CN104099483A - Preparation method of highly pure vanadium pentoxide - Google Patents
Preparation method of highly pure vanadium pentoxide Download PDFInfo
- Publication number
- CN104099483A CN104099483A CN201310125862.2A CN201310125862A CN104099483A CN 104099483 A CN104099483 A CN 104099483A CN 201310125862 A CN201310125862 A CN 201310125862A CN 104099483 A CN104099483 A CN 104099483A
- Authority
- CN
- China
- Prior art keywords
- vanadium
- precipitation
- poly
- high purity
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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 relates to the field of the chemical industry, and especially relates to a preparation method of highly pure vanadium pentoxide. The method comprises the following steps: oxidizing tetravalent vanadium in back extraction water obtained in a total hydrometallurgical vanadium extraction process to form pentavalent vanadium; forming an oversaturated system of pentavalent vanadium, precipitating to obtain a polyvanadic acid precipitate, carrying out solid-liquid separation to separate a solution containing a high content of impurities, washing the polyvanadic acid precipitate, adding the washed precipitate to a sulfuric acid solution, carrying out heat insulation uniform stirring, and adding an ammonium bicarbonate solution to prepare a highly pure product, wherein polyvanadic acid gradually forms a polyammonium vanadate precipitate having a lower solubility due to the solubility of polyammonium vanadate is less than the solubility of polyvanadic acid; and calcining the polyammonium vanadate precipitate to generate vanadium pentoxide. The method has the advantages of no influences on present technologic main flow or production equipment, short production flow, low production cost, and no leakage or environmental protection due to closed circular running of the highly pure vanadium pentoxide production flow and original flow. 3000t of the highly pure vanadium pentoxide can be produced yearly.
Description
Technical field
The present invention relates to chemical field, relate in particular to a kind of preparation method of high purity vanadic anhydride.
Background technology
The compound of vanadium and vanadium is development modern industry, modern national defense and the indispensable important materials of modern science and technology, be widely used in, in the every field such as ferrous metallurgy, non-ferrous metal, petrochemical complex, the energy, aerospace and nuclear industry, being referred to as " VITAMIN of modern industry ".In the explored vanadium reserves in the world, the occupancy volume of Chinese vanadium occupies third place in the world.Bone coal is the navajoite resource of a kind of uniqueness of China, verified and in bone coal, contained Vanadium Pentoxide in FLAKES and just reach 1.1797 hundred million tons, wherein content is 7707.5 power tons at more than 0.5% reserves, be 6.7 times of vanadium reserves in China's vanadium titano-magnetite, so the development and utilization of Rock coal containing alum have special resources advantage in China.Along with the development of national economy and the raising of scientific and technological level, the range of application of vanadium is constantly widened, more and more higher to the purity requirement of vanadium product, and the market requirement of high purity vanadic anhydride is also increasing.The concrete application of high purity vanadic anhydride mainly contains following aspect: (1) all-vanadium flow energy storage battery.(2) vanadium base solid solution hydrogen storage alloy.(3) optical transition coating.(4) luminescent material of vanadium.(5) vanadium pigment and off-color material.(6) nano vanadium oxide catalyzer.(7) Yttrium Orthovanadate (YVO
1) crystalline material.
Shaanxi Wuzhou Mining Co., Ltd. is China extracting vanadium from stone coal enterprise of maximum at present, in recent years, owing to conscientiously carrying out the relevant energy-conserving and environment-protective policy of country, widely popularize aborning and apply environmentally safe, efficient bone coal navajoite wet method vanadium extraction advanced technologies technology, under extracting vanadium from stone coal scope of the enterprise obtained developing rapidly growth, Vanadium Pentoxide in FLAKES industrial scale has reached year production more than 5000 tons, and its production control is positioned at top standard in similar enterprise at home and abroad with technical indicator.But because acidleach process choosing is poor, impurity element under strong acidic condition in mineral and vanadium together enter solution, cause leach liquor complicated component, although get enrichment removal of impurities through extracting-back extraction, but the impurity content in back extraction water intaking is still higher, wherein, with iron, aluminium, the impact of the elements such as sodium is the most serious, adopt acid ammonium salt precipitation, in products obtained therefrom, contain the metallic impurity of Chemical bond class as aluminium, sodium etc., form double salt or binary double salt, after precipitation is complete, adopt simple washing, even high temperature washing is difficult to these impurity to remove, Vanadium Pentoxide in FLAKES purity is hovered in 98% left and right substantially, produce high purity product and have certain difficulty.
