CN104694769B - A kind of production method of clean vanadium liquid - Google Patents
A kind of production method of clean vanadium liquid Download PDFInfo
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- CN104694769B CN104694769B CN201510082938.7A CN201510082938A CN104694769B CN 104694769 B CN104694769 B CN 104694769B CN 201510082938 A CN201510082938 A CN 201510082938A CN 104694769 B CN104694769 B CN 104694769B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a kind of production method of clean vanadium liquid, the processing step is:Vanadium slag carries out NH after saltless roasting4 +Leach, amount of water is 1 ~ 4 times of vanadium slag quality, leaching process NH4 +Concentration is 1 ~ 50g/L, and filtering obtains low impurity content ammonium leaching vanadium liquid, i.e., clean vanadium liquid.The present invention simplifies follow-up impurity removal process step, reduces reagent consumption, production cost is low, process cleans are conducive to industrial production using the technique of Sources controlling leachate impurity content.
Description
Technical field
The invention belongs to vanadium field of chemical metallurgical technology, and in particular to a kind of production method of clean vanadium liquid.
Background technology
Vanadic anhydride production conventional method be vanadium slag sodium roasting-vanadium liquid purification-ammonium salt precipitation method, wherein 65% with
On vanadium product come from the method.So-called vanadium liquid purification, exactly removing influences the impurity element of precipitation effect in vanadium liquid, influence
The principal element of vanadium liquid precipitation effect has impurity element(Silicon, phosphorus, iron, aluminium)And suspension in stoste.According to raw material vanadium slag feature,
Vanadium liquid impurity situation Si contents are between 600mg/L to 800mg/L, and P content is between 80mg/L to 100mg/L.
At present, removal of impurities is carried out in 25g/L~30g/L vanadium solutions to vanadium concentration, using traditional vanadium liquid impurity removal process:It is a kind of
It is regulation vanadium liquid pH, silicon, the phosphorus added into vanadium liquid in aluminum sulfate solution, co-precipitation liquid phase;Another is the pH for controlling vanadium liquid,
Calcium or magnesia additives are added into vanadium liquid, silicon, phosphorus in liquid phase is removed.Qualified solution impurity after domestic vanadium industry removal of impurities contains
Measure and be:Silicon is less than 500mg/L, and phosphorus content is less than 15mg/L.
The ammonium salt precipitation method have two kinds:A kind of is that the pH value of the solution containing pentavalent vanadium first is adjusted into 8.5~9.5, then by molten
V in liquid2O5With the mass ratio 1 of ammonium salt:1.3~1.5 add ammonium salt Precipitation ammonium metavanadate;Another reconciled using substep
The pH value of solution adds ammonium salt Precipitation ammonium poly-vanadate to 1.5~2.5, after obtained ammonium metavanadate or ammonium poly-vanadate are passed through
Calcining obtains vanadic anhydride.Because the impurity that precipitation process is carried secretly does not have suitable method to be gone in follow-up process
Remove, so the vanadic anhydride impurity content obtained using process above is higher, the grade of vanadic anhydride only has 98% left side
The right side, containing impurity elements such as Fe, Al, K, Na, Ca, Mg, Si, P, S and As, it is difficult to meet multiple fields to purity of vanadium pentoxide
Requirement.
As can be seen here, using the method for purification is precipitated, it is necessary to add the cleanser of a large amount of calcics, magnesium, aluminium or sodium plasma, produce
Cost is higher and easily causes that the element single index of these in product is exceeded, so the vanadium product purity that production is obtained is not high,
98.5% or so.
The content of the invention
The technical problem to be solved in the present invention is the purification process of simplified vanadium liquid, reduces the use of additives, reduction purification
Cost, improves vanadium production efficiency, realizes the clean manufacturing of clean vanadium liquid.
In order to solve the above technical problems, the present invention takes following technical proposals:
A kind of production method of clean vanadium liquid, vanadium slag carries out NH after saltless roasting4 +Leach, amount of water is vanadium slag quality
1 ~ 4 times, leaching process NH4 +Concentration is 1 ~ 50g/L, and filtering obtains low impurity content ammonium leaching vanadium liquid, i.e., clean vanadium liquid.
