CN103663557A - Method for preparing high-purity vanadium pentoxide from coarse vanadium - Google Patents
Method for preparing high-purity vanadium pentoxide from coarse vanadium Download PDFInfo
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Abstract
The invention provides a method for preparing high-purity vanadium pentoxide from coarse vanadium. The method comprises the steps that coarse vanadium is dissolved in caustic soda; the final pH value of dissolution is controlled to be 7 to 8.5; ferric hydroxide colloid is removed after static filtration; then hydrogen peroxide is added into the filtrate to oxidize, filter and remove the colloid; resin is exchanged by anion; after the resin is saturated, acid solution is used for analysis; analytical solution is added with ammonia molybdenum precipitation, vanadium pentoxide is produced, filtered and washed by pure water; the vanadium pentoxide is roasted to produce high-purity vanadium pentoxide with the purity of above 99.9 percent.
Description
Technical field
The present invention is the method for purification field that belongs to Vanadium Pentoxide in FLAKES, is specifically related to a kind of method that thick vanadium is prepared high purity vanadic anhydride.
Background technology
Vanadium is a kind of important resource, and because of its intrinsic physics-chem characteristic, vanadium is widely used in the every field of national defence and economic construction.Current China vanadium industry development is rapid, and especially extracting vanadium from stone coal industry is extracted constantly maturation of Vanadium Pentoxide in FLAKES technique, and novel process is constantly put in production process, impels China's vanadium industry output significantly to increase.
China current vanadium industry production enterprise common product is 98 vanadium, and in product, pentoxide content is 98%, and this product is the low-end product of vanadium industry, is generally used as the additive of steel industry, belongs to traditional Application Areas.Along with the expansion of vanadium in other field application, as at aerospace material, in the application process of special steel material and alloy, its control to impurity element requires strict, therefore also more and more higher to the purity requirement of vanadium product, for the preparation method's of high purity vanadium research, seem particularly important.The method of at present conventional purification Vanadium Pentoxide in FLAKES has the removal of impurities of the chemical precipitation method of purification, solvent extration removal of impurities and ion exchange method removal of impurities.
The production of high purity vanadic anhydride, current domestic cleaners such as Tai-Ace S 150, calcium chloride, oxalic acid, sulphosalicylic acid that mostly adopt, in different pH values, reduce vanadium respectively in the content of silicon, phosphorus, iron.Its technical process is long, and work consuming is many, and production cost is high, and Vanadium Pentoxide in FLAKES product purity does not all reach the requirement of vanadium for some high-end products mostly.
Summary of the invention
The technical problem that the present invention mainly solves is, in order to overcome in existing high purity vanadic anhydride preparation process, cost is high, technical sophistication, technical process are long, and the defects such as raw materials consumption height, are intended to propose a kind of method of preparing high purity vanadic anhydride from thick vanadium.It adopts comparatively simple technique, mainly, by techniques such as caustic soda dissolving, iron removal by oxidation, ion-exchanges, has simplified preparation technology's flow process, has reduced operation, improves the quality of products.
