CN103422111A - Preparing method for sodium metavanadate - Google Patents
Preparing method for sodium metavanadate Download PDFInfo
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- CN103422111A CN103422111A CN2012101495905A CN201210149590A CN103422111A CN 103422111 A CN103422111 A CN 103422111A CN 2012101495905 A CN2012101495905 A CN 2012101495905A CN 201210149590 A CN201210149590 A CN 201210149590A CN 103422111 A CN103422111 A CN 103422111A
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Abstract
The invention discloses a preparing method for sodium metavanadate. The preparing method comprises the steps: a sodium vanadate solution as an anode electrolyte solution undergoes ionic membrane electrolysis, a sodium metavanadate solution with a pH value of 7.0-8.0 and the molar ratio between sodium and vanadium being 0.95-1.05 according to sodium element and vanadium element is obtained at an anode under the ionic membrane electrolysis condition. According to the preparation method of sodium metavanadate, vanadium pentoxide does not need to be firstly prepared, sodium metavanadate can be directly prepared by the sodium vanadate solution, and thus the production steps are simplified; moreover, because sulfuric acid does not need to be employed to adjust the pH value and ammonium sulfate does not need to be employed to precipitate ammonium vanadate, vanadium precipitation wastewater containing sodium sulfate and ammonium sulfate is not produced, and thus the burden on the environment is reduced; and because the vanadium precipitation wastewater containing sodium sulfate and ammonium sulfate is not produced, the vanadium precipitation wastewater does not need to be processed, and thus the production cost is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of sodium metavanadate.
Background technology
Sodium metavanadate (NaVO
3) be the crystallization of colourless monocline prism-shaped, 630 ℃ of fusing points, can be water-soluble, do not fire, low toxicity.Be generally used for chemical fertilizer, coal gas desulfurization, photograph etc., also as mordant.
The preparation method of existing sodium metavanadate, usually first by containing vanadium minerals, preparing highly purified Vanadium Pentoxide in FLAKES, and then be dissolved in Vanadium Pentoxide in FLAKES in highly purified sodium hydroxide solution, through evaporation concentration, crystallization, obtains the sodium metavanadate product.The preparation process of Vanadium Pentoxide in FLAKES is: will obtain alkaline sodium vanadate solution through sodium roasting, water logging containing vanadium minerals; Alkaline sodium vanadate solution is carried out to purification and impurity removal and obtain alkaline vanadic acid sodium qualifying liquid; Add ammonium salt precipitation ammonium vanadate in alkaline vanadic acid sodium qualifying liquid after, ammonium vanadate is carried out to the oxidizing roasting decomposition and obtain high-purity vanadium pentoxide.In alkaline vanadic acid sodium qualifying liquid, precipitate in the process of ammonium vanadate, need to add the sulphur acid for adjusting pH value, then add the ammonium sulfate precipitation ammonium vanadate, precipitation obtains ammonium vanadate and vanadium wastewater, contain a small amount of vanadium in vanadium wastewater and reduced the rate of recovery of vanadium, and, owing to adopting sulphur acid for adjusting pH value and ammonium sulfate precipitation ammonium vanadate, make in vanadium wastewater and contain a large amount of sodium sulfate and ammonium sulfate, thereby increased the burden of environment, and increased the processing cost of vanadium wastewater.Therefore, existing technique exists that step is numerous and diverse, the vanadium loss is large, production cost is high, the wastewater treatment difficulty large, to distinct issues such as environment are unfriendly.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of new sodium metavanadate.The preparation method of sodium metavanadate provided by the invention, not only step is simple, cost is low, and environmentally friendly.
The present inventor is dexterously by carrying out electrolysis with ion-exchange film using sodium vanadate solution as anolyte, reduced the pH value in de-sodium, thereby obtained highly purified sodium metavanadate solution, and preferably the sodium metavanadate solution obtained is carried out to condensing crystal, thereby can access highly purified sodium metavanadate.
To achieve these goals, the invention provides a kind of preparation method of sodium metavanadate, wherein, the method comprises carries out electrolysis with ion-exchange film using sodium vanadate solution as anolyte, the condition of electrolysis with ion-exchange film makes to obtain the pH value for 7.0-8.0 at anode, and in sodium element and v element, the sodium metavanadate solution that the mol ratio of sodium and vanadium is 0.95-1.05.
