CN102923775A - Preparation method of high-purity vanadium pentoxide - Google Patents
Preparation method of high-purity vanadium pentoxide Download PDFInfo
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- CN102923775A CN102923775A CN2012104885664A CN201210488566A CN102923775A CN 102923775 A CN102923775 A CN 102923775A CN 2012104885664 A CN2012104885664 A CN 2012104885664A CN 201210488566 A CN201210488566 A CN 201210488566A CN 102923775 A CN102923775 A CN 102923775A
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Abstract
The invention discloses a preparation method of high-purity vanadium pentoxide. The preparation method comprises the following steps of: returning and dissolving coarse vanadium in aqueous alkali, and filtering the solution to remove metal impurities, which are subjected to precipitation reaction with the aqueous alkali, in the coarse vanadium, thus obtaining a primary returned solution; slowly pouring the primary returned solution into a sulfuric acid solution, adjusting the pH value of the solution to be 1.0-2.0 to obtain a liquid-solid mixture, and performing solid-liquid separation on the liquid-solid mixture; filtering and washing precipitates obtained from the solid-liquid separation of the mixture, and returning and dissolving the mixture into the aqueous alkali, thus obtaining a secondary returned solution; adding ammonium sulfate into the secondary returned solution for precipitating vanadium, and filtering the solution to obtain ammonium metavanadate; and processing the ammonium metavanadate to obtain the high-purity vanadium pentoxide. The preparation method adopting multiple stages of returned dissolving can be used for effectively removing the metal canon impurities of the vanadium pentoxide, and further obtaining the high-purity vanadium pentoxide with the metal canon impurity contents of less than 0.001% and the vanadium pentoxide content of 99.99%.
Description
Technical field
The present invention relates to a kind of preparation method of Vanadium Pentoxide in FLAKES, more particularly, relate to a kind of multistage preparation method that molten operation prepares high-purity vanadium pentoxide that returns that utilizes.
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.Because vanadium is at aerospace material, in the application process of special steel material and alloy, its control to impurity element is strict, and is therefore also more and more higher to the purity requirement of vanadium product, seems particularly important for the preparation method's of high purity vanadium research.Contain navajoite according to difference and produce resource, impurity element and content in the vanadium product are different, but most of impurity element is metallic impurity and silicon.The method of purification Vanadium Pentoxide in FLAKES commonly used has the removal of impurities of the chemical precipitation method of purification, solvent extration removal of impurities and ion exchange method removal of impurities at present.
At present, by solvent extration removal of impurities and ion exchange method removal of impurities, its main advantage is, for the lower solution of vanadium concentration, can carry out the enrichment of vanadium by extraction or ion-exchange, carries out the production of vanadium product after reaching certain vanadium concentration again.But extraction agent and ion exchange resin are along with the increase of vanadium concentration, and consumption can sharply increase, and cause the production cost of whole vanadium product to raise, thereby are applied in the suitability for industrialized production relatively less; The removal of impurities of the chemical precipitation method of purification be by adding precipitation agent impurity element in the vanadium to be removed, but its technical process is longer, and complicated operation, also can cause the impurity element in the precipitation agent to be introduced in the vanadium product, causes the purity of vanadium product to be difficult to improve.
Summary of the invention
For the deficiencies in the prior art, one of purpose of the present invention is to solve the one or more problems that exist in the above-mentioned prior art.
To achieve these goals, the invention provides a kind of preparation method of high-purity vanadium pentoxide, described preparation method comprises the steps: thick vanadium returned and is dissolved in the alkaline solution, filters to remove in the thick vanadium metallic impurity with alkaline solution generation precipitin reaction, obtains the first step and returns solution; The first step of gained is returned solution slowly pour in the sulphuric acid soln, and regulate pH value to 1.0～2.0, obtain solidliquid mixture and carry out solid-liquid separation; The throw out that solid-liquid separation is obtained obtains the second stage and returns solution through filtering, after the washing, again returning and be dissolved in the alkaline solution; Return solution adding ammonium sulfate to the second stage of gained and carry out precipitation, filter and obtain ammonium meta-vanadate; Process described ammonium meta-vanadate high-purity Vanadium Pentoxide in FLAKES.
