CN102181635A - Method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore - Google Patents

Method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore Download PDF

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Publication number
CN102181635A
CN102181635A CN2011100879547A CN201110087954A CN102181635A CN 102181635 A CN102181635 A CN 102181635A CN 2011100879547 A CN2011100879547 A CN 2011100879547A CN 201110087954 A CN201110087954 A CN 201110087954A CN 102181635 A CN102181635 A CN 102181635A
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vanadium
extraction
sulfuric acid
vanadium pentoxide
flakes
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王成彦
尹飞
居中军
杨永强
李强
陈永强
揭晓武
阮书峰
王振文
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Beijing General Research Institute of Mining and Metallurgy
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Beijing General Research Institute of Mining and Metallurgy
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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
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Abstract

The invention relates to a method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore, particularly a method for preparing high-purity vanadium pentoxide from sulfuric acid leach liquor of low-impurity-content stone coal vanadium ore. The method is characterized by sequentially comprising the following steps: (1) extracting leach liquor, which is obtained by leaching stone coal vanadium ore with sulfuric acid, to remove impurities; (2) carrying out back extraction on sulfuric acid to carry an organic phase; (3) oxidizing the back extraction liquor; (4) carrying out hydrolysis to precipitate vanadium; and (5) calcining the vanadium precipitate slag to obtain the vanadium pentoxide. Compared with the traditional technique, by using oxydol, persulfuric acid and the like as oxidants in the oxidation process, the method provided by the invention can avoid introducing other impurity cations, thereby ensuring the purity of the product vanadium pentoxide. Compared with the traditional ammonium-salt vanadium-precipitation technique, the method provided by the invention saves the alkali consumption required by neutralization. The purity of the prepared vanadium pentoxide is up to 99.9%, and the recovery rate of vanadium is up to above 98%; and meanwhile, the invention can implement no pollution and cyclic utilization of the back extraction agent.

Description

A kind of bone coal navajoite sulphuric leachate prepares the method for Vanadium Pentoxide in FLAKES
Technical field
A kind of bone coal navajoite sulphuric leachate prepares the method for Vanadium Pentoxide in FLAKES, relates to the method that a kind of impure low bone coal navajoite sulphuric leachate prepares high purity vanadic anhydride.
Technical background
The fusing point of vanadium is very high, and normal and niobium, tantalum, tungsten, molybdenum also are called refractory metal.Have good ductility, matter is hard, salt tolerant acid and vitriolic performance, and better in the performance of gasproof-salt-aqueous corrosion than most of stainless steels.Therefore vanadium has purposes very widely in the industry of metallurgy, chemical industry, iron and steel.Along with the high speed development of China's modernization construction, the demand of vanadium and compound thereof is increasing.
The vanadium resource of China is mainly contained in bone coal navajoite, and according to estimates, the vanadium reserves are 2.7 times of vanadium reserves in the vanadium titano-magnetite in China's bone coal navajoite, but the vanadium grade of bone coal navajoite is generally on the low side.Majority has all related to reduction leach liquor extracting-back extraction-ammonium salt precipitation workshop section in the process for extracting vanadium from stone coal.
It is sulphuric leachate behind the organic extractant phase bone coal navajoite torrefaction that Chinese patent publication number CN 101451199A discloses with the N235+TBP+ sulfonated kerosene, with Na2CO3 is after reverse-extraction agent obtains strip liquor, adjust the pH precipitation with ammoniacal liquor or ammonium salt and obtain the ammonium meta-vanadate vanadium slag, calcine vanadium slag again and obtain Vanadium Pentoxide in FLAKES.
It is sulphuric leachate behind the organic extractant phase bone coal navajoite torrefaction that Chinese patent publication number CN 101450814A discloses with the P204+TBP+ sulfonated kerosene, with sulfuric acid is that reverse-extraction agent obtains strip liquor, strip liquor is earlier with sodium chlorate or potassium permanganate oxidation, ammonification water condition pH to 1.5～2.0 again, hydrolysis obtains ammonium meta-vanadate, and calcining obtains Vanadium Pentoxide in FLAKES.