China is in the world main Chan Fan big country, within 2012, Vanadium Pentoxide in FLAKES production capacity is over 100,000 tons, output reaches 70,000 tons, account for global vanadium output 50%, predict that Vanadium Pentoxide in FLAKES manufacturing enterprise production capacity in 2013 is 13.6 ten thousand tons, will be over 200,000 tons to China's Vanadium Pentoxide in FLAKES production capacity in 2017, actual output is over 150,000 tons.On short terms, Iron And Steel Industry is still the most important demand direction of vanadium, but steel industry is difficult to form the explosive chance increasing to the demand of vanadium.Therefore, the coming years, the market competition of common low-grade Vanadium Pentoxide in FLAKES is fiercer, and conventional vanadium product and common 98% grade of Vanadium Pentoxide in FLAKES profit space are generally on the low side.Existing handicraft product removal of impurities process is complicated, and quality product portion is stable, complex procedures, and production degree is low continuously, and production cost is higher.
Summary of the invention
Object of the present invention: solve high purity vanadium production process removal of impurities program more, unstable product quality, the present situation of complex procedures, reduces the cost in production process.
In order to reach as above object, the present invention takes following technical scheme:
A preparation method for high purity vanadic anhydride, is characterized in that, comprises following steps, and the tetravalence vanadium in the back extraction water intaking of full wet method vanadium extraction operation gained is oxidized to pentavalent vanadium; Form the supersaturation system of pentavalent vanadium, separate out poly vanadic acid precipitation, pass through solid-liquid separation, by impure high solution separating, after the washing of precipitate of poly vanadic acid, join in sulphuric acid soln, after insulated and stirred is even, add ammonium bicarbonate soln to prepare high purity product, because the solubleness of the poly ammonium vanadate generating is less than poly vanadic acid, make poly vanadic acid progressively generate the more poly ammonium vanadate precipitation of indissoluble; Poly ammonium vanadate precipitation is calcined, generate Vanadium Pentoxide in FLAKES.
The further technical scheme of the present invention is, also comprises following steps, and it is that precipitation reaction is carried out in precipitation agent that the solution after solid-liquid separation is adopted to bicarbonate of ammonia, again carries out subsequently solid-liquid separation, and solid part is calcined and generated Vanadium Pentoxide in FLAKES.
The further technical scheme of the present invention is, the poly ammonium vanadate of full wet method vanadium extraction operation gained is dissolved in NaOH solution, due under alkaline environment, iron and part metals impurity can not dissolve and exist with precipitation forms, add again reagent removal of impurities, can make silicon, phosphorus, arsenic and aluminium sedimentation, by adding flocculation agent-solid-liquid separating method, remove solid impurity, make the rich vanadium solution of alkalescence of gained pure limpid, then control precipitation system in pH >=9.5, take ammonium chloride as precipitation agent, precipitation under alkaline condition, add sequestering agent simultaneously, like this, impurity aluminum exists in solution with aluminate form, through filtering, after washing, resulting solid is white ammonium meta-vanadate, after calcination, obtain Vanadium Pentoxide in FLAKES.
The further technical scheme of the present invention is, the described oxygenant that tetravalence vanadium is oxidized to pentavalent vanadium is NaClO
3.
The further technical scheme of the present invention is, described sulphuric acid soln is that mass fraction is 15% sulfuric acid.
The further technical scheme of the present invention is, described ammonium bicarbonate soln mass concentration is 40%; Add bicarbonate of ammonia temperature 50 C; Add bicarbonate of ammonia quality and be 1.4 times of Vanadium Pentoxide in FLAKES quality in solution; 22 ℃ of mother liquor settling temperature.
The further technical scheme of the present invention is, back extraction water intaking sulfur acid 1.5mol/L; Secondary is dissolved to sulfur acid 1.5mol/L; Precipitation terminal pH=0.6; Wash temperature is greater than 90 ℃, and washing terminal PH is greater than 5.
