CN101746822A - Method for extracting sodium metavanadate from vanadium extraction leaching solution - Google Patents
Method for extracting sodium metavanadate from vanadium extraction leaching solution Download PDFInfo
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- CN101746822A CN101746822A CN200910215723A CN200910215723A CN101746822A CN 101746822 A CN101746822 A CN 101746822A CN 200910215723 A CN200910215723 A CN 200910215723A CN 200910215723 A CN200910215723 A CN 200910215723A CN 101746822 A CN101746822 A CN 101746822A
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Abstract
The invention discloses a method for extracting sodium metavanadate from a vanadium extraction leaching solution, comprising the following steps of: adjusting the pH value of the sodium-ionized vanadium extraction leaching solution to 4-4.5 by using inorganic acid, then heating the solution to the temperature of 75-85 DEG C, then adding a soluble ammonium salt into the solution according to the mass ratio of NH4+:V=1.5-2, fully and uniformly stirring, and obtaining sodium polyvanadate containing ammonium after the reaction is finished; putting the obtained sodium polyvanadate containing ammonium into a sealed reactor, adding sodium hydroxide according to the mol ratio of Na:V=0.8-0.9, stirring at the temperature ranging from 90 DEG C to the boiling temperature till the solution starts to precipitate a white or light yellow solid, cooling the solution to the room temperature under the condition of stirring, filtering and drying to obtain a sodium metavanadate solid.
Description
Technical field
The present invention relates to a kind of method of producing sodium metavanadate from the vanadium extraction leach liquor.
Background technology
Sodium metavanadate is of many uses on chemical industry, can be used as chemical reagent, catalyzer, siccative, mordant, makes ammonium vanadate and potassium metavanadate, also can be used for medical treatment photograph, plant inoculation and inhibitor etc.
At present, preparing sodium metavanadate both at home and abroad mainly is to extract from the sodium roasting leach liquor that contains vanadium, and main method has three kinds: a kind of method is utilized vanadium extraction leach liquor evaporating, concentrating and crystallizing method; Second kind is to utilize vanadium extraction leach liquor precipitation ammonium poly-vanadate earlier, uses the sodium hydroxide solution dissolution method then; The third is to dissolve V with sodium hydroxide solution
2O
5Method.
The evaporating, concentrating and crystallizing method is exactly that the vanadium extraction leach liquor that will leach gained obtains the sodium metavanadate solid through carrying out evaporating, concentrating and crystallizing after the removal of impurity, this method technology is simple, easy to operate, but leach liquor complicated component, Impurity removal is incomplete, cause product purity not high, be difficult to be used widely.Ammonium poly-vanadate solid alkali solution technique will contain vanadium leachate exactly and add ammonium salt precipitation and obtain ammonium poly-vanadate, require precipitation temperature about 90-95 ℃, adding sodium hydrate solid then returns molten, obtain the sodium metavanadate solid, the shortcoming of this method is that the pH value is adjusted to 2-2.5 in the precipitation ammonium poly-vanadate process, consumes a large amount of acid, returning at hydro-oxidation sodium then needs in the molten process to add and the sodium hydroxide of vanadium with equimolar amount, quantity of alkali consumption is big, so production cost is higher, and reaction principle is (NH
4)
2V
6O
16+ 6NaOH=6NaVO
3+ 2NH
3↑+4H
2O; Ammonium poly-vanadate presents cotton-shaped or polycrystalline aggregate usually, contains the difficult washings of impurity such as sodium sulfate, causes product purity not high.The third method is to dissolve V with sodium hydroxide solution
2O
5Method, heating fully obtains sodium metavanadate after the reaction, and this method is easy to operate, and the product purity height has solved the generation of polluting the waste gas ammonia, and this method 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, and reaction principle is V
2O
5+ 2NaOH=2NaVO
3+ H
2O.
Summary of the invention
At prior art in the problem that preparation exists during sodium metavanadate, the invention provides a kind of less energy consumption, low in the pollution of the environment, the acid and alkali consumption amount is little, cost is low, product purity is high, and the preparation method of the high sodium metavanadate of vanadium recovery.