For achieving the above object, technical scheme of the present invention is:
Thick vanadium is prepared a method for high purity vanadic anhydride, and the method comprises the following steps:
1) thick vanadium ore grinding is extremely Powdered, make powder size be less than 0.15mm, obtain thick vanadium powder end; Described thick vanadium purity > 98%; In the sodium hydroxide solution of 1mol/L ~ 3mol/L, add described thick vanadium powder end, stir, control 30 ℃ ~ 80 ℃ of whipping temps, along with adding of thick vanadium powder end, Vanadium Pentoxide in FLAKES dissolves gradually, the pH value of solution constantly reduces, controlling pH value of solution to 7 ~ 8.5 o'clock is the terminal that adds thick vanadium powder end, stirs 1.0h-1.5h after reaching terminal again, then finishes to stir, standing 10 h ~ 30h, obtains thick vanadium solution;
2) described thick vanadium solution is filtered, remove not molten material and ferric hydroxide colloid in solution; Add again hydrogen peroxide 5mL ~ 40mL to be oxidized 10 h ~ 30h, obtain oxidizing solution; The add-on of described hydrogen peroxide is 2-3 times of the molar weight of iron in described thick vanadium solution; Described oxidizing solution is filtered, remove the ferric hydroxide colloid producing in oxidizing solution, obtain the oxidizing solution after filtration;
3) oxidizing solution after described filtration is diluted with deionized water, make V in solution
2o
5concentration is that 50 g/L ~ 80g/L is as the criterion, and obtains diluent; Described diluent is crossed to anionite-exchange resin absorption, saturated to anionite-exchange resin after, stop ionic adsorption;
4) anionite-exchange resin after the hydrochloric acid soln that is 2.0 ~ 2.5 with pH washing is saturated, is 7.0 ~ 7.5 until resin flows out the pH of solution, then uses the deionized water wash resin with respect to 5 ~ 8 times of resin volumes, to resin washings without color till;
5) use again the hydrochloric acid soln of 2.8mol/L-3.2mol/L as ion desorbed solution, described ion exchange resin is resolved, resolve to color of resin and return to before absorption, obtain the desorbed solution containing Vanadium Pentoxide in FLAKES 60g/L ~ 100g/L;
6) described desorbed solution is added to hydrogen peroxide oxidation, by weight, every 100 parts of desorbed solutions add 1mL ~ 10mL hydrogen peroxide to hydrogen peroxide add-on, then with ammoniacal liquor, adjust pH to 2 ~ 2.5, heat to 90 ℃ ~ 95 ℃, and insulation 2h ~ 3.0h, filters, and obtains throw out; Use with respect to the deionization of 3 ~ 5 times of volumes of throw out and wash 3 ~ 5 times, obtain the throw out after washing;
7) throw out after washing is calcined to 2.5 h ~ 3.0h under 500 ℃ ~ 550 ℃ conditions, obtain the Vanadium Pentoxide in FLAKES that purity is greater than 99.9%.
The described thick vanadium of step (1) is preferably 98 vanadium, mainly becomes as V
2o
5> 98%, Si < 0.2%, Fe < 0.3%, P < 0.05%, S < 0.03%, As < 0.02%, Na
2o+ K
2o < 1.5%, total impurities content < 2%.
The described anionite-exchange resin of step (4) is preferably D318 type resin anion(R.A) exchange resin.
The described hydrogen peroxide of step (2) and step (6) is that mass concentration is the hydrogen peroxide of 20%-30%, the hydrogen peroxide that more preferably mass concentration is 30%.
Below the present invention will be further explained:
High purity vanadic anhydride of the present invention refers to that purity is more than or equal to 99.9% Vanadium Pentoxide in FLAKES.
Of the present inventionly prepare in high purity vanadium method thick vanadium solution and adopt caustic soda soln, use hydrogen peroxide oxidation to produce ferric hydroxide colloid deep iron removal, containing colloidal solution, use and remove ferric hydroxide colloid, use the resin anion(R.A) exchange adsorption vanadium such as D318, realize the separated of vanadium and iron ion and sodium ion, and then output high purity vanadic anhydride.
The thick vanadium of the present invention is prepared the method for high purity vanadic anhydride, preferably use raw material for meeting 98 vanadium of the ferrous metallurgy industry standard < < Vanadium Pentoxide in FLAKES > > of the People's Republic of China (PRC) (YB/T5304-2011), mainly become as V
2o
5> 98%, Si < 0.2%, Fe < 0.3%, P < 0.05%, S < 0.03%, As < 0.02%, Na
2o+ K
2o < 1.5%, total impurities content < 2%.The method comprises the following steps:
Get a certain amount of thick vanadium (containing V
2o
598%), requiring thick vanadium is powder, and granularity is less than 0.15mm.Sodium hydroxide is mixed with to the solution of 1 ~ 3mol/L with deionized water.In sodium hydroxide solution, slowly add Powdered 98 vanadium, mechanical stirring, 30 ~ 80 ℃ of holding temperatures.Along with thick vanadium adds, Vanadium Pentoxide in FLAKES dissolves gradually, and the pH value of solution constantly reduces, and controls solution terminal pH7 ~ 8.5.Reach mechanical stirring 1.0h after terminal.Stirring finishes rear standing 10 ~ 30h.In thick vanadium solution process, present blackish greenly, present garnet after standing.