Preparation method according to sodium metavanadate of the present invention, by sodium vanadate solution is directly carried out to electrolysis with ion-exchange film as anolyte, slough superfluous sodium ion by electrolysis with ion-exchange film, reach the pH value that the sodium ion for preparing sodium metavanadate required and reduced simultaneously solution, thereby, without first preparing Vanadium Pentoxide in FLAKES, just can directly by sodium vanadate solution, prepare sodium metavanadate, simplified production stage; And due to without adopting sulphur acid for adjusting pH value and ammonium sulfate precipitation ammonium vanadate, therefore do not produce the vanadium wastewater that contains sodium sulfate and ammonium sulfate, reduced the burden of environment; Owing to not producing the vanadium wastewater that contains sodium sulfate and ammonium sulfate, thereby without vanadium wastewater is processed, thereby production cost reduced.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only, for description and interpretation the present invention, is not limited to the present invention.
Preparation method according to sodium metavanadate of the present invention, the method comprises carries out electrolysis with ion-exchange film using sodium vanadate solution as anolyte, the condition of electrolysis with ion-exchange film makes to obtain the pH value for 7.0-8.0 at anode, and in sodium element and v element, the sodium metavanadate solution that the mol ratio of sodium and vanadium is 0.95-1.05.
In the present invention, to sodium vanadate solution, there is no particular limitation, so long as this area is usually used in preparing the sodium vanadate solution of sodium metavanadate, gets final product.For example, described sodium vanadate solution can be the solution that vanadium raw materials is obtained through sodium roasting, water logging.The method of the sodium vanadate solution that vanadium raw materials is obtained through sodium roasting, water logging can be carried out with reference to method well known to those skilled in the art.
According to the present invention, under preferable case, in v element, in described sodium vanadate solution, vanadium concentration is 20-35g/L; The pH value is 9-14; In sodium element and v element, the sodium in sodium vanadate solution and the mol ratio of vanadium are 1.5-2.5.More preferably, in v element, in described sodium vanadate solution, vanadium concentration is 25-35g/L; The pH value is 10.5-12; In sodium element and v element, the sodium in sodium vanadate solution and the mol ratio of vanadium are 1.5-1.8.
According to the present invention, the method comprises directly carries out electrolysis with ion-exchange film as anolyte using sodium vanadate solution, by electrolysis with ion-exchange film, sloughs superfluous sodium ion, reaches the pH value that the sodium ion for preparing sodium metavanadate required and reduced simultaneously solution.And the condition by electrolysis with ion-exchange film is controlled at the pH value of the sodium metavanadate solution that obtains in specific scope, and the mol ratio of the sodium in the sodium metavanadate solution obtained and vanadium is controlled in specific scope, thereby obtains highly purified sodium metavanadate.
In the present invention, it is 7.0-8.0 that the condition of described electrolysis with ion-exchange film makes the pH value of the sodium metavanadate solution that obtains at anode, and, in sodium element and v element, the mol ratio of sodium and vanadium is 0.95-1.05; In order further to improve the sodium metavanadate solution that obtains and the purity of sodium metavanadate, it is 7.0-7.5 that the condition of preferred described electrolysis with ion-exchange film makes the pH value of the sodium metavanadate solution that obtains at anode, and, in sodium element and v element, the mol ratio of sodium and vanadium is 0.98-1.02.
In the present invention, the selectable range of the condition of described electrolysis with ion-exchange film is wider.Under preferable case, the condition of described electrolysis with ion-exchange film comprises: voltage is 5-15V, and electric current is 0.01-1.5A, and electrolysis time is 2-8 hour; More preferably voltage is 10-15V, and electric current is 0.05-1.5A, and electrolysis time is 3-6 hour.
In addition, in described electrolysis with ion-exchange film, preferably catholyte is water or sodium hydroxide solution; Water more preferably.In the present invention, in electrolytic process, sodium ion sees through cationic exchange membrane and moves to cathode compartment, enter the hydroxide ion that the sodium ion of catholyte produces together with negative electrode By Electrolysis water and generate sodium hydroxide, therefore can directly recycle as catholyte of the present invention without any processing.