The invention provides a kind of method for preparing sodium metavanadate, this method may further comprise the steps: with mineral acid the pH value of sodium vanadium extraction leach liquor is adjusted to 4-4.5, and is heated 75 ℃-85 ℃, then according to NH
4 +: the mass ratio of V=1.5-2 adds the solubility ammonium salt in solution, stir, and obtains containing many vanadic acid sodiums of ammonium solid after the reaction; Gained is contained many vanadic acid sodiums of ammonium solid place sealed reactor, mol ratio according to Na: V=0.8-0.9 adds sodium hydroxide solution, stir to the condition of boiling temperature at 90 ℃, in solution, begin white to occur or faint yellow solid is separated out, then solution is cooled to room temperature under agitation condition, filter, drying, thus obtain the sodium metavanadate solid.
Description of drawings
Fig. 1 shows the schema of producing the method for sodium metavanadate according to of the present invention from the vanadium extraction leach liquor.
Embodiment
The invention provides a kind of method of producing sodium metavanadate from the vanadium extraction leach liquor, this method may further comprise the steps:
(1) with mineral acid with sodium vanadium extraction leach liquor ([V
5+]: 20-30g/L, [Na
+]: 15-20g/L, [Cr
6+]: 1-1.5g/L, [Si]: 0.5-1g/L, the pH value of P＜0.05g/L) is adjusted to 4-4.5, is heated to 75 ℃-85 ℃ then, then according to NH
4 +: the mass ratio of V=1.5-2 adds the solubility ammonium salt in solution, stir, and reacts to obtain containing many vanadic acid sodiums of ammonium solid after 30-50 minute.Reaction principle is:
V
10O
28 6-+4NH
4 ++2Na
++10H
2O＝(NH
4)
4Na
2V
10O
28.10H
2O↓
(2) gained is contained many vanadic acid sodiums of ammonium solid and place sealed reactor, mol ratio according to Na: V=0.8-0.9 adds sodium hydroxide solution, stir to the condition of boiling temperature at 90 ℃, in solution, begin white to occur or faint yellow solid is separated out, then solution is cooled to room temperature under agitation condition, filters drying, can obtain the sodium metavanadate solid, sodium metavanadate content is more than 99%.Mother liquor of precipitation of ammonium is returned and is contained the use of many vanadic acid sodiums of ammonium precipitation process.The ammonia that produces in the reaction process adopts the vitriol oil to absorb, and the ammonium sulfate that obtains returns precipitation and contains ammonium ammonium poly-vanadate sodium operation and recycle.Reaction principle is:
(NH
4)
4Na
2V
10O
28.10H
2O+8NaOH＝10NaVO
3+4NH
3↑+16H
2O
2NH
3+H
2SO
4＝(NH
4)
2SO
4
In the method for preparing sodium metavanadate according to the present invention, what described mineral acid can be in sulfuric acid, hydrochloric acid, the nitric acid is at least a; Described solubility ammonium salt can be in ammonium sulfate, ammonium chloride, the ammonium nitrate at least a.
According to the method for preparing sodium metavanadate of the present invention, in step (1), to contain many vanadic acid sodiums of ammonium temperature be 75 ℃-85 ℃ to precipitation, and when precipitation temperature during greater than 85 ℃, part contains the many vanadic acid sodiums of ammonium and is converted into ammonium poly-vanadate in the throw out, causes Na in the precipitated product
+Parcel sulfur impurity content rises in content reduction and the product, and when precipitation temperature was lower than 75 ℃, sedimentation time then prolonged.
According to the method for preparing sodium metavanadate of the present invention, in step (1), the pH value that precipitation contains the many vanadic acid sodiums of ammonium is 4-4.5.When the pH value was lower than 4, precipitated product was converted into ammonium poly-vanadate, and then sulfur impurity content increases in the throw out, and sodium hydroxide consumption increases in the subsequent step.When pH greater than 4.5 the time, the yield of vanadium descends.
According to the method for preparing sodium metavanadate of the present invention, in step (1), the amount that adds ammonium is according to NH
4 +: the mass ratio of V=1.5-2 adds.Work as NH
4 +: V＜1.5 o'clock, the vanadium deposition rate is less than 95%; NH
4 +: V＞2 o'clock, vanadium deposition rate increase rate is little, causes the waste of ammonium salt.