The further technical scheme of the present invention is, NaOH initial concentration is 7.5%; Poly ammonium vanadate solvent temperature >=90 ℃; Vanadium Pentoxide in FLAKES meltage is lower than 150g/L; PH >=9.5; Removal of impurities temperature is not less than 40 ℃, filtration temperature should be below 30 ℃; Pure rich vanadium liquid after removal of impurities except ammonium, potassium, sodium and chlorion, other foreign matter content≤10ppm, otherwise should carry out secondary or repeatedly removal of impurities: adding ammonium coefficient is 1.3-1.8; Terminal PH >=8.5.
Another technical scheme of the present invention is: the purposes of bicarbonate of ammonia in precipitation.
Adopt as above the present invention of technical scheme, there is following beneficial effect: with the intermediate back extraction water intaking in the full wet method process for extracting vanadium of domestic existing bone coal navajoite process and poly ammonium vanadate, be raw material direct production high purity vanadic anhydride, do not affect existing technique main flow and production unit, Production Flow Chart is short, production cost is low, high purity vanadic anhydride Production Flow Chart and the operation of former flow process sealing and circulating, without evaporating, emitting, dripping or leaking of liquid or gas and environmental pollution.Can form the ability of producing 3000 tons of high purity vanadic anhydrides per year.
Accompanying drawing explanation
In order to further illustrate the present invention, below in conjunction with accompanying drawing, further describe:
Fig. 1 is technique for producing vanadium pentoxide and deposition vanadium mother liquid ammoniacal liquor recovery process schema;
That Fig. 2 is that poly vanadic acid supersaturation-precipitation turns is molten-ammonium bicarbonate precipitation prepares high purity vanadic anhydride process flow sheet transition;
Fig. 3 is that poly ammonium vanadate NaOH dissolving-removal of impurities-alkaline ammonium salt precipitation technique is prepared high purity vanadic anhydride process schematic representation.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are described, embodiment is not construed as limiting the invention:
Fig. 1 is full wet method process for extracting vanadium schematic flow sheet, is prior art.
In conjunction with Fig. 2: poly vanadic acid supersaturation-precipitation turns molten-ammonium bicarbonate precipitation and prepares high purity vanadic anhydride technique transition;
Utilizing the back extraction water intaking producing in the full wet method process for extracting vanadium of bone coal navajoite process is raw material, before carrying out precipitation operation, utilizes oxygenant NaClO3 that the tetravalence vanadium in solution is oxidized to pentavalent vanadium, and chemical equation is as follows:
NaClO
3+6VOSO
1+3H
2O＝3(VO
2)
2SO
4+3H
2SO
4+NaCl
Due to the solubleness of pentavalent vanadium very low (in the aqueous solution only 0.8g/L), and reduce along with the raising of temperature.Principle accordingly, when the actual oxidation operation of oxygenant, speed of response is rapid, and during oxidation, temperature is higher, and after oxidation, in back extraction water intaking, pentavalent vanadium concentration has substantially exceeded its solubleness, forms very soon the supersaturation system of pentavalent vanadium, separates out a large amount of poly vanadic acid precipitations.Pass through solid-liquid separation, by impure high solution separating, after the washing of precipitate of poly vanadic acid, join in a certain amount of pure sulphuric acid soln, after insulated and stirred is even, add ammonium bicarbonate soln, because the solubleness of the poly ammonium vanadate generating is less than poly vanadic acid, therefore, poly vanadic acid turns the more poly ammonium vanadate precipitation of indissoluble of molten generation gradually, through precipitation, make the transition, the impurity overwhelming majority enters solution, the poly ammonium vanadate good crystalline of generation, content is high, after drying, calcining, obtains high purity vanadic anhydride; And liquid portion is still by former technique precipitation, prepare 98% grade of common Vanadium Pentoxide in FLAKES, do not affect full wet method extracting vanadium from stone coal main flow and produce.