According to the preparation method's of a high-purity vanadium pentoxide of the present invention embodiment, described sodium hydroxide solution adopts the sodium hydroxide solution of analytical pure level.
According to the preparation method's of a high-purity vanadium pentoxide of the present invention embodiment, the step of described processing ammonium meta-vanadate can comprise: with described ammonium meta-vanadate filtration washing 3 times, solid-to-liquid ratio is 1: 2; Then obtained high-purity vanadium pentoxide in 2～2.5 hours 50 ℃～60 ℃ oven dry, and 500～550 ℃ of roastings.
According to the preparation method's of a high-purity vanadium pentoxide of the present invention embodiment, described thick vanadium is the metallurgical grade Vanadium Pentoxide in FLAKES.
According to the preparation method's of a high-purity vanadium pentoxide of the present invention embodiment, in the step of described adjusting pH value, take the ratio adding ionized water of liquid-solid ratio as 1: 1.
An embodiment according to the preparation method of high-purity vanadium pentoxide of the present invention in described precipitation step, returns the solution water-bath with the described second stage and is heated to 50 ℃～60 ℃.
An embodiment according to the preparation method of high-purity vanadium pentoxide of the present invention, return in the described filtration step of solution in the acquisition first step, can comprise the essence filtration of first step coarse filtration and the second stage, wherein, described first step coarse filtration filters out the macrobead throw out of particle diameter greater than 80 microns, and described second stage essence is filtered the throw out of particle diameter greater than 5 microns filtered out.
According to the preparation method's of a high-purity vanadium pentoxide of the present invention embodiment, described alkaline solution is sodium hydroxide solution.
The present invention can make highly purified Vanadium Pentoxide in FLAKES, compared with prior art, beneficial effect of the present invention comprises that technological process is simple, easy to operate, can effectively remove cation impurity in the Vanadium Pentoxide in FLAKES, and not introduce in process of production other impurity elements and environmental pollution little etc.
Embodiment
The invention provides a kind of preparation method of high-purity vanadium pentoxide, described preparation method comprises the steps:
(1) thick vanadium is returned is dissolved in alkaline solution, then filter to remove in the thick vanadium metallic impurity with alkaline solution generation precipitin reaction, obtain the first step and return solution.
Wherein, thick vanadium is the metallurgical grade Vanadium Pentoxide in FLAKES, contains the nonmetallic ion impurity such as impurity metal ions such as chromium, sodium and silicon in the used thick vanadium of the present invention.Preferably, alkaline solution adopts sodium hydroxide solution, further, sodium hydroxide solution can adopt the sodium hydroxide solution of analytical pure level, certainly other can dissolve in the thick vanadium vanadium and with thick vanadium in metallic cation reaction generate the alkaline solution of precipitation of hydroxide can.In one exemplary embodiment of the present invention, in order to improve filtration efficiency, save filtration time, filtering and impurity removing is divided into two steps, comprise the essence filtration of first step coarse filtration and the second stage, first step coarse filtration refers to particle diameter is removed fast greater than 80 microns macrobead throw out, and second stage essence is filtered and referred to particle diameter is removed greater than 5 microns throw out.Filtration can be adopted various ways, can use Büchner funnel, band filter or pressure filter, wherein industrial general employing Bush funnel.
(2) first step of gained is returned solution and slowly poured in the sulphuric acid soln, stir simultaneously, and regulate pH value to 1.0～2.0, for acid precipitation provides favourable condition, if the pH value, then can cause the vanadium loss not in this interval.In this process, return the continuous adding of solution along with the first step, a large amount of red solid are produced in reaction, soltion viscosity strengthens, add deionized water with 1: 1 ratio of liquid-solid ratio this moment, and diluting soln is beneficial to impurity Si and enters liquid phase, and vanadium enters solid phase, obtain solidliquid mixture, and carry out solid-liquid separation by methods commonly used such as suction filtrations.