The main principles of chemistry: V
2o
5+ 2NaOH=2NaVO
3+ H
2o
Thick vanadium solution after standing filters, and filters and adopts accurate filter paper filtering, removes not molten to material and most ferric hydroxide colloid in solution.According to vanadium in solution and concentration of iron, add 5 ~ 40mL hydrogen peroxide, oxidation 10 ~ 30h, is oxidized standing rear solution container bottom and occurs white floss, and main component is ironic hydroxide.Filter, remove a small amount of ferric hydroxide colloid producing in oxidizing solution.
Oxidising process: 2H
++ Fe
2++ H
2o
2=Fe
3++ 2H
2o
Fe
3++3OH
-=Fe(OH)
3↓
Oxidizing solution after filtration is diluted to V with deionized water
2o
5concentration is 50 ~ 80g/L, slowly adds through anionite-exchange resin such as pretreated D318, and absorption flow is according to V
2o
5concentration is controlled, V in liquid after ion-exchange
2o
5concentration is generally 0.3 ~ 0.5g/L, after waiting until that exchange resin is saturated, stops ionic adsorption.
The hydrochloric acid soln that is 2.0 ~ 2.5 with pH by the ion exchange resin after saturated washing is 7.0 ~ 7.5 until resin flows out the pH of solution.With the deionized water wash resin of 5 ~ 8 times of resin volumes, guarantee that the solution flowing out from resin is without color.
With analytical pure hydrochloric acid and deionized water, prepare 3mol/L hydrochloric acid soln as ion desorbed solution.Ion exchange resin is resolved to color of resin and is returned to before absorption, obtains containing Vanadium Pentoxide in FLAKES 60 ~ 100g/L solution.
Precipitation: desorbed solution adds hydrogen peroxide oxidation, add-on adds 1 ~ 10mL hydrogen peroxide according to every 100 parts of desorbed solutions, then adjusts pH value of solution 2 ~ 2.5 with analytical pure ammoniacal liquor; Heat to 90 ~ 95 ℃, maintain 2 ~ 3.0h and obtain redness or garnet throw out, filter the red vanadium of output afterwards, the deionized water drip washing that use throw out volume is 3 ~ 5 times 3 ~ 5 times.
Red vanadium calcining: the throw out after washing is calcined to 2.5 ~ 3.0h under 500 ~ 550 ℃ of conditions, obtain pulverous high purity vanadic anhydride.
Compared with prior art, advantage of the present invention is:
1, the present invention overcomes in existing high purity vanadic anhydride preparation process that cost is high, technical sophistication, technical process be long, and the defects such as raw materials consumption height, provide a kind of method of preparing high purity vanadic anhydride.
2, of the present inventionly prepare in high purity vanadium method thick vanadium solution and adopt caustic soda soln, use hydrogen peroxide oxidation to produce ferric hydroxide colloid deep iron removal, containing colloidal solution, use and remove ferric hydroxide colloid, use the resin anion(R.A) exchange adsorption vanadium such as D318, realize the separated of vanadium and iron ion and sodium ion, thereby obtain high purity vanadic anhydride, technique is simple.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that in the embodiment of the present invention, thick vanadium is prepared high purity vanadic anhydride.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
embodiment 1
The caustic soda soln of getting 1.0L1mol/L deionized water preparation, slowly adds thick Vanadium Pentoxide in FLAKES wherein, and constantly stirs, and maintains 40 ℃ of whipping temps, controls pH value of solution most 8 ~ 9, adds altogether thick vanadium 142.5g, and solution terminal pH is 8.4.Solution was once thought sap green, and standing 24h filters, and filtrate presents redness.