Handling at present impure low vanadium solution adopts substantially in reduction-extracting-back extraction-oxidation and to obtain vanadate with precipitation and calcine and obtain Vanadium Pentoxide in FLAKES, all related to the precipitation of oxidation ammonium salt in the treating processes in the technology of vanadium strip liquor, perhaps adopt yellow soda ash, alkali lye precipitations such as sodium hydroxide, liquid will be handled again after the precipitation, if with acid is reverse-extraction agent, also need pH is neutralized to about 2.0 before the precipitation, these technologies all can produce pollution problems such as ammonium salt or sodium salt, can exist ammonia to pollute in the calcination process or product in the exceeding standard of other impurity, and N-process can waste a large amount of bronsted lowry acids and bases bronsted lowries, all do not meet Green Chemistry and technical process economy principle.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of and can effectively reduce pollution, reduce acid, alkali consumption, effectively improve product purity, raising vanadium recovery, reverse-extraction agent bone coal navajoite sulphuric leachate capable of circulation prepare the method for Vanadium Pentoxide in FLAKES.
The objective of the invention is to be achieved through the following technical solutions.
A kind of bone coal navajoite sulphuric leachate prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that the steps in sequence of its preparation process comprises:
(1) sulfuric acid is leached the leach liquor of bone coal navajoite gained, carry out abstraction impurity removal;
(2) sulfuric acid back extraction load organic phases;
(3) strip liquor oxidation;
(4) hydrolysis precipitation;
(5) precipitation slag calcining preparation Vanadium Pentoxide in FLAKES.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that the vanadiumcontent of the leach liquor of described sulfuric acid leaching bone coal navajoite gained is 0.1～10g/L.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, the leach liquor that sulfuric acid is leached the bone coal navajoite gained that it is characterized in that step (1) carries out the abstraction impurity removal process, earlier leach liquor being adjusted the pH value is 1.5～2.5, the current potential of control solution is 100～350mV, carry out 15～120 minutes reduction reaction time, after the filtration, carry out abstraction impurity removal again.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, the extracted organic phase that it is characterized in that described abstraction impurity removal process is the P204+ sulfonated kerosene, wherein P204 is an extraction agent, sulfonated kerosene is a thinner, the volumetric concentration of extraction agent is controlled at 5%～50%, the volume ratio of organic phase and water is controlled at 0.2:1～5:1 during extraction, the extraction residence time is 3～20 minutes, counter-current extraction is adopted in extraction, the extracting stage numerical control is built in the 3-10 level, and the load organic phases of extraction is handled through carrying out back extraction behind the weak acid scrubbing.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, the sulfuric acid back extraction load organic phases process of carrying out that it is characterized in that step (2), load organic phases is adopted as the sulfuric acid reverse-extraction agent, free sulfuric acid concentration is 100～200g/L in the reverse-extraction agent, the volume ratio of back extraction organic phase and water is controlled at 10:1～1:1,3～10 stage countercurrent back extractions are adopted in back extraction, and liquid vanadium concentration is 15～70g/L after the back extraction; Organic phase after the back extraction is returned step (2) and is extracted behind process peracid washed metal.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that liquid returns step (2) after the precipitation of described step (3) to recycle as strip liquor.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that the strip liquor oxidising process of described step (3); Be that the vanadium solution that contains that obtains after the back extraction with step (2) carries out oxidation, make the tetravalence vanadium in the strip liquor be oxidized to the pentavalent vanadium; Oxygenant is hydrogen peroxide or persulfuric acid; Or sodium chlorate; Or Sodium Persulfate; The consumption of oxygenant is 0.8～5 times of tetravalence vanadium in the solution, and oxidizing reaction temperature is 30～105 ℃, and current potential 900～1300 mV of oxidated solution are with respect to the hydrogen scalar potential; Oxidization time is 15～120 minutes.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, the strip liquor oxidising process oxidated solution hydrolytic process that it is characterized in that described step (4) is that oxidated solution directly is warmed up to 75～110 ℃, and hydrolysis time is 0.5～6 hour.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that precipitation slag drying that the hydrolysis after-filtration of described step (5) goes out after, under 540 ℃～610 ℃ temperature, calcined 0.5～5 hour again.