(3) throw out that solid-liquid separation is obtained is through filtering, washing to remove various metallic cations, and in an example of the present invention, after three washings, a large amount of silicon, chromium enter in the filtered liquid.In washing process, the part vanadium ion enters in the filtrate, for the vanadium ion that is lost in the solution is recycled, the filtrate cycle detergent can be used.Throw out after then will washing returns to be dissolved in the alkaline solution to throw out and dissolves fully, obtains the second stage and returns solution.Here the preferred sodium hydroxide solution of alkaline solution, in returning molten process, usually, the throw out after at first will filtering and a certain proportion of water mix, and then add sodium hydrate solid throw out is dissolved.
(4) return solution to the second stage of gained and add ammonium sulfate, carry out precipitation except sodium.In precipitation except before the sodium, in order to improve the yield of ammonium meta-vanadate, and make be heated more even, can return solution to the second stage carries out heating in water bath and temperature is controlled at 50 ℃～60 ℃, after stirring reaction is complete, filters and obtain ammonium meta-vanadate, sodium ion is stayed in the filtered liquid.
(5) process described ammonium meta-vanadate high-purity Vanadium Pentoxide in FLAKES.Preferably, in another exemplary embodiment of the present invention, process ammonium meta-vanadate and comprise: with ammonium meta-vanadate filtration washing 3 times, solid-to-liquid ratio is 1: 0.5～and 1: 2, wherein, " Gu " refer to throw out, " liquid " refers to deionized water.Then the metavanadic acid acid ammonium that filtration is obtained obtained high-purity vanadium pentoxide in 2～2.5 hours 500～550 ℃ of roastings after 50 ℃～60 ℃ oven dry.
Come the preparation method of high-purity vanadium pentoxide of the present invention is further described below in conjunction with concrete example.Following example only is used for explanation the present invention, rather than limits by any way the present invention.
Example 1
The thick vanadium of 100g returned be dissolved in the sodium hydroxide solution (being mixed by 50g sodium hydrate solid and 400ml deionized water), the gained pH is 8.93, then filters to remove insoluble impurity, obtains the first step and returns solution; With the 200ml vitriol oil and 600ml deionized water preparation sulphuric acid soln, again the 1100ml first step of gained being returned solution slowly pours in the sulphuric acid soln for preparing, stir simultaneously, and adjusting pH value to 1.0, in this process, return the continuous adding of solution along with the first step, a large amount of red solid are produced in reaction, soltion viscosity strengthens, add deionized water with 1: 1 ratio of liquid-solid ratio this moment, diluting soln is beneficial to impurity Si and enters liquid phase, vanadium enters solid phase, obtains solidliquid mixture, and realizes solid-liquid separation by suction filtration, the throw out that solid-liquid separation obtains is through filtering, after the washing, by analysis: the massfraction of vanadium is 47% in the solid sediment, the massfraction of sodium is 3%, the massfraction of silicon is 0.008%, the massfraction of chromium＜0.001%.Then claim throw out after the 650g washing again to return to be dissolved in the sodium hydroxide solution to dissolve fully to throw out, obtain the second stage and return solution, measuring its pH value is 9.8; Solution is returned in the second stage carry out heating in water bath and temperature is controlled at 50 ℃, then add 750g ammonium sulfate, stirring reaction one hour filters and obtains ammonium meta-vanadate; With ammonium meta-vanadate filtration washing 3 times, solid-to-liquid ratio is 1: 2; Then the metavanadic acid acid ammonium that filtration is obtained is after 50 ℃ of oven dry, and under 500 ℃ of conditions, roasting obtained high-purity vanadium pentoxide in 2 hours in retort furnace, took out in the roasting process and stirred once so that ammonium meta-vanadate fully reacts.