This technology key technical indicator:
1. back extraction water intaking sulfur acid 1.5mol/L;
2. secondary is dissolved to sulfur acid 1.5mol/L;
3. precipitation terminal pH=0.6;
4. wash temperature is greater than 90 ℃, and washing terminal PH is greater than 5;
5. subsequent mother liquor is returned to main flow, with the precipitation of bicarbonate of ammonia secondary.Ammonium bicarbonate soln concentration 40%; Add bicarbonate of ammonia temperature 60 C; Add bicarbonate of ammonia quality and be 1.4 times of Vanadium Pentoxide in FLAKES quality in solution; 22 ℃ of mother liquor settling temperature.
It should be explained that 1. the poly vanadic acid precipitation generating under peracid preferentially separatedly with impure high solution, solid part is molten in pure sulfuric acid system transfer, has reduced impurity and has brought into; Under acidic conditions, add bicarbonate of ammonia, by precipitation isomerization, the impurity (iron, aluminium, sodium etc.) that makes to be originally present in poly vanadic acid dissolves into into solution with constantly turning of precipitation, the poly ammonium vanadate precipitation parcel no longer newly being formed, only absorption impurity can remove by washing, and the purity of gained poly ammonium vanadate precipitation further improves; 2. adopting bicarbonate of ammonia is precipitation agent, replace the ammoniacal liquor in original technique, by controlling the conditions such as precipitation temperature, time and endpoint pH, make the raising of precipitation product purity, complete in crystal formation, precipitation rate increases substantially, ammonia residual declines, and mother liquor TAN declines, and the not treated technique of directly returning is used; 3. build mother liquor pond, can generate the bright vanadium crystal of ammonium after mother liquor is cooling, most ammonia-nitrogen exists with precipitation forms, and mother liquor, without removing ammonia through neutralization-steam stripping, can directly return to production line and use; 4. take solid-liquid separation after the oxidation of precipitation operation partly to prepare high purity vanadium, liquid portion still by the short flow and method of former technique precipitation.Therefore, adopt this technique to prepare high purity vanadium, increased added value of product, improved the Vanadium Pentoxide in FLAKES rate of recovery, greatly simplified production technique, reduced to produce consuming.
According to above scheme, with poly vanadic acid supersaturation-precipitation, turning molten-ammonium bicarbonate precipitation makes the transition and to prepare 99.5% grade of high purity vanadic anhydride.
In conjunction with Fig. 3:
The poly ammonium vanadate that adopts conventional acid ammonium salt precipitation technique gained, its major impurity is iron, aluminium, sodium element, and three's summation accounts for 2% left and right, and all the other also contain the impurity such as other a small amount of metals and silicon, phosphorus and arsenic.The poly ammonium vanadate of full wet method vanadium extraction operation gained is dissolved in NaOH dilute solution, and due under alkaline environment, iron and part metals impurity can not dissolve and exist with precipitation forms, then add certain reagent removal of impurities, can make silicon, phosphorus, arsenic and aluminium sedimentation.By adding flocculation agent-solid-liquid separating method, remove solid impurity, make the rich vanadium solution of alkalescence of gained pure limpid, then control precipitation system in pH >=9.5, take ammonium chloride as precipitation agent, precipitation under alkaline condition, add sequestering agent, like this, impurity aluminum exists in solution with aluminate form simultaneously, after filtering, washing, resulting solid is white ammonium meta-vanadate, after calcination, can guarantee that Vanadium Pentoxide in FLAKES product purity is up to more than 99.9%.Flocculation agent can be selected anion-polyacrylamide class flocculation agent, and the reagent of removal of impurities can selective chlorination magnesium; Shelter formulation piece and can select citric acid.
This technology key technical indicator is:
1. NaOH initial concentration 7.5%;
2. poly ammonium vanadate solvent temperature >=90 ℃;
3. Vanadium Pentoxide in FLAKES meltage is lower than 150g/L; PH >=9.5;
4. removal of impurities temperature is not less than 40 ℃, filtration temperature should be below 30 ℃;
5. the pure rich vanadium liquid after removal of impurities is except ammonium, potassium, sodium and chlorion, other foreign matter content≤10ppm, otherwise should carry out secondary or repeatedly removal of impurities:
6. add ammonium coefficient 1.3-1.8; Terminal PH >=8.5.