Vanadium slag saltless roasting temperature of the present invention is 850 ~ 1050 DEG C, and roasting time is 1-5h, and clinker extraction temperature is 0
~ 50 DEG C, roasting process is without additives.
Leaching pH value of the present invention is 7 ~ 11.
Control ph method of the present invention is that CO is supplemented into solution2, for pressurization tonifying Qi, moulding pressure be 0.1 ~
1MPa。
NH of the present invention4 +Concentration control method is that NH is supplemented into solution3, for pressurization tonifying Qi, moulding pressure be 0.1 ~
1MPa。
The content range of impurity element is as follows in clean vanadium liquid of the present invention:Al<1.0ppm, As<1.0ppm, Ca<
20.0 ppm;Cr<8.0ppm, Fe<10.0ppm, Mg<20.0ppm;Mn<5.0ppm;K<50.0ppm, Na<1000.0 ppm, P<
50.0, Si<50.0ppm;S<100.0ppm.
Obtained purification vanadium liquid of the present invention is suitable for producing high purity vanadium.
Vanadium slag of the present invention meets《Vanadium slag GB5062-85》In regulation.
It is using the beneficial effect produced by above-mentioned technical proposal:The present invention uses Sources controlling leachate impurity content
Technique, simplify follow-up impurity removal process step, reduce reagent consumption, production cost is low, process cleans, be conducive to industrial life
Production.
Embodiment
With embodiment, the present invention is further detailed explanation below.
Embodiment 1
A kind of production method of clean vanadium liquid described herein is carried out according to following technique:
Vanadium slag carries out saltless roasting 1h under the conditions of 1050 DEG C, obtains after roasting clinker, carries out NH4 +Leach, extraction temperature
For 10 DEG C, amount of water is 2 times of vanadium slag quality, and leaching process supplements NH by the 0.1MPa that pressurizes3, adjust NH4 +Concentration is 30g/
L;To solution pressurization 0.1MPa supplements CO2, it is 10 that pH value is leached in adjustment, after stirring, filtering, obtains the leaching of low impurity content ammonium
Vanadium liquid, i.e., clean vanadium liquid, obtained purification vanadium liquid is suitable for producing high purity vanadium.
The content range such as following table of impurity element in the clean vanadium liquid:
Embodiment 2
A kind of production method of clean vanadium liquid described herein is carried out according to following technique:
Vanadium slag carries out saltless roasting 5h under the conditions of 850 DEG C, obtains after roasting clinker, carries out NH4 +Leach, extraction temperature
For 50 DEG C, amount of water is 3 times of vanadium slag quality, and leaching process supplements NH by the 0.5MPa that pressurizes3, adjust NH4 +Concentration is 10g/
L;To solution pressurization 0.3MPa supplements CO2, it is 11 that pH value is leached in adjustment, after stirring, filtering, obtains the leaching of low impurity content ammonium
Vanadium liquid, i.e., clean vanadium liquid, obtained purification vanadium liquid is suitable for producing high purity vanadium.
The content range such as following table of impurity element in the clean vanadium liquid:
Embodiment 3
A kind of production method of clean vanadium liquid described herein is carried out according to following technique:
Vanadium slag carries out saltless roasting 3.5h under the conditions of 930 DEG C, obtains after roasting clinker, carries out NH4 +Leach, leach temperature
Spend for 0 DEG C, amount of water is 1 times of vanadium slag quality, leaching process supplements NH by the 1MPa that pressurizes3, adjust NH4 +Concentration is 1g/L;
To solution pressurization 1MPa supplements CO2, it is 7 that pH value is leached in adjustment, after stirring, filtering, obtains low impurity content ammonium leaching vanadium liquid,
I.e. clean vanadium liquid, obtained purification vanadium liquid is suitable for producing high purity vanadium.
