CN101723455A - Method for preparing sodium metavanadate - Google Patents
Method for preparing sodium metavanadate Download PDFInfo
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- CN101723455A CN101723455A CN200910265893A CN200910265893A CN101723455A CN 101723455 A CN101723455 A CN 101723455A CN 200910265893 A CN200910265893 A CN 200910265893A CN 200910265893 A CN200910265893 A CN 200910265893A CN 101723455 A CN101723455 A CN 101723455A
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- sodium
- solidliquid mixture
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- leach liquor
- vanadium
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Abstract
The invention discloses a method for preparing sodium metavanadate, which comprises the following steps: a. adjusting the pH value of a leach solution obtained by sodium treatment and vanadium extraction to 1.1-1.6 by an inorganic acid, then heating the leach solution to 90 DEG C until boiling, and keeping for 60-90 minutes to generate solid sodium polyvanadate; b. adding sodium hydroxide solution to the obtained solid sodium polyvanadate, and stirring the obtained solid-liquid mixture, so that the pH value of the solution in the solid-liquid mixture is 8-8.5; and c. heating the solid-liquid mixture to 90 DEG C until boiling to generate solid sodium metavanadate. By the method, high-purity sodium metavanadate can be prepared and the method has small consumption of alkali and low cost.
Description
Technical field
The present invention relates to a kind of method for preparing sodium metavanadate, more particularly, relate to a kind of method for preparing sodium metavanadate by sodium vanadium extraction leach liquor.
Background technology
Sodium metavanadate (NaVO
3) of many uses at chemical field, useful as catalysts, siccative, mordant are made ammonium vanadate and potassium metavanadate, also can be used for medical image, plant inoculation and inhibitor etc.At present, can extract sodium metavanadate from the sodium roasting leach liquor that contains vanadium, main method has two kinds.
First method is with evaporating, concentrating and crystallizing after the removal of impurities of vanadium extraction leach liquor, thereby obtains the sodium metavanadate solid.This method technology is simple, easy to operate, but vanadium extraction leach liquor complicated component, and Impurity removal is incomplete, cause product purity not high, so this method is difficult to be used widely.
Second method is to make vanadium extraction leach liquor precipitation ammonium poly-vanadate earlier, uses sodium hydroxide and ammonium poly-vanadate prepared in reaction sodium metavanadate then.Specifically, adding ammonium salt to the vanadium extraction leach liquor under 90 ℃～95 ℃ is precipitated out ammonium poly-vanadate, the ammonium poly-vanadate solid that filtration obtains wetting, then with water dissolution wet ammonium poly-vanadate solid and sodium hydrate solid, ammonium poly-vanadate and sodium hydroxide generate sodium metavanadate and ammonia in liquid phase reaction, and concentration of reaction solution obtains the sodium metavanadate solid afterwards.The shortcoming of this method is to need in the molten process to use and the sodium hydroxide of vanadium with equimolar amount returning with sodium hydroxide, and quantity of alkali consumption is big, so production cost is higher.In addition, ammonium poly-vanadate presents cotton-shaped usually or exists with the form of polycrystalline aggregate, contains impurity such as sodium sulfate and is difficult for washing, causes product purity not high.In addition, this method produces waste gas (ammonia).
In addition, also having a kind of method is to dissolve V with sodium hydroxide solution under the condition of heating
2O
5, fully obtain sodium metavanadate after the reaction.This method is easy to operate, and the product purity height does not produce and pollutes waste gas (ammonia), is present most popular method.But this method is to V
2O
5Purity requirement is higher, V
2O
5Price is more expensive, so the production cost height.
Summary of the invention
The method for preparing sodium metavanadate that provides a kind of product purity high is provided one object of the present invention.
The method for preparing sodium metavanadate that provides a kind of quantity of alkali consumption little is provided.
The method for preparing sodium metavanadate that provides a kind of cost low is provided another purpose of the present invention.