A kind of bone coal navajoite sulphuric leachate of the present invention prepares the method for Vanadium Pentoxide in FLAKES, compare with traditional technology, because it is oxygenant that oxidising process adopts hydrogen peroxide, persulfuric acid etc., can avoid the introducing of other impurity cationics, has guaranteed the purity of Vanadium Pentoxide in FLAKES product.
Hydrolysis under the direct peracid condition of precipitation process is because pentavalent vanadium hydrolytic process can discharge H +, add the H that tetravalence vanadium oxidising process is discharged +, then offset the H that the back extraction process is consumed just +, so whole back extraction-oxidation-hydrolysis precipitation process, H +Do not reduce, realized the recycle of reverse-extraction agent vitriolic.In addition,, therefore compare, saved the alkali that neutralization will consume with traditional ammonium salt precipitation technology because hydrolytic process does not need to adjust pH.
The NH3 that the precipitation process does not need traditional technology and added +And other metal ion ions, therefore effectively avoided ammonium salt and other metal ion pollutions, the gained of precipitation simultaneously contains the vanadium intermediate product, rather than the resulting ammonium poly-vanadate of traditional technology, does not pollute so calcination process does not produce ammonia.Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of and can effectively reduce pollution, reduce acid, alkali consumes, the present invention proposes a kind of leach liquor with sulfuric acid leaching bone coal navajoite gained is raw material, liquid directly adds the method that a spot of acid recycles as strip liquor after making it advance washing calcining-precipitation through abstraction impurity removal-sulfuric acid back extraction load organic phases-strip liquor through direct oxidation precipitation-precipitation slag, because the present invention does not mix other metallic impurity elements in extraction back extraction oxidising process, so the purity of the Vanadium Pentoxide in FLAKES of present method preparation is for can reach 99.9%, the rate of recovery of vanadium can reach more than 98%, realizes pollution-free simultaneously, the reverse-extraction agent recycle.
Description of drawings
Fig. 1 process flow sheet of the present invention.
Embodiment
A kind of bone coal navajoite sulphuric leachate prepares the method for Vanadium Pentoxide in FLAKES, the leach liquor that leaches the bone coal navajoite gained with sulfuric acid is a raw material, the a spot of acid of the direct interpolation of liquid is reclaimed the Vanadium Pentoxide in FLAKES of preparation as the method that strip liquor recycles after making it advance washing calcining-precipitation through abstraction impurity removal-sulfuric acid back extraction load organic phases-strip liquor through direct oxidation precipitation-precipitation slag, and the rate of recovery of vanadium can reach more than 98%.This method comprises the steps:
1, will contain vanadium 0.1～10g/L solution adding neutralizing agent makes the acidity pH value of solution be controlled at 1.5～2.5, the current potential that adds a spot of reductive agent (iron powder, S-WAT etc.) control solution simultaneously is at 100～350mV, with respect to the hydrogen scalar potential, filter and obtain solution.This operation mainly is to exist ferric iron to be reduced to ferrous iron in the solution in order to make, and the pentavalent vanadium is reduced to the tetravalence vanadium, improves the extraction efficiency of P204 to vanadium.Treated solution obtains solution after filtering and continues step 2.
2, the solution that will neutralize after reducing extracts, extracted organic phase is the P204+ sulfonated kerosene, wherein P204 is an extraction agent, sulfonated kerosene is a thinner, and the volumetric concentration of extraction agent is controlled at 5～50%, and the volume ratio of organic phase and water is controlled at 0.2:1～5:1 during extraction, the extraction residence time is 3～20 minutes, counter-current extraction is adopted in extraction, and the extracting stage numerical control is built in 3～10 grades, and the load organic phases of extraction is handled through carrying out back extraction behind the weak acid scrubbing.
3, with the load organic phases of step 2 gained, adopt the sulfuric acid back extraction, reverse-extraction agent free sulfuric acid concentration is 100～200g/L, back extraction makes the volume ratio of organic phase and water be controlled at 10:1～1:1,3～10 stage countercurrent back extractions are adopted in back extraction, liquid vanadium concentration is 15～70g/L after the back extraction, continues step 4, and the organic phase after the back extraction is returned step 2 and extracted behind process peracid washed metal.
