CN109868365A - The method of the vanadium extraction of depth containing vanadium raw materials - Google Patents
The method of the vanadium extraction of depth containing vanadium raw materials Download PDFInfo
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- CN109868365A CN109868365A CN201910221221.4A CN201910221221A CN109868365A CN 109868365 A CN109868365 A CN 109868365A CN 201910221221 A CN201910221221 A CN 201910221221A CN 109868365 A CN109868365 A CN 109868365A
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Abstract
The present invention relates to the methods of the vanadium extraction of depth containing vanadium raw materials, belong to the metallurgical technology field of vanadium.Present invention solves the technical problem that being that existing process for extracting vanadium vanadium loss is big, process flow is more complex.The invention discloses the method for the vanadium extraction of depth containing vanadium raw materials, A. mixes vanadium-containing material, phosphate with sulfuric acid, controls mixed slurry pH=0.5~1.5, carries out acidleach, obtains leachate through being separated by solid-liquid separation；B. leachate pH=3.0~4.2 are adjusted, is separated by solid-liquid separation and obtains phosphate slag and dephosphorization solution；C. phosphate slag return step A is recycled, and dephosphorization solution is used to prepare vanadium oxide.The present invention shortens process for extracting vanadium process, reduces production cost, have the advantages that easy to operate for acidleach depth vanadium extraction of vanadium-containing material.
Description
Technical field
The invention belongs to the metallurgical technology fields of vanadium, and in particular to the method for the vanadium extraction of depth containing vanadium raw materials.
Background technique
Vanadium is widely used in fields such as metallurgy, chemical industry, aerospaces, is extremely important strategic resource.Industrial vanadium
The most important raw materials for production of product are vanadium titano-magnetites, and typical process flow is that blast furnace ironmaking-vanadium-bearing hot metal vanadium extraction-vanadium slag is raw
Produce vanadium oxide；In addition there is part vanadium rule of origin in bone coal, navajoite and secondary containing vanadium resource.In oxidation technique for producing vanadium, contain
Vanadium material blank or calcification baking-acidleach are a typical process for extracting vanadium, and after roasting a vanadium-containing material, vanadium is with pentavalent vanadium
Form exists, and leachate pH is lower, solution system is unstable in the higher situation of pentavalent vanadium concentration, vanadium is easy hydrolytic precipitation and makes
At loss.In order to avoid adversely affecting caused by vanadium hydrolysis, mode acid-leaching vanadium-extracted twice is industrially generallyd use, i.e., for the first time
Acidleach pH=2.8~3.5 are controlled, high concentration pentavalent vanadium can be stabilized within the scope of the pH；Second secondary control acidleach pH and leaching
Liquid vanadium concentration is lower out, leaches vanadium sufficiently and does not hydrolyze.However, above-mentioned mode operating process acid-leaching vanadium-extracted twice is more, work
Skill higher cost.
Summary of the invention
Present invention solves the technical problem that being that existing process for extracting vanadium vanadium loss is big, process flow is more complex.
Technical proposal that the invention solves the above-mentioned problems is to provide the method for the vanadium extraction of depth containing vanadium raw materials, including walks as follows
It is rapid:
A. vanadium-containing material, phosphate are mixed with sulfuric acid, carries out acidleach, obtain leachate through being separated by solid-liquid separation；
B. it adjusts leachate pH and carries out dephosphorization, be separated by solid-liquid separation and obtain phosphate slag and dephosphorization solution；
C. phosphate slag return step A is recycled as acidleach material, and dephosphorization solution is used to prepare vanadium oxide.
Wherein, vanadium-containing material refers to V in step A5+Mass content is 1% or more containing vanadium raw materials.
Wherein, phosphate is at least one of aluminum phosphate, ferric phosphate.
Wherein, step A acidleach process control mixed slurry pH=0.5~1.5.
Wherein, it is 0.3~3g/L, V that step A, which controls phosphorus concentration in leachate,5+Concentration is 10~30g/L.