The method for preparing sodium metavanadate according to the present invention may further comprise the steps: a. is adjusted to 1.1～1.6 with mineral acid with the pH value of sodium vanadium extraction leach liquor, is heated 90 ℃ then to boiling, keeps 60～90 minutes, generates many vanadic acid sodiums solid; B. add sodium hydroxide solution to many vanadic acid sodiums solid of gained, and stir the solidliquid mixture of gained, make that the pH value of the solution in the solidliquid mixture is 8～8.5; C. solidliquid mixture is heated to 90 ℃ to boiling, generates the sodium metavanadate solid.
According to an aspect of the present invention, sodium vanadium extraction leach liquor contains the V of 20～30g/L
5+, 15～20g/L Na
+, 1～1.5g/L Cr
6+, 0.5～1g/L the Si element and be less than the P element of 0.05g/L.
According to an aspect of the present invention, prepare sodium vanadium extraction leach liquor by following steps: to vanadium slag, bone coal with contain at least a at least a interpolation yellow soda ash in the vanadium solid waste, sodium-chlor, the sodium sulfate, the vanadium of multivalence attitude is converted into the sodium salt of water-soluble pentavalent vanadium by roasting, again product of roasting is carried out water logging, thereby obtain sodium vanadium extraction leach liquor.
According to an aspect of the present invention, step a also comprises: sodium vanadium extraction leach liquor is being remained on 90 ℃ to the process of boiling state, adding mineral acid to sodium vanadium extraction leach liquor, making that the pH value of sodium vanadium extraction leach liquor is 1.1～1.6.
According to an aspect of the present invention, mineral acid is at least a in sulfuric acid, hydrochloric acid, the nitric acid.
According to an aspect of the present invention, mineral acid is that concentration is the sulfuric acid more than 98%.
According to an aspect of the present invention, the step of adding sodium hydroxide solution and stirring the solidliquid mixture of gained to many vanadic acid sodiums solid of gained comprises: adding mass concentration to many vanadic acid sodiums solid of gained is 40%～50% sodium hydroxide solution, and fully stirs the solidliquid mixture of gained.
According to an aspect of the present invention, step c also comprises: solidliquid mixture being heated to 90 ℃ to the boiling, solidliquid mixture is remained on 90 ℃ to boiling, till the white that occurs or faint yellow solid no longer increase.
According to an aspect of the present invention, solidliquid mixture was kept 60～120 minutes to boiling state at 90 ℃.
According to an aspect of the present invention,, add sodium hydroxide solution, make that the pH value of the solution in the solidliquid mixture is 8～8.5 to solidliquid mixture solidliquid mixture being remained on 90 ℃ to the ebullient process.
The method for preparing sodium metavanadate of the present invention has following advantage: the raw material type of (1) preparation sodium metavanadate is few, has only sodium vanadium extraction leach liquor, mineral acid and sodium hydroxide solution; (2) by not having environmental pollution in conjunction with electrodialysis process, whole process does not have waste gas such as sulfurous gas, ammonia to produce; (3) technological operation is simple, is convenient to suitability for industrialized production.
Embodiment
At first, the pH value of sodium vanadium extraction leach liquor is adjusted to 1.1～1.6, is heated 90 ℃ then, kept 60～90 minutes to boiling with mineral acid.In this process, the soluble vanadium acid group is along with progressively hydrolysis of solution acidic increase, generates many vanadic acid root (six vanadic acid root V for example
6O
16 2-, ten vanadic acid root V
10O
28 6-, 12 vanadic acid root V
12O
31 2-, V
12O
32 4-, V
12O
33 6-Deng).Preferably, keep 90 ℃ of stirred solutions to boiling state the time, to promote the carrying out of reaction.
Sodium vanadium extraction leach liquor can contain the V of 20～30g/L
5+, 15～20g/L Na
+, 1～1.5g/L Cr
6+, 0.5～1g/L the Si element and be less than the P element of 0.05g/L, yet the sodium vanadium extraction leach liquor that the present invention uses is not limited thereto.The preparation of sodium vanadium extraction leach liquor is known to those skilled in the art.For example, to vanadium slag, bone coal with contain at least a adding sodium salt additive (for example yellow soda ash, sodium-chlor, sodium sulfate etc.) in the vanadium solid waste, the vanadium of multivalence attitude is converted into the sodium salt of water-soluble pentavalent vanadium by roasting, to the direct water logging of sodium roasting product, can contain the vanadium extraction leach liquor of vanadium and small amount of impurities again.Can get vanadium-bearing hot metal through blast-furnace smelting by v-ti magnetite concentrate, obtain vanadium slag through bessemerizing again.