The back extraction reaction equation is:
VOR 2+ H 2SO 4→ VOSO 4+ 2HR(HR represents P 204)
By the back extraction reaction equation as can be known, the sulfuric acid of back extraction process consumption is 1 times of amount of substance of vanadium.
4, with the high vanadium solution that obtains after the back extraction, carry out oxidation and make tetravalence vanadium in the strip liquor, be oxidized to the pentavalent vanadium.For obtaining high purity vanadium, oxygenant is chosen as the not oxygenant of metal ion such as hydrogen peroxide, persulfuric acid.If must not also can add oxygenants such as sodium chlorate, Sodium Persulfate by high purity product.The processing condition of oxidation are: oxidizing temperature is 30 ~ 105 ℃, and the some position 900～1300mV(of oxidated solution is with respect to the hydrogen scalar potential), oxidization time is 15～120m minute.Solution after the oxidation is proceeded step 5
The oxidation equation formula is:
2VOSO 4+H 2O 2→?(VO 3) 2SO 4+?H 2SO 4
By the oxidation equation formula as can be known, the sulfuric acid that oxidising process produces is 0.5 times of amount of substance of vanadium, if can produce 1.5 times sulfuric acid with persulfuric acid, back extraction can not mended acid substantially.
5, oxidated solution directly is warmed up to 75～110 ℃, hydrolysis time is 0.5～6 hour, the slurries of oxidation obtain the intermediate solid product through filtration washing, if the free acid concentration of filtering filtrate quite directly returns step (3) with reverse-extraction agent, if return step (3) after the low evaporation concentration of concentration.
Hydrolysis precipitation reaction equation is:
(VO 2) 2SO 4+2H 2O→2HVO 3↓+H 2SO 4
By hydrolysis precipitation reaction equation as can be known, the sulfuric acid that produces in the hydrolytic process is 0.5 times of amount of substance of vanadium.
The reactional equation of comprehensive step 3 and step 4 as can be known, the vitriolic amount of substance that produces in the vanadium oxydrolysis process is a times of vanadium.So sulfuric acid consumption offsets just with generation in whole back extraction, oxidation and the hydrolytic precipitation process, back extraction, oxidation and hydrolytic process do not need supplemental acid, with respect to traditional ammonium salt precipitation technology, can save a large amount of acid consumptions and the needed alkaline consumption that neutralizes.
6, the solid intermediate product of step 5 gained is 200～350 ℃ of dryings, and controlling calcining temperature again is 540 ℃～610 ℃, and calcination time is 0.5～5 hour.Can obtain the high purity vanadic anhydride product.
Embodiment 1
The leach liquor that the direct acidleach bone coal navajoite of certain sulfuric acid obtains contains vanadium 1.69g/L.The vanadium solution that obtains through neutralization reduction pre-treatment contains vanadium 1.60g/L, and pH is 1.5, and solution potential is 180mV, adopting 10%P204+90% sulfonated kerosene (volume ratio) is extracted organic phase, under 35 ℃ of constant temperatures, compare 6 grades of extractions of O/A=1:2.5 adverse current, raffinate contains vanadium and is lower than 0.02g/L.Load organic phases is with the sulfuric acid back extraction of 150g/L, and the back extraction condition is for comparing O/A=10:1,4 stage countercurrent back extractions, and the strip liquor that obtains contains vanadium 33.20g/L and (rolls over V 2O 559.23g/L), H 2SO 480.38g/L.Adding hydrogen peroxide oxidation in the strip liquor is 900mV to solution potential, keeps under 60 ℃ 30 minutes, is warming up to 100 ℃ subsequently, and lasting hydrolysis precipitation 2 hours obtains liquid, liquid H after the precipitation by analysis after precipitation intermediate product and the precipitation 2SO 4137.03g/L liquid is supplemented to 150g/L with sulfuric acid concentration after this precipitation, directly is used as reverse-extraction agent.The vanadium slag calcining that the hydrolysis precipitation obtains, 550 ℃ of calcining temperatures, calcination time 3h obtains V 2O 5Grade be 99.9%.