Wherein, step B adjusts leachate pH=3.0~4.2.
Wherein, it is ammonium hydroxide, ammonium carbonate, ammonium hydrogen carbonate, magnesia, magnesium hydroxide, carbon that step B, which adjusts the reagent of leachate pH,
At least one of sour magnesium, calcium oxide, calcium hydroxide, calcium carbonate.
Beneficial effects of the present invention:
Phosphate is added during acidleach in the present invention, can inhibit the hydrolytic precipitation of vanadium, effectively reduces vanadium loss；This hair
Bright elder generation carries out acidleach in pH reduced levels, can sufficiently leach to containing the vanadium in vanadium raw materials, then by adjusting pH in leachate
Phosphorus be removed, to achieve the purpose that depth vanadium extraction；The present invention shortens acidleach depth vanadium extraction of vanadium-containing material
Process for extracting vanadium process, reduces production cost, has the advantages that easy to operate.
Specific embodiment
The present invention provides the method for the vanadium extraction of depth containing vanadium raw materials, specifically comprises the following steps:
A. vanadium-containing material, phosphate are mixed with sulfuric acid, controls mixed slurry pH=0.5~1.5, carry out acidleach, through solid
Liquid separation obtains leachate；
B. it adjusts leachate pH=3.0~4.2 and carries out dephosphorization, be separated by solid-liquid separation and obtain phosphate slag and dephosphorization solution；
C. phosphoric acid aluminium slag return step A is recycled as acidleach material, and dephosphorization solution is used to prepare vanadium oxide.
Wherein, vanadium-containing material described in step A is particularly with V5+Mass content is 1% or more containing vanadium raw materials, through acidleach
Gained leachate V5+≥10g/L。
Firstly, it is to make in vanadium-containing material that the present invention, which controls the mixed slurry pH containing vanadium-containing material 0.5~1.5,
Vanadium sufficiently dissolve enter leachate, while during acidleach be added phosphate be to improve mixed slurry and leachate
In phosphorus concentration, so that vanadium and phosphorus is formed vanadium phospha polyacid complex compound, vanadium hydrolytic precipitation avoided to cause the loss of vanadium.
Wherein, phosphate is at least one of aluminum phosphate, ferric phosphate.
Then, pH=3.0~4.2 for the leachate that regulating step A of the present invention is obtained make phosphorus, aluminium, iron shape in leachate
Enter phosphate slag at aluminum phosphate and (or) ferric phosphate precipitating, to achieve the purpose that separation of phosphorus.
Wherein, it is 0.3~3g/L, V that step A, which controls phosphorus concentration in leachate,5+Concentration is 10~30g/L.
Wherein, it is ammonium hydroxide, ammonium carbonate, ammonium hydrogen carbonate, magnesia, magnesium hydroxide, carbon that step B, which adjusts the reagent of leachate pH,
At least one of sour magnesium, calcium oxide, calcium hydroxide, calcium carbonate.
The present invention will be further explained by the following examples and explanation.
Embodiment 1
Vanadium-containing material (V after taking roasting2O517.85%, P 0.04%) 100g, it is added to together with 2.98g aluminum phosphate
In 350mL tap water, slurry pH=0.6~0.8 is adjusted with sulfuric acid under room temperature and is stirred to react 60min, is separated by solid-liquid separation, obtains
V in acidleach residue2O5Content is 0.75%, V leaching rate 96.0%；Leachate V5+Concentration 27.46g/L, P concentration 2.55g/L；
Leachate pH=3.8 is adjusted with calcium oxide, the solution P concentration 0.05g/L being separated by solid-liquid separation can be used for preparing vanadium oxide.
Embodiment 2
Vanadium-containing material (V after taking roasting2O517.85%, P 0.04%) 100g, it is added to together with 2.67g aluminum phosphate
In 450mL tap water, slurry pH=1.0~1.2 are adjusted with sulfuric acid under room temperature and are stirred to react 60min, is separated by solid-liquid separation, obtains
V in acidleach residue2O5Content is 0.83%, V leaching rate 95.7%；Leachate V5+Concentration 21.26g/L, P concentration 1.72g/L；
Leachate pH=4.0 is adjusted with magnesia, the solution P concentration 0.05g/L being separated by solid-liquid separation can be used for preparing vanadium oxide.