According to the present invention, the cationic exchange membrane in described electrolysis with ion-exchange film can be this area various ion-exchange membranees commonly used.Such as this ion-exchange membrane, it can be the film made from the anionic functional groups' such as sulfonic group and/or carboxylic acid group (per) fluoropolymer on side chain, the perfluorinated sulfonic acid that perhaps can strengthen for poly-fluorohydrocarbon fabric-perfluorocarboxylic acid composite membrane, and described ion-exchange membrane can be by commercially available.
According to the present invention, described electrolysis with ion-exchange film can be carried out in ion-membrane electrolysis device known in the art, and for example, described ion-membrane electrolysis device generally includes anolyte compartment and the cathode compartment separated by dividing plate; Described anolyte compartment for example can be on the titanium support mesh at the titanium dish, and one deck anode of burn-oning forms anolyte compartment's (by thin, thick shape net and titanium plate, forming anolyte compartment), and the material of anode can be titanium, is mesh-like; Described cathode compartment for example can for the nickel dish the nickel support mesh on, cover the Elasticity Ni that one deck is woven into by nickel wire, on Elasticity Ni, tiling one deck active nickel negative electrode, form cathode compartment (by thick, soft, thin three kinds of cathode compartments that nickel screen forms), the material of negative electrode is nickel, the elasticity nickel screen, consists of.
According to the present invention, under preferable case, the method also comprises carries out condensing crystal by the sodium metavanadate solution obtained, and obtains sodium metavanadate.The method of described condensing crystal and condition are well known in the art.For example, sodium metavanadate solution can be concentrated under 40-95 ℃, be concentrated into that crystal occurs or during 0.1-0.5 times of original solution, temperature dropped to below 40 ℃ and carries out decrease temperature crystalline, also can, after temperature being dropped to below 40 ℃, by standing or stirring, further carry out crystallization.Crystallization obtains sodium metavanadate solid and filtrate by solid-liquid separation.The method of solid-liquid separation is well known in the art, such as filtering, centrifugal etc.
In addition, in the present invention, in order further to reduce costs, above-mentioned filtrate directly can also be returned to leaching system (while by vanadium raw materials, preparing sodium vanadate solution) recycle.And what generate at negative electrode after electrolysis is sodium hydroxide, can directly recycle as catholyte of the present invention without any processing.
Below will describe the present invention by embodiment.
Sodium vanadate solution in following examples: carry out water logging vanadium extraction after sodium roasting according to the method described in " external vanadium metallurgy " (metallurgical industry press publishes 121 pages in 1985), obtain sodium vanadate solution.
In following examples, the contents on dry basis of sodium metavanadate adopts following measuring method to be measured.
(1) by the sodium metavanadate solid drying that obtains in embodiment to constant weight, as specimen;
(2) with the sodium content in the Atomic Absorption Spectrometry sample;
(3) method of the content of vanadium in working sample is: accurately take specimen 0.25g, add 50ml water, slowly inject 10ml sulfuric acid, heating for dissolving, cooling, add 4 0.1% phenylanthranilic acid ethanolic solns, be titrated to solution with 0.1mol/L ferrous ammonium sulphate standardized solution and become bright green by red-purple.Volume and the concentration of the l ferrous ammonium sulfate solution of then using according to titration are calculated content of vanadium.
(4) calculate the amount of sodium metavanadate in sample according to sodium vanadium mol ratio 1:1;
(5) contents on dry basis of the weight calculating sodium metavanadate of dried sodium metavanadate solid in the amount by sodium metavanadate in sample and step (1).