According to the method for preparing sodium metavanadate of the present invention, in step (1), sedimentation time is 30 minutes to 50 minutes.When sedimentation time was less than 30 minutes, precipitation not exclusively; When sedimentation time in the time of unnecessary 50 minutes, deposition rate is not obvious after 50 minutes, prolongs sedimentation time and causes production efficiency to reduce and increase energy consumption.
According to the method for preparing sodium metavanadate of the present invention, in step (2), dissolution of sodium hydroxide contain many vanadic acid sodiums of ammonium temperature be 90 ℃ to boiling temperature.The temperature height helps the volatilization of ammonia, helps improving product purity; The simultaneous temperature height helps the volatilization of moisture, and the crystallization that helps sodium metavanadate is separated out.
According to the method for preparing sodium metavanadate of the present invention, in step (2), absorb ammonia with the vitriol oil, gained ammonium sulfate returns precipitation and contains the many vanadic acid sodiums uses of ammonium; Mother liquor behind the crystallization sodium metavanadate returns precipitation and contains the use of many vanadic acid sodiums of ammonium process, realizes the recycle of whole process of production material, and no waste water, waste gas and waste residue produce, and realize cleaning production.
Further describe the present invention below in conjunction with accompanying drawing and concrete example.
Embodiment 1
Get the sodium roasting leach liquor (vanadium concentration is 29.23g/L) of 500mL, the pH value of solution value is adjusted to 4.2, solution is heated to 75 ℃, according to NH with the vitriol oil
4 +: the mass ratio of V=1.5 adds (NH in solution
4)
2SO
4Solid fully stirs, and react after 50 minutes the gained solid filtering, washs fast and obtains containing the crystallization of many vanadic acid sodiums of ammonium.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.8 drops into the 100mL sodium hydroxide solution, under 90 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 33.3g, product purity is 99.6%, and the rate of recovery is 95%.
Embodiment 2
Get the sodium roasting leach liquor (vanadium concentration is 21.5g/L) of 500mL, the pH value of solution value is adjusted to 4.5, solution is heated to 80 ℃, according to NH with concentrated hydrochloric acid
4 +: the mass ratio of V=1.8 adds NH in solution
4The Cl solid fully stirs, and react after 30 minutes the gained solid filtering, washs fast and obtains containing the crystallization of many vanadic acid sodiums of ammonium.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.8 drops into the 50mL sodium hydroxide solution, under 92 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 23.3g, product purity is 99.5%, and yield is 90%.
Embodiment 3
Get the sodium roasting leach liquor (vanadium concentration is 25.47g/L) of 500mL, the pH value of solution value is adjusted to 4.0, solution is heated to 82 ℃, according to NH with concentrated nitric acid
4 +: the mass ratio of V=2 adds NH in solution
4NO
3Solid fully stirs, and react after 40 minutes the gained solid filtering, washs fast and obtains containing the crystallization of many vanadic acid sodiums of ammonium.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.9 drops into the 150mL sodium hydroxide solution, under 94 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 28.5g, product purity is 99.4%, and yield is 93%.
Embodiment 4
Get the sodium roasting leach liquor (vanadium concentration is 29.23g/L) of 500mL, the pH value of solution value is adjusted to 4.4, solution is heated to 85 ℃, according to NH with the vitriol oil
4 +: the mass ratio of V=1.5 adds (NH in solution
4)
2SO
4Solid fully stirs, and react after 50 minutes the gained solid filtering, washs fast and obtains containing many vanadic acid sodiums of ammonium mixture.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.85 drops into the 100mL sodium hydroxide solution, under 95 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 33.3g, product purity is 99.7%, and yield is 95%.
The comparative example 1
Get the sodium roasting leach liquor (vanadium concentration is 29.23g/L) of 500mL, the pH value of solution value is adjusted to 4.2, solution is heated to 70 ℃, according to NH with the vitriol oil
4 +: the mass ratio of V=1.5 adds (NH in solution
4)
2SO
4Solid fully stirs, if reaction after 50 minutes with the gained solid filtering, washing obtains containing the crystallization of many vanadic acid sodiums of ammonium fast.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.8 drops into the 100mL sodium hydroxide solution, under 90 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 26.6g, product purity is 99.6%, and yield is 76%; If with the gained solid filtering, washing obtains containing the crystallization of many vanadic acid sodiums of ammonium fast after 110 minutes in reaction.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.8 drops into the 100mL sodium hydroxide solution, under 90 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 33.3g, product purity is 99.6%, and yield is 95%.
