CN104003443A - Method for preparing ammonium metavanadate by adding seed crystals - Google Patents
Method for preparing ammonium metavanadate by adding seed crystals Download PDFInfo
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- CN104003443A CN104003443A CN201410265103.0A CN201410265103A CN104003443A CN 104003443 A CN104003443 A CN 104003443A CN 201410265103 A CN201410265103 A CN 201410265103A CN 104003443 A CN104003443 A CN 104003443A
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Abstract
The invention provides a method for preparing ammonium metavanadate by adding seed crystals. The method includes the following steps which are conducted in sequence that pH of purification solutions containing vanadium is adjusted to 7-12, and then the purification solutions containing the vanadium are cooled to be at the normal temperature; the seed crystals are added to the purification solutions containing the vanadium, and crystallizing agents are added to the purification solutions containing vanadium for reaction after the seed crystals are completely dissolved, wherein the seed crystals are soluble polyvanadate, the crystallizing agents are inorganic ammonium salt, and the addition of the crystallizing agents is determined according to the mole ratio of 1:4 of NH4+ in the crystals to V elements in the solutions; wet ammonium metavanadate is obtained through filtration and is dried to obtain powdery ammonium metavanadate. The method has the advantages that the process is simple and easy to use, the requirement for vanadium solution components is low, the requirement for equipment is low, operation is convenient to carry out and cost is low; reaction time can be shortened to 30-60 min, even 30-45 min, and consequently, the production rhythm can be quickened, and energy consumption can be reduced.
Description
Technical field
The invention belongs to vanadium extraction chemical technology field, specifically, relate to a kind of technology that crystal seed is prepared ammonium meta-vanadate precipitation that adds.
Background technology
Conventionally, ammonium meta-vanadate is faint yellow or white crystal, and mainly, as chemical reagent, catalyzer, siccative, mordant etc., ceramic industry is widely used as glaze, also can be used for producing Vanadium Pentoxide in FLAKES.The method of producing ammonium meta-vanadate in industry is mainly in the sodium vanadate solution after purifying treatment, to add ammonium chloride or ammonium sulfate, obtains ammonium meta-vanadate precipitation: NaVO
3+ NH
4cl=NH
4vO
3↓+NaCl.
Yet, because the solubleness of ammonium meta-vanadate in water is relatively large, higher (1～2.5 grams per liter V of the content of vanadium in waste liquid
2o
5), the whole operating time long (for example, reaching 120min left and right), energy expenditure is larger.
The patent documentation that publication number is CN101121961A provides a kind of pressurization of heating to produce method and the pressurization decomposition tower of heating thereof of ammonium meta-vanadate, this patent documentation has been announced a kind of method of new production ammonium meta-vanadate, its content mainly: first navajoite stone flour being broken into fineness is 80～200 object breezes; Breeze and dilute sulphuric acid or soda ash solution are mixed into ore pulp; Above ore pulp is put into the pressurization decomposition tower pressurization of heating of heating, 80 ℃～240 ℃ of the scopes of heating, pressurization scope 0～3MPa, heats and pressurizes 5～35 minutes; Slag in ore pulp after decomposing, with separated containing vanadium solution, will be sent into extraction tank extraction containing vanadium solution; Then add the back extraction of carbon ammonium, ammonification salt is settled out ammonium meta-vanadate, and ammonium meta-vanadate obtains ammonium meta-vanadate product after centrifuge dehydration, oven dry.Yet this patent documentation adopts the method that adds ammonium salt after back extraction also to have the industrial problems such as in waste liquid, content of vanadium is high, the precipitation time is long, fail fundamentally to solve the preparation problem of ammonium meta-vanadate.
Summary of the invention
The object of the invention is to solve at least one in prior art above shortcomings.
For example, one of object of the present invention is to provide a kind of method of preparing ammonium meta-vanadate that can reduce operating time and energy expenditure.
The invention provides a kind of method that crystal seed is prepared ammonium meta-vanadate that adds.Described method comprises the following steps of carrying out successively: regulate pH to 7～12 containing vanadium scavenging solution, be cooled to subsequently normal temperature; To adding crystal seed containing in vanadium scavenging solution, after dissolving completely, crystal seed adds crystallizing agent, react, wherein, crystal seed is solvable vanadate, crystallizing agent is inorganic ammonium salt, and the add-on of crystallizing agent is according to NH in crystallization
4+be 1～4 to determine with the mol ratio of V element in solution; Filtration obtains wet ammonium meta-vanadate, dry, obtains powdery ammonium meta-vanadate.
In one exemplary embodiment of the present invention, the described TV containing vanadium scavenging solution can be greater than 5g/L.
In one exemplary embodiment of the present invention, it is 8～10 that described adjusting can be controlled the pH containing vanadium scavenging solution containing the step of vanadium scavenging solution pH.