Embodiment 1
The present embodiment is for illustrating the preparation of sodium metavanadate
At ion-membrane electrolysis device, (be purchased from Di Nuola electrode (Suzhou) company limited, ion-exchange membrane is Nafion117, and anode is the titanium net, and negative electrode is nickel screen; Below identical) in anolyte compartment add sodium vanadate solution (in v element, in sodium vanadate solution, the concentration of vanadium be 30g/L; In sodium element and v element, sodium vanadium mol ratio is 1.5; PH is 12) 500mL, negative electrode adds the water of same volume, and voltage control is at 12V, and the connection galvanic current is 0.05A, electrolysis 3 hours, obtaining pH is 7.2, and in sodium element and v element, the sodium metavanadate solution that sodium vanadium mol ratio is 0.99.After under 80 ℃, the sodium metavanadate solution decompression being concentrated to 100ml, more under agitation be cooled to 25 ℃ of crystallize outs, and filtration obtains the sodium metavanadate solid.The contents on dry basis of the sodium metavanadate obtained is 98.6 % by weight.
Embodiment 2
The present embodiment is for illustrating the preparation of sodium metavanadate
Anolyte compartment in ion-membrane electrolysis device adds sodium vanadate solution, and (in v element, in sodium vanadate solution, the concentration of vanadium is 35g/L; In sodium element and v element, sodium vanadium mol ratio is 1.8; PH is 11) 500mL, negative electrode adds the water of same volume, and voltage control is at 15V, and the connection galvanic current is 1.2A, electrolysis 4 hours, obtaining pH is 7.5, and in sodium element and v element, the sodium metavanadate solution that sodium vanadium mol ratio is 0.98.After under 80 ℃, the sodium metavanadate solution decompression being concentrated to 100ml, more under agitation be cooled to 25 ℃ of crystallize outs, and filtration obtains the sodium metavanadate solid.The contents on dry basis of the sodium metavanadate obtained is 98.3 % by weight.
Embodiment 3
The present embodiment is for illustrating the preparation of sodium metavanadate
Anolyte compartment in ion-membrane electrolysis device adds sodium vanadate solution, and (in v element, in sodium vanadate solution, the concentration of vanadium is 25g/L; In sodium element and v element, sodium vanadium mol ratio is 1.6; PH is 10.5) 500mL, negative electrode adds the water of same volume, and voltage control is at 15V, and the connection galvanic current is 1.5A, electrolysis 6 hours, obtaining pH is 7.0, and in sodium element and v element, the sodium metavanadate solution that sodium vanadium mol ratio is 1.02.After under 80 ℃, the sodium metavanadate solution decompression being concentrated to 100ml, more under agitation be cooled to 25 ℃ of crystallize outs, and filtration obtains the sodium metavanadate solid.The contents on dry basis of the sodium metavanadate obtained is 98.7 % by weight.
Embodiment 4
The present embodiment is for illustrating the preparation of sodium metavanadate
Method according to embodiment 3 is carried out, and different is the sodium hydroxide solution that negative electrode adds 10 % by weight of same volume, and voltage control is at 12V, the connection galvanic current is 1.2A, electrolysis 6 hours, and obtaining pH is 8.0, and in sodium element and v element, the sodium metavanadate solution that sodium vanadium mol ratio is 1.05.After under 80 ℃, the sodium metavanadate solution decompression being concentrated to 100ml, more under agitation be cooled to 25 ℃ of crystallize outs, and filtration obtains the sodium metavanadate solid.The contents on dry basis of the sodium metavanadate obtained is 98.1 % by weight.
Known by embodiment 1-4, adopt electrolysis with ion-exchange film can slough superfluous sodium ion, reach the pH value that the sodium ion for preparing sodium metavanadate required and can reduce simultaneously solution.And, control the pH value of the sodium metavanadate solution obtained by the condition of electrolysis with ion-exchange film in specific scope, and the mol ratio of controlling sodium in the sodium metavanadate solution obtain and vanadium can access the highly purified sodium metavanadate of contents on dry basis more than 98 % by weight in specific scope.
In addition, known by embodiment 1-4, adopt method of the present invention directly sodium vanadate solution to be carried out to electrolysis as anolyte and obtain sodium metavanadate, therefore without first preparing Vanadium Pentoxide in FLAKES, just can directly by sodium vanadate solution, prepare sodium metavanadate, simplify production stage; In addition, due to without adopting sulphur acid for adjusting pH value and ammonium sulfate precipitation ammonium vanadate, therefore do not produce the vanadium wastewater that contains sodium sulfate and ammonium sulfate, reduced the burden of environment; Owing to not producing the vanadium wastewater that contains sodium sulfate and ammonium sulfate, thereby without vanadium wastewater is processed, thereby production cost reduced.