According to the method for preparing sodium metavanadate of the present invention, with mineral acid the pH value of sodium vanadium extraction leach liquor is adjusted to 1.1～1.6, be heated to 90 ℃ then to boiling state insulation 60～90 minutes down, vanadium hydrolytic precipitation rate is reached more than 99.5%.In the process of insulation, carry out more fully in order to guarantee reaction, can add mineral acid to reactant and make the pH value maintain 1.1～1.6.
If the pH value is less than 1.1, then not only acid consumption increases, and vanadium easily changes into the VO of solubilised state
2 +Positively charged ion, the vanadium deposition rate significantly descends.If the pH value is greater than 1.6, then the solvability of many vanadic acid radical ion strengthens, and the vanadium deposition rate significantly descends.Mineral acid can be selected at least a in sulfuric acid, hydrochloric acid, the nitric acid etc. for use.The concentration of mineral acid is unrestricted, and preferably working concentration is the vitriol oil more than 60%, and more preferably working concentration is the vitriol oil more than 98%.
If soaking time is less than 60 minutes, then vanadium hydrolytic precipitation rate is lower than 99.5%; If soaking time more than 90 minutes, is then carried the foreign matter content height secretly, and filtration difficulty.
Subsequently, can reaction mixture, filter, wash, obtain many vanadic acid sodiums solid.Filter the filtrate of above-mentioned reaction mixture gained and the washing lotion of washing leaching cake gained and can obtain mineral acid through electrodialysis process, this mineral acid can be through concentrating or without the pH value that is used to regulate sodium vanadium extraction leach liquor after concentrating, having realized the recycle of mineral acid.
Then, add sodium hydroxide solution, and stir the solidliquid mixture of gained, make that the pH value of solution is 8～8.5 in the solidliquid mixture, afterwards solidliquid mixture is heated to 90 ℃ to seething with excitement to many vanadic acid sodiums solid of gained.For example, can add mass concentration to many vanadic acid sodiums solid of gained gradually and be 40%～50% sodium hydroxide solution, fully stir the solidliquid mixture and the real-time pH value of measuring solution of gained, make that the pH value of solution is 8～8.5 in the solidliquid mixture, afterwards solidliquid mixture is heated to 90 ℃ to boiling.
In this process, many vanadic acid root is transformed into metavanadic acid root (V along with the increase of solution alkalescence
3O
9 3-Or V
4O
12 4-, claim VO again
3 -), promptly generate white or flaxen sodium metavanadate.Solidliquid mixture being heated to 90 ℃ to the boiling, solidliquid mixture can be remained on 90 ℃ to boiling state, till the white that occurs or faint yellow solid no longer increase, for example with reactant insulation 60～120 minutes.Can add sodium hydroxide solution in the process of insulation, make that the pH value of solution is 8～8.5, carry out more fully to guarantee reaction.Can reaction stirred in the insulating process, to promote the carrying out of reaction.
As mentioned above, many vanadic acid root is transformed into the metavanadic acid root along with the increase of solution alkalescence.If, then there are part ten vanadic acid roots less than 8 in the pH value in the solution, the transformation efficiency that promptly generates the metavanadic acid root reduces; If the pH value is greater than 8.5, then many vanadic acid root easily generates V
2O
7 4-, the transformation efficiency that promptly generates the metavanadic acid root also reduces.
Afterwards, reaction mixture can be cooled off, filters, washing, dry cake obtain the sodium metavanadate solid.Filter the filtrate of above-mentioned reaction mixture gained and the washing lotion of washing leaching cake gained and can obtain sodium hydroxide solution through electrodialysis process, this sodium hydroxide solution can be through concentrating or without many vanadic acid sodiums of the art breading solid that is used for after concentrating according to as above, having realized the recycle of sodium hydroxide solution.