In one exemplary embodiment of the present invention, described crystal seed can be 0.01～0.05 with the mass ratio containing v element in vanadium scavenging solution, preferably, is 0.02～0.04.
In one exemplary embodiment of the present invention, described crystallizing agent can be one or more in ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium oxalate, volatile salt and bicarbonate of ammonia.
In one exemplary embodiment of the present invention, the add-on of described crystallizing agent can be according to NH in crystallization
4+be 2～3 to determine with the mol ratio of V element in solution.
In one exemplary embodiment of the present invention, the temperature of described drying step can be 40～80 ℃.
Compared with prior art, beneficial effect of the present invention comprises: technique is simple and easy to use, the requirement of vanadium liquid composition is loose, equipment requirements is low, easy to operate, cost is low; And can make the reaction times foreshorten to 30～60min (30～45min even), thereby can gather, reduce energy consumption by faster production joint.
Embodiment
Hereinafter, in connection with exemplary embodiment, the method that crystal seed is prepared ammonium meta-vanadate that adds of the present invention is described.
In one exemplary embodiment of the present invention, add crystal seed and prepare the method for ammonium meta-vanadate and formed by following steps:
(1) regulate potential of hydrogen and the temperature containing vanadium scavenging solution
Specifically, regulate pH to 7～12 containing vanadium scavenging solution, will regulate the vanadium scavenging solution that contains after pH value to be cooled to normal temperature subsequently.While regulating pH, can adopt conventional inorganic acid alkali, for example, mineral acid can be the conventional acids such as sulfuric acid, hydrochloric acid, nitric acid, and mineral alkali can be the conventional mineral alkalis such as sodium hydroxide, sodium carbonate, potassium hydroxide, salt of wormwood, saleratus, sodium bicarbonate, ammoniacal liquor.Preferably, the pH containing vanadium scavenging solution being controlled is 8～10.In this exemplary embodiment, containing vanadium scavenging solution, can blow for molten iron scavenging solution, extracting vanadium from stone coal vanadium liquid scavenging solution (or claiming desorbed solution) or the thick vanadium product dissolving gained vanadium liquid etc. of vanadium vanadium slag Leaching Vanadium liquid.
In addition, preferably, containing the TV > 5g/L of vanadium scavenging solution.
(2) add crystal seed and crystallizing agent and form ammonium meta-vanadate precipitation
Specifically, what to step (1), obtain adds crystal seed containing in vanadium scavenging solution, after crystal seed dissolves completely, adds crystallizing agent, reacts, and obtains ammonium meta-vanadate precipitation.The reaction times of this exemplary embodiment is shortened greatly, and for example, the reaction times can be 30～60min, can be even 30～45min.
Wherein, crystal seed is solvable vanadate.The crystal seed adding can be 0.01～0.05 with the mass ratio containing v element in vanadium scavenging solution.For example, crystal seed can be ammonium poly-vanadate and/or many vanadic acid sodiums.
Crystallizing agent is inorganic ammonium salt, and the add-on of crystallizing agent is according to NH in crystallization
4+be 1～4 to determine with the mol ratio of V element in solution.Preferably, the add-on of crystallizing agent is according to NH in crystallization
4+be 2～3 to determine with the mol ratio of V element in solution.For example, crystallizing agent can be one or more in ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium oxalate, volatile salt and bicarbonate of ammonia.
(3) filtration, the dry powdery ammonium meta-vanadate that obtains
The reaction product of filtration step (2), obtains wet ammonium meta-vanadate, and subsequent drying obtains powdery ammonium meta-vanadate.For example, can be positioned in baking oven and be dried.For example, the temperature of drying step can be 40～80 ℃, is preferably 50～60 ℃.
In addition,, in another exemplary embodiment of the present invention, all carry out under the condition stirring above-mentioned steps (1) and (2).
In addition, in another exemplary embodiment of the present invention, after dissolving completely, crystal seed can add at once crystallizing agent.In addition, add at a slow speed crystallizing agent, in adding crystallizer process, add the operations such as strong mixing by taking, also can effectively improve the yield of ammonium meta-vanadate.
The crystal seed that adds of the present invention is prepared the method for ammonium meta-vanadate and is applicable to multiple vanadium liquid, and for example, vanadium liquid can dissolve gained vanadium liquid etc. for scavenging solution, extracting vanadium from stone coal desorbed solution or the thick vanadium product that molten iron blow vanadium vanadium slag Leaching Vanadium liquid.
Below in conjunction with concrete example, exemplary embodiment of the present invention is described in further detail.
Example 1 to 3 vanadium liquid used is the vanadium liquid of table 1 ingredients listed.