The comparative example 2
Get the sodium roasting leach liquor (vanadium concentration is 21.5g/L) of 500mL, the pH value of solution value is adjusted to 4.7, solution is heated to 80 ℃, according to NH with concentrated hydrochloric acid
4 +: the mass ratio of V=1.8 adds NH in solution
4The Cl solid fully stirs, and react after 30 minutes the gained solid filtering, washs fast and obtains containing the crystallization of many vanadic acid sodiums of ammonium.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.8 drops into the 50mL sodium hydroxide solution, under 92 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 17.3g, product purity is 99.5%, and yield is 67%.
The comparative example 3
Get the sodium roasting leach liquor (vanadium concentration is 25.47g/L) of 500mL, the pH value of solution value is adjusted to 3.8, solution is heated to 82 ℃, according to NH with concentrated nitric acid
4 +: the mass ratio of V=2 adds NH in solution
4NO
3Solid fully stirs, and react after 40 minutes the gained solid filtering, washs fast and obtains containing the crystallization of many vanadic acid sodiums of ammonium.Gained is contained the many vanadic acid sodiums of ammonium place sealed reactor, mol ratio according to Na: V=0.9 drops into the 150mL sodium hydroxide solution, under 94 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 30.6g, product purity is 92.7%, and yield is 93%.
The comparative example 4
Get the sodium roasting leach liquor (vanadium concentration is 29.23g/L) of 500mL, the pH value of solution value is adjusted to 4.4, solution is heated to 90 ℃, according to NH with the vitriol oil
4 +: the mass ratio of V=1.5 adds (NH in solution
4)
2SO
4Solid fully stirs, and react after 50 minutes the gained solid filtering, washs the mixture that obtains containing many vanadic acid sodiums of ammonium and ammonium poly-vanadate fast.The mixture that gained is contained many vanadic acid sodiums of ammonium and ammonium poly-vanadate places sealed reactor, mol ratio according to Na: V=0.85 drops into the 100mL sodium hydroxide solution, under 95 ℃ of conditions, stir, in solution, begin white solid to occur and separate out, then solution is cooled to room temperature under agitation condition, filter, dry, can obtain sodium metavanadate solid 37.2g, product purity is 89.2%, and yield is 95%.
By embodiments of the invention 1-4 and comparative example 1-4 being compared as can be known the product purity height of the sodium metavanadate that the method according to this invention prepares, rate of recovery height.
In addition, according to the method for preparing sodium metavanadate of the present invention, (1) contains in the process of the many vanadic acid sodiums of ammonium in precipitation, and the sodium of part has entered product in the leach liquor, has saved the consumption of sodium hydroxide, has reduced production cost; (2) to contain the required pH of the many vanadic acid sodiums of ammonium be 4-4.5 to precipitation, saved sour consumption than acid ammonium salt; (3) to contain the many vanadic acid sodiums of ammonium temperature required be 75 ℃-85 ℃ to precipitation, and speed of response is fast, and energy consumption is lower; (4) sedimentaryly contain many vanadic acid sodiums of ammonium perfect crystalline, crystal grain is thick, structure in the form of sheets, impurity such as the sulphur of absorption, phosphorus, chromium are lower; Final product sodium metavanadate purity height (reaching more than 99%), foreign matter content is low; (5) operation is simple, is convenient to suitability for industrialized production; (6) realized the recycle of ammonium salt.