Embodiment 2
The leach liquor that the direct acidleach bone coal navajoite of certain sulfuric acid obtains contains vanadium 6.2g/L.Contain vanadium 6.1g/L through solution many and that reduction is handled, pH is 2.3, and solution potential is that 310mV adopts 25%P204+75% sulfonated kerosene (volume ratio) for extracted organic phase, under 35 ℃ of constant temperatures, compare 6 grades of extractions of O/A=1:1 adverse current, raffinate contains vanadium and is lower than 0.05g/L.Liquid was mended acid again to 150g/L after load organic phases adopted oxydrolysis, and the back extraction condition is for comparing 8:1,5 stage countercurrent back extractions, and the strip liquor that obtains contains vanadium 52g/L, H2SO4 40.29g/L.Add hydrogen peroxide in the strip liquor, 100 ℃ of following oxidation limit hydrolysis, continue the hydrolysis precipitation 3 hours, and obtained liquid, liquid H2SO4 140.03g/L after the precipitation by analysis after precipitation intermediate product and the precipitation, contain vanadium 9.28g/L, the vanadium slag that the hydrolysis precipitation obtains is calcined 600 ℃ of calcining temperatures again through washing drying, calcination time 2h obtains grade and is 99.95% Vanadium Pentoxide in FLAKES product.
Embodiment 3
The leach liquor that the direct acidleach bone coal navajoite of certain sulfuric acid obtains contains vanadium 3.89g/L.The vanadium solution that obtains through neutralization reduction pre-treatment contains vanadium 3.60g/L, and pH is 2.1, and solution potential is 250mV, adopting 15%P204+85% sulfonated kerosene (volume ratio) is extracted organic phase, under 35 ℃ of constant temperatures, compare 6 grades of extractions of O/A=1:1 adverse current, raffinate contains vanadium 0.02g/L.Load organic phases with oxydrolysis after liquid acidity be 137.03g/L, contain vanadium 8.54g/L, the back extraction condition is for comparing 10:1,5 stage countercurrent back extractions, the strip liquor that obtains contains vanadium 42.1g/L, H2SO4 74.65g/L.Adding oversulfated in the strip liquor is 900mV to solution potential, keeps under 60 ℃ 30 minutes, is warming up to 80 ℃ subsequently, continue the hydrolysis precipitation 5 hours, and obtained liquid, liquid H2SO4 132.4g/L after the precipitation by analysis after precipitation intermediate product and the precipitation, contain vanadium 16.8g/L, return extraction.The calcining of vanadium slag that the hydrolysis precipitation obtains, 580 ℃ of calcining temperatures, calcination time 3h obtains grade and is 99.98% high purity vanadic anhydride.

Claims (9)

1. a bone coal navajoite sulphuric leachate prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that the steps in sequence of its preparation process comprises:
(1) sulfuric acid is leached the leach liquor of bone coal navajoite gained, carry out abstraction impurity removal;
(2) sulfuric acid back extraction load organic phases;
(3) strip liquor oxidation;
(4) hydrolysis precipitation;
(5) precipitation slag calcining preparation Vanadium Pentoxide in FLAKES.
2. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that the vanadiumcontent of the leach liquor of described sulfuric acid leaching bone coal navajoite gained is 0.1～10g/L.
3. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, the leach liquor that sulfuric acid is leached the bone coal navajoite gained that it is characterized in that step (1) carries out the abstraction impurity removal process, earlier leach liquor being adjusted the pH value is 1.5～2.5, the current potential of control solution is 100～350mV, carry out reduction reaction time 15～120min, after the filtration, carry out abstraction impurity removal again.
4. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, the extracted organic phase that it is characterized in that described abstraction impurity removal process is the P204+ sulfonated kerosene, wherein P204 is an extraction agent, sulfonated kerosene is a thinner, the volumetric concentration of extraction agent is controlled at 5%-50%, the volume ratio of organic phase and water is controlled at 0.2:1～5:1 during extraction, the extraction residence time is 3～20 minutes, counter-current extraction is adopted in extraction, the extracting stage numerical control is built in 3～10 grades, and the load organic phases of extraction is handled through carrying out back extraction behind the weak acid scrubbing.
5. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, the sulfuric acid back extraction load organic phases process of carrying out that it is characterized in that step (2), load organic phases is adopted as the sulfuric acid reverse-extraction agent, free sulfuric acid concentration is 100～200g/L in the reverse-extraction agent, the volume ratio of back extraction organic phase and water is controlled at 10:1～1:1,3～10 stage countercurrent back extractions are adopted in back extraction, and liquid vanadium concentration is 15～70g/L after the back extraction; Organic phase after the back extraction is returned step (2) and is extracted behind process peracid washed metal.
6. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that liquid returns step (2) after the precipitation of described step (3) to recycle as strip liquor.
7. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that the strip liquor oxidising process of described step (3); Be that the vanadium solution that contains that obtains after the back extraction with step (2) carries out oxidation, make the tetravalence vanadium in the strip liquor be oxidized to the pentavalent vanadium; Oxygenant is hydrogen peroxide or persulfuric acid; Or sodium chlorate; Or Sodium Persulfate; The consumption of oxygenant is 0.8～5 times of tetravalence vanadium in the solution, and oxidizing reaction temperature is 30～105 ℃, and current potential 900～1300 mV of oxidated solution are with respect to the hydrogen scalar potential; Oxidization time is 15～120 minutes.
8. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, the strip liquor oxidising process oxidated solution hydrolytic process that it is characterized in that described step (4) is that oxidated solution directly is warmed up to 75-110 ℃, and hydrolysis time is 0.5-6 hour.
9. a kind of bone coal navajoite sulphuric leachate according to claim 1 prepares the method for Vanadium Pentoxide in FLAKES, it is characterized in that precipitation slag drying that the hydrolysis after-filtration of described step (5) goes out after, under 540 ℃～610 ℃ temperature, calcined 0.5～5 hour again.
CN2011100879547A 2011-04-08 2011-04-08 Method for preparing vanadium pentoxide from sulfuric acid leach liquor of stone coal vanadium ore Pending CN102181635A (en)

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CN103555962A (en) * 2013-10-23 2014-02-05 北京矿冶研究总院 Method for comprehensively recovering selenium, vanadium and silver from vanadium silver polymetallic ore containing selenium employing wet process
CN104017999A (en) * 2014-06-25 2014-09-03 攀钢集团攀枝花钢铁研究院有限公司 Vanadium extraction method for converter vanadium slag
CN104711430A (en) * 2015-03-23 2015-06-17 紫阳县广润煤炭实业有限公司 Production method for preparing vanadium product by taking stone coal as raw material
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CN108516587A (en) * 2018-04-12 2018-09-11 四川星明能源环保科技有限公司 Vanadic anhydride and preparation method thereof
US10099939B2 (en) 2015-01-30 2018-10-16 Institute Of Process Engineering, Chinese Academy Of Sciences System and method for producing high-purity vanadium pentoxide powder
US10112846B2 (en) 2015-01-30 2018-10-30 Institute Of Process Engineering, Chinese Academy Of Sciences System and method for producing high-purity vanadium tetraoxide powder
US10125024B2 (en) 2015-01-30 2018-11-13 Institute Of Procees Engineering Chinese Academy Of Sciences System and method for purifying and preparing high-purity vanadium pentoxide powder
CN109706316A (en) * 2019-02-11 2019-05-03 广东省稀有金属研究所 A method of recycling valuable metal from deposition vanadium mother liquid
US10294118B2 (en) 2015-01-30 2019-05-21 Institute Of Process Engineering, Chinese Academy Of Sciences System and method for purifying vanadium pentoxide
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CN110172576A (en) * 2019-03-27 2019-08-27 杨秋良 The recovery method of vanadium in a kind of hydrochloric acid system
CN111020233A (en) * 2020-01-14 2020-04-17 中南大学 Method for preparing vanadium pentoxide by ammonium-free vanadium precipitation
CN112575207A (en) * 2020-12-04 2021-03-30 攀钢集团研究院有限公司 Method for preparing vanadium oxide by low-concentration acidic vanadium liquid extraction

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