The content range such as following table of impurity element in the clean vanadium liquid:
Embodiment 4
A kind of production method of clean vanadium liquid described herein is carried out according to following technique:
Vanadium slag carries out saltless roasting 2h under the conditions of 1000 DEG C, obtains after roasting clinker, carries out NH4 +Leach, extraction temperature
For 25 DEG C, amount of water is 4 times of vanadium slag quality, and leaching process supplements NH by the 0.3MPa that pressurizes3, adjust NH4 +Concentration is 50g/
L;To solution pressurization 0.5MPa supplements CO2, it is 7 that pH value is leached in adjustment, after stirring, filtering, obtains the leaching of low impurity content ammonium
Vanadium liquid, i.e., clean vanadium liquid, obtained purification vanadium liquid is suitable for producing high purity vanadium.
The content range such as following table of impurity element in the clean vanadium liquid:
Embodiment 5
A kind of production method of clean vanadium liquid described herein is carried out according to following technique:
Vanadium slag carries out saltless roasting 4h under the conditions of 950 DEG C, obtains after roasting clinker, carries out NH4 +Leach, extraction temperature
For 30 DEG C, amount of water is 1.5 times of vanadium slag quality, and leaching process supplements NH by the 1MPa that pressurizes3, adjust NH4 +Concentration is 45g/
L;To solution pressurization 1MPa supplements CO2, it is 9 that pH value is leached in adjustment, after stirring, filtering, obtains low impurity content ammonium leaching vanadium
Liquid, i.e., clean vanadium liquid, obtained purification vanadium liquid is suitable for producing high purity vanadium.
The content range such as following table of impurity element in the clean vanadium liquid:
Claims (3)
1. a kind of production method of clean vanadium liquid, it is characterised in that vanadium slag carries out NH after saltless roasting4 +Leach, amount of water
For 1~4 times of vanadium slag quality, leaching process NH4 +Concentration is 1~50g/L, and filtering obtains low impurity content ammonium leaching vanadium liquid, i.e.,
Clean vanadium liquid;
Clinker extraction temperature is 0~50 DEG C;
The leaching pH value is 7~11;
Control ph method is that CO is supplemented into solution2, for pressurization tonifying Qi, moulding pressure is 0.1~1MPa;
The NH4 +Concentration control method is that NH is supplemented into solution3, for pressurization tonifying Qi, moulding pressure is 0.1~1MPa;
The content range of impurity element is as follows in the clean vanadium liquid:Al<1.0ppm, As<1.0ppm, Ca<20.0 ppm;Cr<
8.0ppm, Fe<10.0ppm, Mg<20.0ppm;Mn<5.0ppm;K<50.0ppm, Na<1000.0 ppm, P<50.0 ppm, Si<
50.0ppm;S<100.0ppm.
2. a kind of production method of clean vanadium liquid according to claim 1, it is characterised in that:The vanadium slag saltless roasting temperature
Spend for 850~1050 DEG C, roasting time is 1-5h, clinker extraction temperature is 0~50 DEG C.
3. a kind of production method of clean vanadium liquid according to claim 1 or 2, it is characterised in that:The clean vanadium liquid is fitted
Share in production high purity vanadium.
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CN110247050A (en) * | 2019-06-21 | 2019-09-17 | 东北大学 | A method of four vanadic sulfides/graphene composite material is prepared using containing vanadium leachate |
CN111378846A (en) * | 2020-04-08 | 2020-07-07 | 东北大学 | Method for extracting vanadium from manganese vanadium slag prepared based on vanadium blowing of converter |
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CN103572063B (en) * | 2013-11-04 | 2015-08-19 | 中国科学院过程工程研究所 | A kind of vanadium slag reclaims the method for vanadium without sodium roasting clean and effective |
CN103952565B (en) * | 2014-04-11 | 2017-01-18 | 中国科学院过程工程研究所 | Method used for preparing ammonium metavanadate from vanadium slag via ammonium salt leaching |
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Address after: 067102 A block 520, Luanhe town finance square, Shuangluan District, Chengde, Hebei Patentee after: River steel Limited by Share Ltd Chengde branch Address before: 067102 Luanhe Town, Shuangluan District, Chengde, Hebei Patentee before: Chengde Branch Co., Ltd. of Hebei Iron & Steel Group |