In filtrate, add 10mL hydrogen peroxide, standing 20h, occurs in solution that a small amount of white floss is deposited in solution bottom, filters the vanadium solution that output is high-purity.
With deionized water diluting soln, to being wherein 80g/L containing vanadium concentration, obtain solution 1.35L and join in the exchange resin containing 300gD318 resin, control flow is 0.5h/L, and solution circulated absorption presents golden yellow until resin is saturated.Resin is with deionized water wash to neutral, and in resin, flowing out wash water pH is 7.0.
With the 3mol/L hydrochloric acid soln 1L of deionized water and hydrochloric acid preparation, slowly logical oversaturated resin, resolves the vanadium in resin, obtains containing Vanadium Pentoxide in FLAKES 90g/L solution.
To desorbed solution 1.0L, add 20mL hydrogen peroxide (mass concentration is 30%) oxidation 0.5h, in oxidising process, constantly stir, then adjust pH value of solution 2.0 with analytical pure ammoniacal liquor; Heat to 90 ~ 95 ℃, maintain 2.0h and obtain garnet throw out, filter the red vanadium of output afterwards, the deionized water drip washing that use throw out volume is 3 times 3 times.
Red vanadium calcining: the throw out after washing is calcined to 2.5 ~ 3.0h under 500 ~ 550 ℃ of conditions, obtain pulverous high purity vanadic anhydride, containing Vanadium Pentoxide in FLAKES 99.93%.
embodiment 2
The caustic soda soln of getting 1.0L2.0mol/L deionized water preparation, slowly adds thick Vanadium Pentoxide in FLAKES wherein, and constantly stirs, and maintains 60 ℃ of whipping temps, controls pH value of solution most 7 ~ 8, adds altogether thick vanadium 290g, and solution terminal pH is 7.5.Solution was once thought garnet, and standing 24h filters.
In filtrate, add 30mL hydrogen peroxide, standing 28h, occurs in solution that white floss is deposited in solution bottom, filters the vanadium solution that output is high-purity.
With deionized water diluting soln, to being wherein 90g/L containing vanadium concentration, obtain solution 2.90L and join in the exchange resin containing D318 resin, control flow is 0.5h/L, and solution circulated absorption presents golden yellow until resin is saturated.Resin is first 7.0 with the analytical pure hydrochloric acid soln drip washing of pH2.5 to flowing out pH value of solution in resin.Extremely neutral with deionized water wash again, in resin, flowing out wash water pH is 7.0.
With the 3mol/L hydrochloric acid soln 1.5L of deionized water and hydrochloric acid preparation, slowly logical oversaturated resin, resolves the vanadium in resin, obtains containing Vanadium Pentoxide in FLAKES 105g/L solution.
To desorbed solution 1.5L, add 40mL hydrogen peroxide (mass concentration is 30%) oxidation 1.0h, in oxidising process, constantly stir, then adjust pH value of solution 2.0 with analytical pure ammoniacal liquor; Heat to 90 ~ 95 ℃, maintain 1.5h and obtain garnet throw out, filter the red vanadium of output afterwards, the deionized water drip washing that use throw out volume is 5 times 4 times.
Red vanadium calcining: the throw out after washing is calcined to 2.5 ~ 3.0h under 500 ~ 550 ℃ of conditions, obtain pulverous high purity vanadic anhydride, containing Vanadium Pentoxide in FLAKES 99.99%.