Claims (8)
1. the preparation method of a sodium metavanadate, it is characterized in that, the method comprises carries out electrolysis with ion-exchange film using sodium vanadate solution as anolyte, the condition of electrolysis with ion-exchange film makes to obtain the pH value for 7.0-8.0 at anode, and in sodium element and v element, the sodium metavanadate solution that the mol ratio of sodium and vanadium is 0.95-1.05.
2. method according to claim 1, wherein, it is 7.0-7.5 that the condition of described electrolysis with ion-exchange film makes the pH value of the sodium metavanadate solution that obtains at anode, and, in sodium element and v element, the mol ratio of sodium and vanadium is 0.98-1.02.
3. method according to claim 1 and 2, wherein, the condition of described electrolysis with ion-exchange film comprises: voltage is 5-15V, and electric current is 0.01-1.5A, and electrolysis time is 2-8 hour.
4. method according to claim 3, wherein, the condition of described electrolysis with ion-exchange film comprises: voltage is 12-15V, and electric current is 0.05-1.5A, and electrolysis time is 3-6 hour.
5. method according to claim 1 and 2, wherein, the condition of described electrolysis with ion-exchange film also comprises: catholyte is water or sodium hydroxide solution.
6. method according to claim 1 and 2, wherein, the solution of described sodium vanadate solution for vanadium raw materials is obtained through sodium roasting, water logging.
7. method according to claim 6, wherein, in v element, in described sodium vanadate solution, vanadium concentration is 20-35g/L; The pH value is 9-14; In sodium element and v element, the sodium in sodium vanadate solution and the mol ratio of vanadium are 1.5-2.5.
8. method according to claim 1, wherein, the method also comprises carries out condensing crystal by the sodium metavanadate solution obtained, and obtains sodium metavanadate.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694748A (en) * | 2015-02-04 | 2015-06-10 | 河北钢铁股份有限公司承德分公司 | Method for removing sodium or potassium by electrodialysis in vanadium-containing solution |
| CN107128973A (en) * | 2017-05-24 | 2017-09-05 | 中国科学院过程工程研究所 | A kind of method that ammonium metavanadate is prepared by sodium vanadate |
| CN108928851A (en) * | 2017-05-24 | 2018-12-04 | 中国科学院过程工程研究所 | A method of ammonium vanadate sodium is prepared by sodium vanadate solution |
| CN113087017A (en) * | 2021-04-06 | 2021-07-09 | 中国科学院理化技术研究所 | Sodium metavanadate nanosphere and preparation method and application thereof |
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| SU1691424A1 (en) * | 1988-07-26 | 1991-11-15 | Дагестанский Государственный Университет Им.В.И.Ленина | Method for obtaining vanadium oxide(v) |
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| US20070039473A1 (en) * | 2005-08-19 | 2007-02-22 | Gholam-Abbas Nazri | Guest-host hydrogen storage material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694748A (en) * | 2015-02-04 | 2015-06-10 | 河北钢铁股份有限公司承德分公司 | Method for removing sodium or potassium by electrodialysis in vanadium-containing solution |
| CN107128973A (en) * | 2017-05-24 | 2017-09-05 | 中国科学院过程工程研究所 | A kind of method that ammonium metavanadate is prepared by sodium vanadate |
| CN108928851A (en) * | 2017-05-24 | 2018-12-04 | 中国科学院过程工程研究所 | A method of ammonium vanadate sodium is prepared by sodium vanadate solution |
| CN108928851B (en) * | 2017-05-24 | 2021-08-03 | 中国科学院过程工程研究所 | Method for preparing sodium ammonium vanadate from sodium vanadate solution |
| CN107128973B (en) * | 2017-05-24 | 2021-11-09 | 中国科学院过程工程研究所 | Method for preparing ammonium metavanadate from sodium vanadate |
| CN113087017A (en) * | 2021-04-06 | 2021-07-09 | 中国科学院理化技术研究所 | Sodium metavanadate nanosphere and preparation method and application thereof |
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