 DEG C to get oxidation；
The addition of the oxidant is fully oxidized to 1.5 of oxidant theoretical molar amount needed for pentavalent vanadium for the vanadium of middle or low price containing vanadium solution
~ 2 times.
Step 2: homogeneous precipitation
By urea: the mass ratio of vanadic anhydride is that (8 ~ 15) ︰ 1, the urea is added in vanadium solution after the oxidation
After the oxidation in vanadium solution, 2 ~ 5h is stirred under the conditions of 75 ~ 95 DEG C, separation of solid and liquid is to get ammonium poly-vanadate and deposition vanadium mother liquid.
Step 3: calcining
The ammonium poly-vanadate under the conditions of 500 ~ 600 DEG C is calcined into 1.5 ~ 2.5h, vanadic anhydride is made.
The oxidant is sodium chlorate.
Embodiment 4
It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution.The present embodiment is sodium chlorate except the oxidant
Outside the mixture of sodium hypochlorite, remaining is the same as embodiment 3.
Embodiment 5
It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution.The specific steps of the present embodiment the method
It is：
Step 1: oxidation
Oxidant is added in containing vanadium solution after 0.6 ~ 1.0h in vanadium solution, is aoxidized under the conditions of 50 ~ 70 DEG C to get oxidation；
The addition of the oxidant for the vanadium of middle or low price containing vanadium solution be fully oxidized to oxidant theoretical molar amount needed for pentavalent vanadium 2 ~
2.5 again.
Step 2: homogeneous precipitation
By urea: the mass ratio of vanadic anhydride is that (3 ~ 10) ︰ 1, the urea is added in vanadium solution after the oxidation
After the oxidation in vanadium solution, 3 ~ 6h is stirred under the conditions of 80 ~ 100 DEG C, separation of solid and liquid is to get ammonium poly-vanadate and deposition vanadium mother liquid.
Step 3: calcining
The ammonium poly-vanadate under the conditions of 550 ~ 650 DEG C is calcined into 2 ~ 3h, vanadic anhydride is made.
The oxidant is sodium hypochlorite.
Embodiment 6
It is a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution.The present embodiment is dioxygen except the oxidant
Outside the mixture of water, sodium chlorate and sodium hypochlorite, remaining is the same as embodiment 5.
Present embodiment has following good effect compared with prior art：
1st, present embodiment is not needed to from acid more impurity containing urea is directly added into during precipitation in vanadium solution to described
Acid more impurity carry out purified treatment containing vanadium solution.In a heated condition, urea slowly decomposes generation ammonia and carbon dioxide, ammonia and makes
The pH value of solution gradually rises and generates ammonium ion, avoids generating local over-concentration phenomenon, is slowly generated in containing vanadium solution more
Ammonium vanadate precipitates, and precipitation rate is more than 98.5%.
2nd, homogeneous precipitation can effectively prevent co-precipitation in present embodiment, and the ammonium poly-vanadate crystal form of generation is complete
It is whole, particle is uniform, impurity content is few, it is no longer necessary to alkali soluble removal of impurities-sulfuric acid tune pH value-ammonium salt precipitation, by ammonium poly-vanadate calcining be
Obtain vanadic anhydride.Obtained purity of vanadium pentoxide is more than 99.0%.
Therefore, present embodiment has that technological process is short, precipitation rate is high and that vanadic anhydride product purity is high is excellent
Point.
Claims (2)
- It is 1. a kind of from acid more methods of the impurity containing precipitation direct in vanadium solution, it is characterised in that the specific steps of the method It is：Step 1: oxidationOxidant is added in containing vanadium solution after 0.2~1.0h in vanadium solution, is aoxidized under the conditions of 40~70 DEG C to get oxidation；Institute State the addition of oxidant for the vanadium of middle or low price containing vanadium solution be fully oxidized to oxidant theoretical molar amount needed for pentavalent vanadium 1.0~ 2.5 again；Step 2: homogeneous precipitationBy urea: after the oxidation in vanadium solution vanadic anhydride mass ratio for (3~20) ︰ 1, will the urea add in described in After oxidation in vanadium solution, 1.0~6.0h is stirred under the conditions of 70~100 DEG C, separation of solid and liquid is female to get ammonium poly-vanadate and precipitation Liquid；Step 3: calciningThe ammonium poly-vanadate under the conditions of 450~650 DEG C is calcined into 0.5~3.0h, vanadic anhydride is made；The chemical composition containing vanadium solution is：Vanadium concentration is more than 6g/L, and aluminum concentration is less than 20g/L, and concentration of iron is less than 1.0g/L, Na concn is less than 30g/L, and potassium concn is less than 2.0g/L, and calcium concentration is less than 1.0g/L；The pH value containing vanadium solution is less than 0.5.
- It is 2. according to claim 1 from acid more methods of the impurity containing precipitation direct in vanadium solution, it is characterised in that described Oxidant is one or more of hydrogen peroxide, sodium chlorate, sodium hypochlorite.
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| CN109534398A (en) * | 2019-01-04 | 2019-03-29 | 武汉科技大学 | A kind of method that microwave precipitation prepares high purity vanadic anhydride |
| CN109534399A (en) * | 2019-01-04 | 2019-03-29 | 武汉科技大学 | A kind of method that hydro-thermal reaction prepares high purity vanadic anhydride |
| CN110835696A (en) * | 2019-11-26 | 2020-02-25 | 河钢股份有限公司承德分公司 | Preparation method of vanadium pentoxide |
| CN112239806B (en) * | 2020-10-29 | 2021-10-12 | 攀枝花市山青钒业有限公司 | Method for extracting vanadium from acidic high-phosphorus vanadium solution |
| CN113353982A (en) * | 2021-07-12 | 2021-09-07 | 陕西金诚杰出钒业有限责任公司 | Method for preparing high-purity vanadium dioxide |
| CN113621833A (en) * | 2021-08-12 | 2021-11-09 | 长江师范学院 | Method for recovering vanadium from aqueous solution |
| CN115449649B (en) * | 2022-10-13 | 2024-06-25 | 神华准能资源综合开发有限公司 | Method for precipitating vanadium from acidic aluminum chloride leaching solution |
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| US3986970A (en) * | 1973-05-02 | 1976-10-19 | The Furukawa Electric Co., Ltd. | Solution for chemical dissolution treatment of tin or alloys thereof |
| CN102167400A (en) * | 2011-03-18 | 2011-08-31 | 中南大学 | Method for preparing vanadium pentoxide from vanadium-containing solution |
| CN102502828A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Preparation method for V2O5 nanometer crystals |
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