Sour leaching-extraction-precipitation technique in conjunction with actual, first adopts in milk of lime replacement of liquid ammonia and leach liquor, through precipitation, reduces the Fe in raw material
3+, Mg
2+, Al
3+, Ca
2+plasma, then after extracting-back extraction is got, can be that more than the leach liquor of 2.5g/l Vanadium Pentoxide in FLAKES is enriched to concentration 100g/L, strip liquor Fe content can be down to below 2g/L by content.
Generally speaking:
Five continents company bone coal navajoite adopts the high Ore Leaching-extraction-precipitation of full wet method technique, in acidleach process, because acidity is too high, overwhelming majority metallic impurity together leach with vanadium, leach liquor impurity is large, although get enrichment removal of impurities through extracting-back extraction, in back extraction water intaking, foreign matter content is still higher, in addition adopting ammoniacal liquor is precipitation agent, precipitation product wraps up a large amount of metals as iron, aluminium, sodium etc., the polyoxovanadate that formation contains molysite, double salt or binary double salt, employing is simply washed, even high temperature washing is difficult to these impurity to remove.Therefore, utilize the full wet processing direct production of bone coal navajoite high-purity vanadium pentoxide product to have certain difficulty.
This project is studied for this situation exactly, in poly vanadic acid supersaturation-precipitation, turning molten-ammonium bicarbonate precipitation prepares in high purity vanadic anhydride technique transition, we utilize the low feature of poly vanadic acid solubleness under peracid, first be oxidized back extraction water intaking and form poly vanadic acid precipitation, impurity element is stayed in liquid phase separated with vanadium, and then utilize poly ammonium vanadate solubleness lower than the principle of poly vanadic acid, precipitation is made the transition, during precipitation, adopting bicarbonate of ammonia is precipitation agent, make resulting poly ammonium vanadate crystalline form better, purity is higher, simultaneously deposition vanadium mother liquid needn't nitrogen removal by air stripping, mother liquor directly Returning process is used.In poly ammonium vanadate-NaOH dissolving-removal of impurities-alkaline ammonium salt precipitation technique, prepare in high purity vanadic anhydride technique, the intermediate poly ammonium vanadate of choosing full wet method process for extracting vanadium is raw material, adopt NaOH to dissolve, control strength of solution, temperature and pH value, add cleaner, flocculation agent and sequestering agent, employing ammonium chloride is sinking agent, can obtain high-quality high purity vanadic anhydride product.The principal feature of this technique is short flow process, in precipitation process, effectively utilizes sequestering agent to suppress metallic impurity and precipitates with vanadium, has improved Vanadium Pentoxide in FLAKES purity.
1. under peracid condition, utilize oxygenant NaClO
3back extraction water intaking oxidation by full wet method process for extracting vanadium, makes tetravalence vanadium all be oxidized to pentavalent vanadium, adjusts solution acidity, makes vanadium in solution generate poly vanadic acid (poly vanadic acid) precipitation, and impurity is stayed in solution, adopts liquid-solid separation to make impurity separated with vanadium.2. utilize the solubleness of poly ammonium vanadate (poly ammonium vanadate) to be less than the characteristic of poly vanadic acid (poly vanadic acid), poly vanadic acid is deposited in to pure sulfuric acid system transfer molten, reduced impurity and brought into; Under acidic conditions, add bicarbonate of ammonia, by precipitation isomerization, the impurity (iron, aluminium, sodium etc.) that makes to be originally present in poly vanadic acid dissolves into into solution with constantly turning of precipitation, no longer by newly-generated poly ammonium vanadate precipitation parcel, only absorption impurity can be removed by washing, and the purity of poly ammonium vanadate precipitation is further improved.3. adopting bicarbonate of ammonia is precipitation agent, replaces the ammoniacal liquor in original technique, by controlling the conditions such as precipitation temperature, time and endpoint pH, makes the raising of precipitation product purity, complete in crystal formation, and precipitation rate increases substantially, and ammonia residual declines, and mother liquor TAN declines.4. build mother liquor pond, can generate the bright vanadium crystal of ammonium after mother liquor is cooling, most ammonia-nitrogen exists with precipitation forms, and mother liquor is without through neutralization-steam stripping-except ammonia, can directly return to production line use.5. in the full wet method process for extracting vanadium of bone coal navajoite, can utilize the preferential high purity vanadic anhydride that extracts of back extraction water intaking, then utilize vanadium extraction mother liquor to produce common 98% grade of Vanadium Pentoxide in FLAKES.6. the back extraction water intaking of the full wet method process for extracting vanadium of bone coal navajoite of take is basis, the full wet method vanadium extraction intermediate poly ammonium vanadate of take is raw material, adopt short flow process NaOH dissolving-removal of impurities-alkaline ammonium salt precipitation technique to prepare high purity vanadic anhydride, during precipitation, add sequestering agent, suppress metallic impurity elements and precipitate with vanadium, improved Vanadium Pentoxide in FLAKES purity.