Table 1 example 1 to 3 vanadium liquid main chemical compositions/gL used
-1
Example 1
In the clean beaker of 2000mL, add the common vanadium liquid in 1000mL table 1, with sulphur acid for adjusting pH value to 10.0, add at normal temperatures 1.70g ammonium poly-vanadate, after crystal seed dissolves according to NH
4 +/ V=1 adds ammonium sulfate, after ammonium sulfate is dissolved in vanadium liquid, after reaction 60min, filters and obtains wet ammonium meta-vanadate, and wet ammonium meta-vanadate is put into 50 ℃ of baking oven inner dryings, and be 12 hours time of drying.Detecting content of vanadium in Upper-liquor of Precipitating Vanadate Process is 0.34g/L, and precipitation rate is 99%.
Example 2
In the clean beaker of 2000mL, add the common vanadium liquid in 1000mL table 1, with sulphur acid for adjusting pH value to 8.0, add at normal temperatures 0.3g ammonium poly-vanadate, according to NH
4 +/ V=4 adds ammonium sulfate, after ammonium sulfate is dissolved in vanadium liquid, after reaction 30min, filters and obtains wet ammonium meta-vanadate, and wet ammonium meta-vanadate is put into 50 ℃ of baking oven inner dryings, and be 12 hours time of drying.Detecting content of vanadium in Upper-liquor of Precipitating Vanadate Process is 0.28g/L, and precipitation rate is 99.2%.
Example 3
In the clean beaker of 2000mL, add the common vanadium liquid in 1000mL table 1, with sulphur acid for adjusting pH value to 9.0, add at normal temperatures the many vanadic acid sodiums of 1.0g, according to NH
4 +/ V=2 adds ammonium sulfate, after ammonium sulfate is dissolved in vanadium liquid, reacts after 50min, filters and obtains wet ammonium meta-vanadate, and wet ammonium meta-vanadate is put into 50 ℃ of baking oven inner dryings, and be 12 hours time of drying.Detecting content of vanadium in Upper-liquor of Precipitating Vanadate Process is 0.17g/L, and precipitation rate is 99.5%.
Composition/the gL of the extracting vanadium from stone coal desorbed solution of table 2 example 4 to 6
-1
Example 4
In the clean beaker of 2000mL, add the extracting vanadium from stone coal desorbed solution in 1000mL table 2, with sulphur acid for adjusting pH value to 10.0, add at normal temperatures the many vanadic acid sodiums of 7.41g, according to NH
4 +/ V=1 adds ammonium sulfate, after ammonium sulfate is dissolved in vanadium liquid, after reaction 30min, filters and obtains wet ammonium meta-vanadate, and wet ammonium meta-vanadate is put into 50 ℃ of baking oven inner dryings, and be 12 hours time of drying.Detecting content of vanadium in Upper-liquor of Precipitating Vanadate Process is 1.47g/L, and precipitation rate is 99%.
Example 5
In the clean beaker of 2000mL, add the extracting vanadium from stone coal desorbed solution in 1000mL table 2, with sulphur acid for adjusting pH value to 10.0, add at normal temperatures the many vanadic acid sodiums of 1.48g, according to NH
4 +/ V=4 adds ammonium sulfate, after ammonium sulfate is dissolved in vanadium liquid, after reaction 30min, filters and obtains wet ammonium meta-vanadate, and wet ammonium meta-vanadate is put into 50 ℃ of baking oven inner dryings, and be 12 hours time of drying.Detecting content of vanadium in Upper-liquor of Precipitating Vanadate Process is 0.74g/L, and precipitation rate is 99.5%.
Example 6
In the clean beaker of 2000mL, add the extracting vanadium from stone coal desorbed solution in 1000mL table 2, with sulphur acid for adjusting pH value to 10.0, add at normal temperatures 5.0g ammonium poly-vanadate, according to NH
4 +/ V=2 adds ammonium sulfate, after ammonium sulfate is dissolved in vanadium liquid, after reaction 40min, filters and obtains wet ammonium meta-vanadate, and wet ammonium meta-vanadate is put into 60 ℃ of baking oven inner dryings, and be 12 hours time of drying.Detecting content of vanadium in Upper-liquor of Precipitating Vanadate Process is 1.03g/L, and precipitation rate is 99.3%.
In sum, the more existing technique of producing ammonium meta-vanadate of the present invention is compared, and has and is simple and easy to the advantages such as, wide adaptability low, easy to operate by, equipment requirements, cost are low, has good Social benefit and economic benefit.
Although described the present invention in conjunction with exemplary embodiment above, those of ordinary skills should be clear, in the situation that do not depart from the spirit and scope of claim, can carry out various modifications to above-described embodiment.