The NaVO of the dry sodium metavanadate product of prepared according to the methods of the invention
3Content can be more than 99%.Below in conjunction with embodiment the method for preparing sodium metavanadate of the present invention is described in detail.
Embodiment 1
Get 500mL sodium vanadium extraction leach liquor (V
5+Concentration is 29.23g/L, Na
+Concentration is 16.2g/L, Cr
6+Concentration is 1.1g/L, the Si concentration of element is 0.7g/L, the P concentration of element is 0.01g/L), being 98% the vitriol oil with concentration is adjusted to 1.1 with the pH value of sodium vanadium extraction leach liquor, is heated to 90 ℃ then, fully stirs, adding concentration between soak and be 98% the vitriol oil makes the pH value remain on 1.1, at 90 ℃ of solids (many vanadic acid sodiums) that keep 60 minutes after-filtration to go out the hydrolysis gained, washing obtains many vanadic acid sodiums xln fast.Many vanadic acid sodiums xln of gained is placed reactor, to add concentration gradually be 40% sodium hydroxide solution and fully stir to it, make in the solidliquid mixture that the pH value of solution is 8 (in the process that adds sodium hydroxide solution gradually, the pH value of solution constantly rises in the solidliquid mixture), be heated to 90 ℃ and kept 60 minutes then under agitation condition, continuing to add concentration between soak and be 40% sodium hydroxide solution, to keep the pH value of solution in the solidliquid mixture be 8.Be incubated after 60 minutes, the white solid of generation no longer increases, and shows that reaction is complete.Stop heating, reaction mixture is cooled to room temperature under agitation condition, filter, washing, dry cake obtain the sodium metavanadate product.NaVO in the sodium metavanadate product
3Content be 99.7%, the V element yield is 95%.
Comparative Examples 1
Except being 98% the vitriol oil with concentration the pH value of sodium vanadium extraction leach liquor is adjusted to 1.1, adopts identical sodium vanadium extraction leach liquor to prepare the sodium metavanadate solid according to the method identical with method among the embodiment 1.NaVO in this sodium metavanadate product
3Content be 99.7%, the V element yield is 48%.
Comparative Examples 2
Except sodium vanadium extraction leach liquor is kept down 50 minutes at 90 ℃, adopt identical sodium vanadium extraction leach liquor to prepare the sodium metavanadate solid according to the method identical with method among the embodiment 1.The NaVO of this sodium metavanadate product
3Content be 99.7%, the V element yield is 76%.
Embodiment 2
Get 500mL sodium vanadium extraction leach liquor (V
5+Concentration is 21.5g/L, Na
+Concentration is 18.9g/L, Cr
6+Concentration is 1.34g/L, the Si concentration of element is 0.78g/L, the P concentration of element is 0.04g/L), being 98% the vitriol oil with concentration is adjusted to 1.3 with the pH value of sodium vanadium extraction leach liquor, is heated to 95 ℃ then, fully stirs, adding concentration between soak and be 98% the vitriol oil makes the pH value remain on 1.3, at 95 ℃ of solids (many vanadic acid sodiums) that keep 70 minutes after-filtration to go out the hydrolysis gained, washing obtains many vanadic acid sodiums xln fast.Many vanadic acid sodiums xln of gained is placed reactor, to add concentration gradually be 50% sodium hydroxide solution and fully stir to it, make in the solidliquid mixture that the pH value of solution is 8 (in the process that adds sodium hydroxide solution gradually, the pH value of solution constantly rises in the solidliquid mixture), be heated to 97 ℃ and kept 90 minutes then under agitation condition, continuing to add concentration between soak and be 50% sodium hydroxide solution, to keep the pH value of solution in the solidliquid mixture be 8.Be incubated after 90 minutes, the white solid of generation no longer increases, and shows that reaction is complete.Stop heating, reaction mixture is cooled to room temperature under agitation condition, filter, washing, dry cake obtain the sodium metavanadate product.NaVO in the sodium metavanadate product
3Content be 99.6%, the V element yield is 91%.