Major advantage of the present invention is: adopting intermediate back extraction water intaking and poly ammonium vanadate in the full wet method process for extracting vanadium of domestic existing bone coal navajoite process is raw material direct production high purity vanadic anhydride, do not affect existing technique main flow and production unit, Production Flow Chart is short, production cost is low, high purity vanadic anhydride Production Flow Chart and the operation of former flow process sealing and circulating, without evaporating, emitting, dripping or leaking of liquid or gas and environmental pollution.Can form the ability of producing 3000 tons of high purity vanadic anhydrides per year.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.Those skilled in the art should understand the present invention and not be restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in claimed scope.
Claims (9)
1. a preparation method for high purity vanadic anhydride, is characterized in that, comprises following steps, and the tetravalence vanadium in the back extraction water intaking of full wet method vanadium extraction operation gained is oxidized to pentavalent vanadium; Form the supersaturation system of pentavalent vanadium, separate out poly vanadic acid precipitation, pass through solid-liquid separation, by impure high solution separating, after the washing of precipitate of poly vanadic acid, join in sulphuric acid soln, after insulated and stirred is even, add ammonium bicarbonate soln to prepare high purity product, because the solubleness of the poly ammonium vanadate generating is less than poly vanadic acid, make poly vanadic acid progressively generate the more poly ammonium vanadate precipitation of indissoluble; Poly ammonium vanadate precipitation is calcined, generate Vanadium Pentoxide in FLAKES.
2. the preparation method of a kind of high purity vanadic anhydride as claimed in claim 1, it is characterized in that, also comprise following steps, it is that precipitation reaction is carried out in precipitation agent that solution after solid-liquid separation is adopted to bicarbonate of ammonia, again carry out subsequently solid-liquid separation, solid part is calcined and generated Vanadium Pentoxide in FLAKES.
3. the preparation method of a kind of high purity vanadic anhydride as claimed in claim 1, it is characterized in that, the poly ammonium vanadate of full wet method vanadium extraction operation gained is dissolved in NaOH solution, due under alkaline environment, iron and part metals impurity can not dissolve and exist with precipitation forms, add again reagent removal of impurities, can make silicon, phosphorus, arsenic and aluminium sedimentation, by adding flocculation agent-solid-liquid separating method, remove solid impurity, make the rich vanadium solution of alkalescence of gained pure limpid, then control precipitation system in pH >=9.5, take ammonium chloride as precipitation agent, precipitation under alkaline condition, add sequestering agent simultaneously, like this, impurity aluminum exists in solution with aluminate form, through filtering, after washing, resulting solid is white ammonium meta-vanadate, after calcination, obtain Vanadium Pentoxide in FLAKES.
4. the preparation method of a kind of high purity vanadic anhydride as claimed in claim 1, is characterized in that, the described oxygenant that tetravalence vanadium is oxidized to pentavalent vanadium is NaClO
3.
5. the preparation method of a kind of high purity vanadic anhydride as claimed in claim 1, is characterized in that, described sulphuric acid soln is that mass fraction is 15% sulfuric acid.
6. the preparation method of a kind of high purity vanadic anhydride as claimed in claim 1, is characterized in that, described ammonium bicarbonate soln mass concentration is 40%; Adding bicarbonate of ammonia temperature is 50 ℃; Add bicarbonate of ammonia quality and be 1.4 times of Vanadium Pentoxide in FLAKES quality in solution; 22 ℃ of mother liquor settling temperature.