Claims (8)
1. add crystal seed and prepare a method for ammonium meta-vanadate, it is characterized in that, described method comprises the following steps of carrying out successively:
Regulate pH to 7～12 containing vanadium scavenging solution, be cooled to subsequently normal temperature;
To adding crystal seed containing in vanadium scavenging solution, after dissolving completely, crystal seed adds crystallizing agent, react, wherein, crystal seed is solvable vanadate, crystallizing agent is inorganic ammonium salt, and the add-on of crystallizing agent is according to NH in crystallization
4+be 1～4 to determine with the mol ratio of V element in solution;
Filtration obtains wet ammonium meta-vanadate, dry, obtains powdery ammonium meta-vanadate.
2. according to claim 1ly add the method that crystal seed is prepared ammonium meta-vanadate, it is characterized in that the described TV > 5g/L containing vanadium scavenging solution.
3. according to claim 1ly add the method that crystal seed is prepared ammonium meta-vanadate, it is characterized in that, it is 8～10 that described adjusting is controlled the pH containing vanadium scavenging solution containing the step of vanadium scavenging solution pH.
4. according to claim 1ly add the method that crystal seed is prepared ammonium meta-vanadate, it is characterized in that, described crystal seed is ammonium poly-vanadate and/or many vanadic acid sodiums.
5. according to claim 1ly add the method that crystal seed is prepared ammonium meta-vanadate, it is characterized in that, described crystallizing agent is one or more in ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium oxalate, volatile salt and bicarbonate of ammonia.
6. according to claim 1ly add the method that crystal seed is prepared ammonium meta-vanadate, it is characterized in that, the add-on of described crystallizing agent is according to NH in crystallization
4+be 2～3 to determine with the mol ratio of V element in solution.
7. according to claim 1ly add the method that crystal seed is prepared ammonium meta-vanadate, it is characterized in that, described in the step of reacting the reaction times be 30～60min.
8. according to claim 1ly add the method that crystal seed is prepared ammonium meta-vanadate, it is characterized in that, the temperature of described drying step is 40～80 ℃.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876268A (en) * | 2015-06-10 | 2015-09-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of high-density ammonium polyvanadate |
| CN106006732A (en) * | 2016-08-05 | 2016-10-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing ammonium polyvanadate from high concentration vanadium liquid |
| CN106044853A (en) * | 2016-08-08 | 2016-10-26 | 大连博融新材料股份有限公司 | Purification method for deep silica removal of ammonium metavanadate |
| CN106241872A (en) * | 2016-07-29 | 2016-12-21 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN107381637A (en) * | 2017-09-04 | 2017-11-24 | 河钢股份有限公司承德分公司 | A kind of method of preventing scaring in ammonium metavanadate crystallization process |
| CN109179504A (en) * | 2018-10-19 | 2019-01-11 | 河钢股份有限公司承德分公司 | A method of preparing big granularity ammonium metavanadate |
| CN110016556A (en) * | 2019-05-20 | 2019-07-16 | 昆明理工大学 | The method of precipitation from alkaline vanadium chromium solution |
| CN110157927A (en) * | 2019-03-27 | 2019-08-23 | 杨秋良 | A kind of no ammonium precipitation vanadium method |
| CN113955801A (en) * | 2021-12-09 | 2022-01-21 | 淄博凡纳蒂斯技术服务有限公司 | Method for preparing high-purity ammonium metavanadate by seed crystal decomposition method |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876268A (en) * | 2015-06-10 | 2015-09-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of high-density ammonium polyvanadate |
| CN106241872A (en) * | 2016-07-29 | 2016-12-21 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN106241872B (en) * | 2016-07-29 | 2018-05-18 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN106006732A (en) * | 2016-08-05 | 2016-10-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing ammonium polyvanadate from high concentration vanadium liquid |
| CN106044853A (en) * | 2016-08-08 | 2016-10-26 | 大连博融新材料股份有限公司 | Purification method for deep silica removal of ammonium metavanadate |
| CN107381637A (en) * | 2017-09-04 | 2017-11-24 | 河钢股份有限公司承德分公司 | A kind of method of preventing scaring in ammonium metavanadate crystallization process |
| CN109179504A (en) * | 2018-10-19 | 2019-01-11 | 河钢股份有限公司承德分公司 | A method of preparing big granularity ammonium metavanadate |
| CN109179504B (en) * | 2018-10-19 | 2020-12-04 | 河钢股份有限公司承德分公司 | Method for preparing large-particle-size ammonium metavanadate |
| CN110157927A (en) * | 2019-03-27 | 2019-08-23 | 杨秋良 | A kind of no ammonium precipitation vanadium method |
| CN110016556A (en) * | 2019-05-20 | 2019-07-16 | 昆明理工大学 | The method of precipitation from alkaline vanadium chromium solution |
| CN113955801A (en) * | 2021-12-09 | 2022-01-21 | 淄博凡纳蒂斯技术服务有限公司 | Method for preparing high-purity ammonium metavanadate by seed crystal decomposition method |
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