Example 2
The thick vanadium of 100g returned be dissolved in the sodium hydroxide solution (being mixed by 50g sodium hydrate solid and 400ml deionized water), the gained pH is 8.93, then filters to remove insoluble impurity, obtains the first step and returns solution; With the 200ml vitriol oil and 600ml deionized water preparation sulphuric acid soln, again the 1100ml first step of gained being returned solution slowly pours in the sulphuric acid soln for preparing, stir simultaneously, and adjusting pH value to 2.0, in this process, return the continuous adding of solution along with the first step, a large amount of red solid are produced in reaction, soltion viscosity strengthens, add deionized water with 1: 1 ratio of liquid-solid ratio this moment, diluting soln is beneficial to impurity Si and enters liquid phase, vanadium enters solid phase, obtains solidliquid mixture, and realizes solid-liquid separation by suction filtration, the throw out that solid-liquid separation obtains is through filtering, after the washing, by analysis: the massfraction of vanadium is 47% in the solid sediment, the massfraction of sodium is 3%, the massfraction of silicon is 0.008%, the massfraction of chromium＜0.001%.Then claim throw out after the 650g washing again to return to be dissolved in the sodium hydroxide solution to dissolve fully to throw out, obtain the second stage and return solution, measuring its pH value is 9.8; Solution is returned in the second stage carry out heating in water bath and temperature is controlled at 60 ℃, then add 750g ammonium sulfate, stirring reaction one hour filters and obtains ammonium meta-vanadate; With ammonium meta-vanadate filtration washing 3 times, solid-to-liquid ratio is 1: 0.5; Then the metavanadic acid acid ammonium that filtration is obtained is after 60 ℃ of oven dry, and under 550 ℃ of conditions, roasting obtained high-purity vanadium pentoxide in 2.5 hours in retort furnace.
Composition contrast in the thick vanadium of table 1 and the rear Vanadium Pentoxide in FLAKES of purifying
Table 1 has provided the Vanadium Pentoxide in FLAKES (numbering 2), the example 2 (numbering 3) that the obtain composition comparative analysis in the Vanadium Pentoxide in FLAKES that obtains of purifying of purifying of thick vanadium (numbering 1), example 1, and wherein, the per-cent of each composition is massfraction in the table.Can find out, adopt and of the present inventionly multistagely return that various metallic cation foreign matter contents are all less than 0.001% in the Vanadium Pentoxide in FLAKES that molten thick vanadium product prepares, pentoxide content reaches 99.99%.
In sum, the preparation method of high-purity vanadium pentoxide of the present invention can effectively remove the metallic cation impurity in the Vanadium Pentoxide in FLAKES, obtain various metallic cation foreign matter contents all less than 0.001% high-purity vanadium pentoxide, wherein, the content of Vanadium Pentoxide in FLAKES reaches more than 99.99%.Method of the present invention also have technological process simple, easy to operate, and do not introduce in process of production the advantages such as other impurity elements and environmental pollution are little.
Although the above has described method of the present invention in conjunction with exemplary embodiment, yet, it will be understood by those skilled in the art that in the situation of the scope that does not break away from the claim protection, can carry out various changes to above-mentioned exemplary embodiment.
Claims (8)
1. the preparation method of a high-purity vanadium pentoxide is characterized in that, described preparation method comprises the steps:
Thick vanadium returned be dissolved in the alkaline solution, filter to remove in the thick vanadium metallic impurity with alkaline solution generation precipitin reaction, obtain the first step and return solution;
The described first step is returned solution slowly pour in the sulphuric acid soln, and regulate pH value to 1.0～2.0, obtain solidliquid mixture and carry out solid-liquid separation;
The throw out that solid-liquid separation is obtained obtains the second stage and returns solution through filtering, after the washing, again returning and be dissolved in the alkaline solution;
Return solution adding ammonium sulfate to the described second stage and carry out precipitation except sodium, filter and obtain ammonium meta-vanadate;
Process described ammonium meta-vanadate high-purity Vanadium Pentoxide in FLAKES.
2. the preparation method of high-purity vanadium pentoxide according to claim 1 is characterized in that, described sodium hydroxide solution adopts the sodium hydroxide solution of analytical pure level.
3. the preparation method of high-purity vanadium pentoxide according to claim 1 is characterized in that, the step of described processing ammonium meta-vanadate comprises:
With described ammonium meta-vanadate filtration washing 3 times, solid-to-liquid ratio is 1: 2; Then obtained high-purity vanadium pentoxide in 2～2.5 hours 50 ℃～60 ℃ oven dry, and 500～550 ℃ of roastings.
4. the preparation method of high-purity vanadium pentoxide according to claim 1 is characterized in that, described thick vanadium is the metallurgical grade Vanadium Pentoxide in FLAKES.