7. the preparation method of a kind of high purity vanadic anhydride as claimed in claim 6, is characterized in that, back extraction water intaking sulfur acid 1.5mol/L; Secondary is dissolved to sulfur acid 1.5mol/L; Precipitation terminal pH=0.6; Wash temperature is greater than 90 ℃, and washing terminal PH is greater than 5.
8. the preparation method of a kind of high purity vanadic anhydride as claimed in claim 3, is characterized in that, NaOH initial concentration is 7.5%; Poly ammonium vanadate solvent temperature >=90 ℃; Vanadium Pentoxide in FLAKES meltage is lower than 150g/L; PH >=9.5; Removal of impurities temperature is not less than 40 ℃, filtration temperature should be below 30 ℃; Pure rich vanadium liquid after removal of impurities except ammonium, potassium, sodium and chlorion, other foreign matter content≤10ppm, otherwise should carry out secondary or repeatedly removal of impurities: terminal PH >=8.5.
9. the purposes of bicarbonate of ammonia in precipitation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310125862.2A CN104099483A (en) | 2013-04-11 | 2013-04-11 | Preparation method of highly pure vanadium pentoxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310125862.2A CN104099483A (en) | 2013-04-11 | 2013-04-11 | Preparation method of highly pure vanadium pentoxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104099483A true CN104099483A (en) | 2014-10-15 |
Family
ID=51668018
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310125862.2A Pending CN104099483A (en) | 2013-04-11 | 2013-04-11 | Preparation method of highly pure vanadium pentoxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104099483A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988337A (en) * | 2015-06-09 | 2015-10-21 | 陕西五洲矿业股份有限公司 | Stone coal vanadium ore leaching process for recycling residual acid |
| CN105087932A (en) * | 2015-09-01 | 2015-11-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing silicon in acid vanadium-enriched liquid and preparation method of vanadium oxide |
| CN106785101A (en) * | 2016-12-12 | 2017-05-31 | 东莞市佳乾新材料科技有限公司 | A kind of solid state battery based on high-purity vanadium pentoxide and preparation method thereof |
| CN107058736A (en) * | 2017-02-13 | 2017-08-18 | 广东省资源综合利用研究所 | It is a kind of from the method that vanadic anhydride is produced containing vanadium solution |
| CN107739825A (en) * | 2017-10-31 | 2018-02-27 | 成都先进金属材料产业技术研究院有限公司 | It is a kind of to utilize the method that vanadium product is prepared containing vanadium leachate |
| CN110157927A (en) * | 2019-03-27 | 2019-08-23 | 杨秋良 | A kind of no ammonium precipitation vanadium method |
| CN111020233A (en) * | 2020-01-14 | 2020-04-17 | 中南大学 | Method for preparing vanadium pentoxide by ammonium-free vanadium precipitation |
| CN111302396A (en) * | 2020-04-20 | 2020-06-19 | 承德燕北冶金材料有限公司 | Preparation method of vanadium pentoxide |
| CN113735171A (en) * | 2021-09-29 | 2021-12-03 | 河钢承德钒钛新材料有限公司 | Preparation method of vanadium pentoxide |
| CN114408971A (en) * | 2022-02-28 | 2022-04-29 | 武汉科技大学 | Method for cleanly and efficiently preparing 99-grade vanadium pentoxide |
-
2013
- 2013-04-11 CN CN201310125862.2A patent/CN104099483A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988337A (en) * | 2015-06-09 | 2015-10-21 | 陕西五洲矿业股份有限公司 | Stone coal vanadium ore leaching process for recycling residual acid |
| CN105087932A (en) * | 2015-09-01 | 2015-11-25 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing silicon in acid vanadium-enriched liquid and preparation method of vanadium oxide |
| CN105087932B (en) * | 2015-09-01 | 2017-08-25 | 攀钢集团攀枝花钢铁研究院有限公司 | The preparation method of the minimizing technology of silicon and vanadium oxide in rich acidic vanadium liquid |
| CN106785101A (en) * | 2016-12-12 | 2017-05-31 | 东莞市佳乾新材料科技有限公司 | A kind of solid state battery based on high-purity vanadium pentoxide and preparation method thereof |