Embodiment 3
Get 500mL sodium vanadium extraction leach liquor (V
5+Concentration is 25.47g/L, Na
+Concentration is 19.4g/L, Cr
6+Concentration is 1.43g/L, the Si concentration of element is 0.92g/L, the P concentration of element is 0.02g/L), being 98% the vitriol oil with concentration is adjusted to 1.6 with the pH value of sodium vanadium extraction leach liquor, is heated to boiling state then, fully stirs, adding concentration between boiling period and be 98% the vitriol oil makes the pH value remain on 1.6, keep 80 minutes after-filtration to go out the solid (many vanadic acid sodiums) of hydrolysis gained under boiling state, washing obtains many vanadic acid sodiums xln fast.Many vanadic acid sodiums xln of gained is placed reactor, to add concentration gradually be 45% sodium hydroxide solution and fully stir to it, make in the solidliquid mixture that the pH value of solution is 8.5 (in the process that adds sodium hydroxide solution gradually, the pH value of solution constantly rises in the solidliquid mixture), be heated to boiling state then and kept 120 minutes under agitation condition, continuing to add concentration between soak and be 45% sodium hydroxide solution, to keep the pH value of solution in the solidliquid mixture be 8.5.Be incubated after 120 minutes, the white solid of generation no longer increases, and shows that reaction is complete.Stop heating, reaction mixture is cooled to room temperature under agitation condition, filter, washing, dry cake obtain the sodium metavanadate product.NaVO in the sodium metavanadate product
3Content be 99.6%, the V element yield is 93%.
Comparative Examples 3
Except being 98% the vitriol oil with concentration the pH value of sodium vanadium extraction leach liquor is adjusted to 1.7, adopts identical sodium vanadium extraction leach liquor to prepare the sodium metavanadate solid according to the method identical with method among the embodiment 3.NaVO in this sodium metavanadate product
3Content be 99.6%, the V element yield is 70%.
Embodiment 4
Get 500mL sodium vanadium extraction leach liquor (V
5+Concentration is 25.47g/L, Na
+Concentration is 18.7g/L, Cr
6+Concentration is 1.22g/L, the Si concentration of element is 0.52g/L, the P concentration of element is 0.03g/L), being 98% the vitriol oil with concentration is adjusted to 1.4 with the pH value of sodium vanadium extraction leach liquor, is heated to boiling state then, fully stirs, adding concentration between boiling period and be 98% the vitriol oil makes the pH value remain on 1.4, keep 90 minutes after-filtration to go out the solid (many vanadic acid sodiums) of hydrolysis gained under boiling state, washing obtains many vanadic acid sodiums xln fast.Many vanadic acid sodiums xln of gained is placed reactor, to add concentration gradually be 50% sodium hydroxide solution and fully stir to it, make in the solidliquid mixture that the pH value of solution is 8.3 (in the process that adds sodium hydroxide solution gradually, the pH value of solution constantly rises in the solidliquid mixture), be heated to boiling state then and kept 120 minutes under agitation condition, continuing to add concentration between soak and be 50% sodium hydroxide solution, to keep the pH value of solution in the solidliquid mixture be 8.3.Be incubated after 120 minutes, the white solid of generation no longer increases, and shows that reaction is complete.Stop heating, reaction mixture is cooled to room temperature under agitation condition, filter, washing, dry cake obtain the sodium metavanadate product.NaVO in the sodium metavanadate product
3Content be 99.5%, the V element yield is 94%.
Comparative Examples 4
Except sodium vanadium extraction leach liquor was kept under the boiling state 95 minutes, adopt identical sodium vanadium extraction leach liquor to prepare the sodium metavanadate solid according to the method identical with method among the embodiment 4.The NaVO of this sodium metavanadate product
3Content be 97.4%, the V element yield is 94%.