5. the preparation method of high-purity vanadium pentoxide according to claim 1 is characterized in that, in the step of described adjusting pH value, take the ratio adding ionized water of liquid-solid ratio as 1: 1.
6. the preparation method of high-purity vanadium pentoxide according to claim 1 is characterized in that, in described precipitation step, the solution water-bath is returned in the described second stage be heated to 50 ℃～60 ℃.
7. the preparation method of high-purity vanadium pentoxide according to claim 1, it is characterized in that, obtaining the first step returns in the described filtration step of solution, comprise the essence filtration of first step coarse filtration and the second stage, wherein, described first step coarse filtration filters out the macrobead throw out of particle diameter greater than 80 microns, and described second stage essence is filtered the throw out of particle diameter greater than 5 microns filtered out.
8. the preparation method of high-purity vanadium pentoxide according to claim 1 is characterized in that, described alkaline solution is sodium hydroxide solution.
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Cited By (14)
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| CN104017993A (en) * | 2014-06-11 | 2014-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium oxide by using sodium salt roasting lixivium of titanium tetrachloride refined tailings |
| CN104477992A (en) * | 2015-01-07 | 2015-04-01 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
| CN104495925A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团研究院有限公司 | Method for preparing sodium metavanadate |
| CN106430307A (en) * | 2016-08-30 | 2017-02-22 | 攀枝花学院 | Preparation method of high-purity vanadium pentoxide |
| 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 |
| 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 |
| 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 |
| CN108975402A (en) * | 2018-10-25 | 2018-12-11 | 河钢股份有限公司承德分公司 | A method of preparing bulky grain high purity vanadic anhydride |
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| US10294118B2 (en) | 2015-01-30 | 2019-05-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for purifying vanadium pentoxide |
| CN115286038A (en) * | 2022-08-08 | 2022-11-04 | 吉林吉恩镍业股份有限公司 | Method for producing ammonium metavanadate by taking phosphorus removal slag as raw material |
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Cited By (18)
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| CN104017993B (en) * | 2014-06-11 | 2016-11-16 | 攀钢集团攀枝花钢铁研究院有限公司 | The method that vanadium oxide prepared by the sodium roasting leachate of tailings is refined with titanium tetrachloride |
| CN104017993A (en) * | 2014-06-11 | 2014-09-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium oxide by using sodium salt roasting lixivium of titanium tetrachloride refined tailings |
| CN104477992A (en) * | 2015-01-07 | 2015-04-01 | 攀钢集团研究院有限公司 | Method for preparing vanadium pentoxide |
| CN104495925A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团研究院有限公司 | Method for preparing sodium metavanadate |
| 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 |
| US10294118B2 (en) | 2015-01-30 | 2019-05-21 | Institute Of Process Engineering, Chinese Academy Of Sciences | System and method for purifying vanadium pentoxide |
| 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 |
| 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 |
| 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 |
| CN106430307A (en) * | 2016-08-30 | 2017-02-22 | 攀枝花学院 | Preparation method of high-purity vanadium pentoxide |
| CN106430307B (en) * | 2016-08-30 | 2018-04-20 | 攀枝花学院 | A kind of high purity vanadic anhydride preparation method |
| 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 |
| 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 |
| 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 |
| CN108975402A (en) * | 2018-10-25 | 2018-12-11 | 河钢股份有限公司承德分公司 | A method of preparing bulky grain high purity vanadic anhydride |
| CN109502644A (en) * | 2019-01-02 | 2019-03-22 | 成都先进金属材料产业技术研究院有限公司 | The method that alkalinity prepares high purity vanadic anhydride containing vanadium leachate |
| CN115286038A (en) * | 2022-08-08 | 2022-11-04 | 吉林吉恩镍业股份有限公司 | Method for producing ammonium metavanadate by taking phosphorus removal slag as raw material |
| CN115286038B (en) * | 2022-08-08 | 2023-10-10 | 吉林吉恩镍业股份有限公司 | Method for producing ammonium metavanadate by taking dephosphorization slag as raw material |
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Application publication date: 20130213 |