| CN107058736A (en) * | 2017-02-13 | 2017-08-18 | 广东省资源综合利用研究所 | It is a kind of from the method that vanadic anhydride is produced containing vanadium solution |
| CN107058736B (en) * | 2017-02-13 | 2019-06-04 | 广东省资源综合利用研究所 | A method of vanadic anhydride is produced from containing vanadium solution |
| CN107739825B (en) * | 2017-10-31 | 2019-05-17 | 成都先进金属材料产业技术研究院有限公司 | A method of vanadium product is prepared using containing vanadium leachate |
| CN107739825A (en) * | 2017-10-31 | 2018-02-27 | 成都先进金属材料产业技术研究院有限公司 | It is a kind of to utilize the method that vanadium product is prepared containing vanadium leachate |
| CN110157927A (en) * | 2019-03-27 | 2019-08-23 | 杨秋良 | A kind of no ammonium precipitation vanadium method |
| CN111020233A (en) * | 2020-01-14 | 2020-04-17 | 中南大学 | Method for preparing vanadium pentoxide by ammonium-free vanadium precipitation |
| CN111302396A (en) * | 2020-04-20 | 2020-06-19 | 承德燕北冶金材料有限公司 | Preparation method of vanadium pentoxide |
| CN113735171A (en) * | 2021-09-29 | 2021-12-03 | 河钢承德钒钛新材料有限公司 | Preparation method of vanadium pentoxide |
| CN114408971A (en) * | 2022-02-28 | 2022-04-29 | 武汉科技大学 | Method for cleanly and efficiently preparing 99-grade vanadium pentoxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104099483A (en) | Preparation method of highly pure vanadium pentoxide | |
| CN101451200B (en) | Rare-earth enrichment recovery method from phosphorite | |
| CN102828025B (en) | Method for extracting V2O5 from stone coal navajoite | |
| CN105132720B (en) | Method for recovering rare earth in ion adsorption type rare earth ore leaching solution through fractional precipitation | |
| RU2736539C1 (en) | Method of producing vanadium oxide of a battery grade | |
| CN103771526B (en) | A kind of take industrial manganic sulfate as the method that high purity manganese sulfate prepared by raw material | |
| CN108707748B (en) | Method for purifying stone coal pickle liquor and recovering aluminum, potassium and iron | |
| CN106893877A (en) | A kind of method that vanadium chromium is extracted in the chromic acid mixed salt solution from vanadium | |
| CN102876887B (en) | Method for comprehensively recycling metal from laterite-nickel ore leaching agent | |
| CN103073061A (en) | Method for extracting tungsten and molybdenum in high molybdenum scheelite | |
| WO2012163200A1 (en) | Method for separating rare earth from phosphorus ore | |
| CN102121068A (en) | Method for preparing vanadium pentoxide | |
| CN109055757B (en) | Method for recovering manganese dioxide and lead in anode slag of electrolytic manganese or electrolytic zinc | |
| CN101880768B (en) | Method for extracting high-purity manganese dioxide from manganese slag | |
| CN106611841A (en) | Method for preparing nickel-cobalt-manganese ternary material precursor by using nickel-cobalt slag material | |
| CN113279048B (en) | Method for preparing high-purity iron phosphate from iron-containing slag | |
| CN103952560A (en) | Method for extracting vanadium from vanadium slag | |
| CN106337135A (en) | Novel method for producing vanadium pentoxide through ammonium-free vanadium precipitation | |
| CN107739040A (en) | Waste material containing lithium produces the production technology of high-purity lithium carbonate | |
| CN101585553B (en) | Method for producing vanadium pentoxide by ore containing vanadium and intermediate material containing vanadium | |
| CN103343235A (en) | Method for recovering neodymium and iron from neodymium iron boron oil sludge through two-step co-precipitation | |
| CN108396158A (en) | A kind of processing method of the complex salt crystal object of electrolytic manganese process | |
| CN104232941A (en) | Method for comprehensive recovery of molybdenum and rhenium from high molybdenum-rhenium concentrate | |
| CN109336177B (en) | Method for cleanly producing high-purity vanadium pentoxide by using hydrogen peroxide and ammonia water | |
| CN103757260A (en) | Treatment method of nickel-containing eluvial ores |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141015 |