Claims (4)
1. method for preparing sodium metavanadate is characterized in that this method may further comprise the steps:
With mineral acid the pH value of sodium vanadium extraction leach liquor is adjusted to 4-4.5, and is heated 75 ℃-85 ℃, then according to NH
4 +: the mass ratio of V=1.5-2 adds the solubility ammonium salt in solution, stir, and obtains containing many vanadic acid sodiums of ammonium solid after the reaction;
Gained is contained many vanadic acid sodiums of ammonium solid place sealed reactor, mol ratio according to Na: V=0.8-0.9 adds sodium hydroxide solution, stir to the condition of boiling temperature at 90 ℃, in solution, begin white to occur or faint yellow solid is separated out, then solution is cooled to room temperature under agitation condition, filter, drying, thus obtain the sodium metavanadate solid.
2. the method for preparing sodium metavanadate according to claim 1 is characterized in that containing in the sodium vanadium extraction leach liquor V of 20-30g/L
5+, 15-20g/L Na
+, 1-1.5g/L Cr
6+, 0.5-1g/L Si and be less than the P of 0.05g/L.
3. 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.
4. the method for preparing sodium metavanadate according to claim 1 is characterized in that described solubility ammonium salt is at least a in ammonium sulfate, ammonium chloride, the ammonium nitrate.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102531055A (en) * | 2011-12-14 | 2012-07-04 | 攀钢集团有限公司 | Method for preparing sodium metavanadate/potassium metavanadate |
| CN103395838A (en) * | 2013-07-09 | 2013-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | High-purity potassium metavanadate and preparation method thereof |
| CN103833078A (en) * | 2014-03-25 | 2014-06-04 | 时国海 | Vanadium precipitation crystallization method for extracting ammonium metavanadate |
| CN104004926A (en) * | 2014-06-11 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadium pentoxide through sodium polyvanadate |
| CN106145188A (en) * | 2016-07-05 | 2016-11-23 | 河北钢铁股份有限公司承德分公司 | A kind of method that sodium vanadium extraction liquid prepares V electrolyte high purity vanadic anhydride |
| CN107117653A (en) * | 2017-05-27 | 2017-09-01 | 河钢股份有限公司承德分公司 | A kind of method for preparing high-purity ammonium poly-vanadate |
| 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 |
| CN107445205A (en) * | 2017-08-17 | 2017-12-08 | 芜湖人本合金有限责任公司 | A kind of method for producing sodium metavanadate and products thereof and application |
| CN107814414A (en) * | 2017-11-09 | 2018-03-20 | 河钢股份有限公司承德分公司 | A kind of industrial high efficiency produces ammonium vanadate sodium technique |
| 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 |
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2009
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102531055A (en) * | 2011-12-14 | 2012-07-04 | 攀钢集团有限公司 | Method for preparing sodium metavanadate/potassium metavanadate |
| CN102531055B (en) * | 2011-12-14 | 2016-01-27 | 攀钢集团有限公司 | The preparation method of sodium metavanadate/potassium metavanadate |
| CN103395838B (en) * | 2013-07-09 | 2015-09-16 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of high purity potassium metavanadate and preparation method thereof |
| CN103395838A (en) * | 2013-07-09 | 2013-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | High-purity potassium metavanadate and preparation method thereof |
| CN103833078A (en) * | 2014-03-25 | 2014-06-04 | 时国海 | Vanadium precipitation crystallization method for extracting ammonium metavanadate |
| CN104004926A (en) * | 2014-06-11 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity vanadium pentoxide through sodium polyvanadate |
| CN104004926B (en) * | 2014-06-11 | 2016-04-27 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method utilizing many vanadic acid sodiums to prepare high-purity vanadium pentoxide |
| CN106145188A (en) * | 2016-07-05 | 2016-11-23 | 河北钢铁股份有限公司承德分公司 | A kind of method that sodium vanadium extraction liquid prepares V electrolyte high purity vanadic anhydride |
| 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 |
| CN107117653A (en) * | 2017-05-27 | 2017-09-01 | 河钢股份有限公司承德分公司 | A kind of method for preparing high-purity ammonium poly-vanadate |
| CN107445205A (en) * | 2017-08-17 | 2017-12-08 | 芜湖人本合金有限责任公司 | A kind of method for producing sodium metavanadate and products thereof and application |
| 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 |
| CN107814414A (en) * | 2017-11-09 | 2018-03-20 | 河钢股份有限公司承德分公司 | A kind of industrial high efficiency produces ammonium vanadate sodium technique |
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