Embodiment 3
Vanadium-containing material (V after taking roasting2O54.43%, P 0.04%) 100g, it is added to together with 0.58g aluminum phosphate
In 250mL tap water, slurry pH=1.3~1.5 are adjusted with sulfuric acid under room temperature and are stirred to react 30min, is separated by solid-liquid separation, obtains
V in acidleach residue2O5Content is 1.07%, V leaching rate 75.82%；Leachate V5+Concentration 13.43g/L, P concentration 0.68g/L；
Leachate pH=4.2 is adjusted with ammonium hydrogen carbonate, the solution P concentration 0.04g/L being separated by solid-liquid separation can be used for preparing vanadium oxide.
Embodiment 4
Vanadium-containing material (V after taking roasting2O54.43%, P 0.04%) 100g, it is added to together with 0.72g ferric phosphate
In 250mL tap water, slurry pH=0.6~0.8 is adjusted with sulfuric acid under room temperature and is stirred to react 30min, is separated by solid-liquid separation, obtains
V in acidleach residue2O5Content is 0.75%, V leaching rate 83.88%；Leachate V5+Concentration 14.86g/L, P concentration 0.68g/L；
Leachate pH=3.2 is adjusted with ammonium hydrogen carbonate, the solution P concentration 0.04g/L being separated by solid-liquid separation can be used for preparing vanadium oxide.
Claims (7)
1. the method for the vanadium extraction of depth containing vanadium raw materials, it is characterised in that include the following steps:
A. vanadium-containing material, phosphate are mixed with sulfuric acid, carries out acidleach, obtain leachate through being separated by solid-liquid separation；
B. it adjusts leachate pH and carries out dephosphorization, be separated by solid-liquid separation and obtain phosphate slag and dephosphorization solution；
C. phosphate slag return step A is recycled as acidleach material, and dephosphorization solution is used to prepare vanadium oxide.
2. the method for the vanadium extraction of depth containing vanadium raw materials according to claim 1, it is characterised in that: object containing vanadium described in step A
Material refers to V5+Mass content is 1% or more containing vanadium raw materials.
3. the method for the vanadium extraction of depth containing vanadium raw materials according to claim 1 or 2, it is characterised in that: phosphoric acid described in step A
Salt is at least one of aluminum phosphate, ferric phosphate.
4. the method for described in any item vanadium extractions of depth containing vanadium raw materials according to claim 1~3, it is characterised in that: described in step A
Acidleach process control mixed slurry pH=0.5~1.5.
5. the method for the vanadium extraction of depth containing vanadium raw materials according to any one of claims 1 to 4, it is characterised in that: step A control
Phosphorus concentration is 0.3~3g/L, V in the leachate5+Concentration is 10~30g/L.
6. the method for described in any item vanadium extractions of depth containing vanadium raw materials according to claim 1~5, it is characterised in that: step B is adjusted
Leachate pH=3.0~4.2.
7. the method for described in any item vanadium extractions of depth containing vanadium raw materials according to claim 1~6, it is characterised in that: step B is adjusted
The reagent of leachate pH be ammonium hydroxide, ammonium carbonate, ammonium hydrogen carbonate, magnesia, magnesium hydroxide, magnesium carbonate, calcium oxide, calcium hydroxide,
At least one of calcium carbonate.
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| CN112795787A (en) * | 2020-11-19 | 2021-05-14 | 重庆第二师范学院 | Method for extracting vanadium and dephosphorizing phosphorus-containing vanadium slag |
| CN114214514A (en) * | 2021-11-12 | 2022-03-22 | 攀钢集团研究院有限公司 | Method for leaching and removing phosphorus in high-phosphorus calcine roasting vanadium-containing clinker and recycling leachate |
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