Claims (10)
1. method for preparing sodium metavanadate said method comprising the steps of:
A. with mineral acid the pH value of sodium vanadium extraction leach liquor is adjusted to 1.1～1.6, is heated 90 ℃ then, kept 60～90 minutes, generate many vanadic acid sodiums solid to boiling;
B. add sodium hydroxide solution to many vanadic acid sodiums solid of gained, and stir the solidliquid mixture of gained, make that the pH value of the solution in the solidliquid mixture is 8～8.5;
C. solidliquid mixture is heated to 90 ℃ to boiling, generates the sodium metavanadate solid.
2. the method for preparing sodium metavanadate according to claim 1 is characterized in that sodium vanadium extraction leach liquor contains the V of 20～30g/L
5+, 15～20g/L Na
+, 1～1.5g/L Cr
6+, 0.5～1g/L the Si element and be less than the P element of 0.05g/L.
3. the method for preparing sodium metavanadate according to claim 1, it is characterized in that preparing sodium vanadium extraction leach liquor: to vanadium slag, bone coal with contain at least a at least a interpolation yellow soda ash in the vanadium solid waste, sodium-chlor, the sodium sulfate by following steps, the vanadium of multivalence attitude is converted into the sodium salt of water-soluble pentavalent vanadium by roasting, again product of roasting is carried out water logging, thereby obtain sodium vanadium extraction leach liquor.
4. the method for preparing sodium metavanadate according to claim 1, it is characterized in that step a also comprises: sodium vanadium extraction leach liquor is being remained on 90 ℃ to the process of boiling state, add mineral acid to sodium vanadium extraction leach liquor, make that the pH value of sodium vanadium extraction leach liquor is 1.1～1.6.
5. the method for preparing sodium metavanadate according to claim 1 is characterized in that described mineral acid is at least a in sulfuric acid, hydrochloric acid, the nitric acid.
6. the method for preparing sodium metavanadate according to claim 5 is characterized in that described mineral acid is that concentration is the sulfuric acid more than 98%.
7. the method for preparing sodium metavanadate according to claim 1, it is characterized in that comprising to the step that many vanadic acid sodiums solid of gained adds sodium hydroxide solution and stirs the solidliquid mixture of gained: adding mass concentration to many vanadic acid sodiums solid of gained is 40%～50% sodium hydroxide solution, and fully stirs the solidliquid mixture of gained.
8. the method for preparing sodium metavanadate according to claim 1, it is characterized in that step c also comprises: solidliquid mixture is heated to 90 ℃ to the boiling after, solidliquid mixture is remained on 90 ℃ to boiling, till the white that occurs or faint yellow solid no longer increase.
9. the method for preparing sodium metavanadate according to claim 8 is characterized in that solidliquid mixture was kept 60～120 minutes to boiling state at 90 ℃.
10. the method for preparing sodium metavanadate according to claim 8 is characterized in that adding sodium hydroxide solution solidliquid mixture being remained on 90 ℃ to the ebullient process to solidliquid mixture, makes that the pH value of the solution in the solidliquid mixture is 8～8.5.
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| CN102502570A (en) * | 2011-11-29 | 2012-06-20 | 芜湖人本合金有限责任公司 | Production method of medical sodium metavanadate |
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| CN104628033A (en) * | 2015-01-27 | 2015-05-20 | 河北钢铁股份有限公司承德分公司 | Method for preparing metavanadate |
| CN105110370A (en) * | 2015-08-19 | 2015-12-02 | 中国科学院上海硅酸盐研究所 | Metavanadate powder and preparation method therefor |
| CN105271406A (en) * | 2015-09-28 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Sodium metavanadate preparation method |
| CN107416900A (en) * | 2017-08-31 | 2017-12-01 | 攀钢集团钒业有限公司 | A kind of method for efficiently preparing high-purity sodium metavanadate |
| CN108588737A (en) * | 2018-05-09 | 2018-09-28 | 湖南钒谷新能源技术有限公司 | A method of processing vanadium-containing waste liquid prepares sodium metavanadate |
| CN109516499A (en) * | 2018-11-30 | 2019-03-26 | 攀钢集团研究院有限公司 | The method that high phosphorus solution containing vanadium produces vanadium oxide |
| CN109516499B (en) * | 2018-11-30 | 2021-04-27 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide from high-phosphorus vanadium-containing liquid |
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