Claims (4)
1. thick vanadium is prepared a method for high purity vanadic anhydride, it is characterized in that, the method comprises the following steps:
1) thick vanadium ore grinding is extremely Powdered, make powder size be less than 0.15mm, obtain thick vanadium powder end; Described thick vanadium purity > 98%; In the sodium hydroxide solution of 1mol/L ~ 3mol/L, add described thick vanadium powder end, stir, control 30 ℃ ~ 80 ℃ of whipping temps, along with adding of thick vanadium powder end, Vanadium Pentoxide in FLAKES dissolves gradually, the pH value of solution constantly reduces, controlling pH value of solution to 7 ~ 8.5 o'clock is the terminal that adds thick vanadium powder end, stirs 1.0h-1.5h after reaching terminal again, then finishes to stir, standing 10 h ~ 30h, obtains thick vanadium solution;
2) described thick vanadium solution is filtered, remove not molten material and ferric hydroxide colloid in solution; Add again hydrogen peroxide 5mL ~ 40mL to be oxidized 10 h ~ 30h, obtain oxidizing solution; The add-on of described hydrogen peroxide is 2-3 times of the molar weight of iron in described thick vanadium solution; Described oxidizing solution is filtered, remove the ferric hydroxide colloid producing in oxidizing solution, obtain the oxidizing solution after filtration;
3) oxidizing solution after described filtration is diluted with deionized water, make V in solution
2o
5concentration is that 50 g/L ~ 80g/L is as the criterion, and obtains diluent; Described diluent is crossed to anionite-exchange resin absorption, saturated to anionite-exchange resin after, stop ionic adsorption;
4) anionite-exchange resin after the hydrochloric acid soln that is 2.0 ~ 2.5 with pH washing is saturated, is 7.0 ~ 7.5 until resin flows out the pH of solution, then uses the deionized water wash resin with respect to 5 ~ 8 times of resin volumes, to resin washings without color till;
5) use again the hydrochloric acid soln of 2.8mol/L-3.2mol/L as ion desorbed solution, described ion exchange resin is resolved, resolve to color of resin and return to before absorption, obtain the desorbed solution containing Vanadium Pentoxide in FLAKES 60g/L ~ 100g/L;
6) described desorbed solution is added to hydrogen peroxide oxidation, by weight, every 100 parts of desorbed solutions add 1mL ~ 10mL hydrogen peroxide to hydrogen peroxide add-on, then with ammoniacal liquor, adjust pH to 2 ~ 2.5, heat to 90 ℃ ~ 95 ℃, and insulation 2h ~ 3.0h, filters, and obtains throw out; Use with respect to the deionization of 3 ~ 5 times of volumes of throw out and wash 3 ~ 5 times, obtain the throw out after washing;
7) throw out after washing is calcined to 2.5 h ~ 3.0h under 500 ℃ ~ 550 ℃ conditions, obtain the Vanadium Pentoxide in FLAKES that purity is greater than 99.9%.
2. thick vanadium is prepared the method for high purity vanadic anhydride according to claim 1, it is characterized in that, the described thick vanadium of step (1) is 98 vanadium, mainly becomes as V
2o
5> 98%, Si < 0.2%, Fe < 0.3%, P < 0.05%, S < 0.03%, As < 0.02%, Na
2o+ K
2o < 1.5%, total impurities content < 2%.
3. according to thick vanadium described in claim 1 or 2, prepare the method for high purity vanadic anhydride, it is characterized in that, the described anionite-exchange resin of step (4) is D318 type resin anion(R.A) exchange resin.
4. according to thick vanadium described in claim 1 or 2, prepare the method for high purity vanadic anhydride, it is characterized in that, the described hydrogen peroxide of step (2) and step (6) is that mass concentration is the hydrogen peroxide of 20%-30%.
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Cited By (6)
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| CN104386747A (en) * | 2014-11-18 | 2015-03-04 | 河北钢铁股份有限公司承德分公司 | Method for preparing high-purity vanadium oxide employing ion exchange method |
| US10053371B2 (en) | 2015-01-30 | 2018-08-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for preparing high-purity vanadium pentoxide powder |
| 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 |
| 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386747A (en) * | 2014-11-18 | 2015-03-04 | 河北钢铁股份有限公司承德分公司 | Method for preparing high-purity vanadium oxide employing ion exchange method |
| CN104386747B (en) * | 2014-11-18 | 2016-03-30 | 河北钢铁股份有限公司承德分公司 | A kind of ion exchange method prepares the method for high purity barium oxide |
| US10053371B2 (en) | 2015-01-30 | 2018-08-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for preparing high-purity vanadium pentoxide powder |
| 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 |
| 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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