CN110016548A - The method of vanadium titano-magnetite concentrate roasting extraction vanadium extraction - Google Patents
The method of vanadium titano-magnetite concentrate roasting extraction vanadium extraction Download PDFInfo
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- CN110016548A CN110016548A CN201910429402.6A CN201910429402A CN110016548A CN 110016548 A CN110016548 A CN 110016548A CN 201910429402 A CN201910429402 A CN 201910429402A CN 110016548 A CN110016548 A CN 110016548A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/28—Amines
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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Abstract
The invention discloses a kind of methods of vanadium titano-magnetite concentrate roasting extraction vanadium extraction, the following steps are included: A, will vanadium titano-magnetite concentrate roasting after must roast clinker, clinker acidleach under conditions of pH is 0.5~2.0 will be roasted, leachate and leached tailings are separated by solid-liquid separation to obtain；B, using organic amine as extractant, extraction leachate obtains organic phase a；C, using alkali as stripping agent, extraction organic phase a obtains rich vanadium liquid and organic phase b；Rich vanadium liquid is after precipitation, calcining up to vanadic anhydride.The present invention uses the direct vanadium extraction of vanadium titano-magnetite concentrate, and process is short, at low cost, vanadium high income, can be recycled after waste water simple process, the tailings after vanadium extraction can be directly used for blast furnace ironmaking.
Description
Technical field
The invention belongs to vanadium extractive technique fields, and in particular to a kind of side of vanadium titano-magnetite concentrate roasting extraction vanadium extraction
Method.
Background technique
Vanadium is a kind of important strategy metal, in the world 85% or more vanadium product be extracted from vanadium titano-magnetite and
?.Currently, vanadium titano-magnetite vanadium extraction mainly uses blast furnace ironmaking-vanadium extraction by converter blowing to obtain vanadium slag, sodium roasting is further used
Or calcification baking produces vanadium oxide product.However, the long flow path, vanadium yield only 45%~50%, and this art production process
In give off a large amount of HCl and Cl2The waste water of gas and the sodium chloride containing high concentration, causes serious environmental pollution.With complete
Attention of the ball to environmental protection and raising utilization of resources, finds new low pollution, efficient process for extracting vanadium has become entirely
A urgent problem to be solved in ball vanadium smelting industry.
CN105483398A discloses a kind of containing vanadium mineral curing extraction vanadium method, comprising the following steps: will first contain vanadium mineral
It is rough and torn, a certain amount of water, phosphoric acid and the concentrated sulfuric acid are then added into resulting miberal powder and is uniformly mixed, the mixed material of acid will be mixed
It is cured under certain high temperature, obtained clinker is gone out with water logging at normal temperatures and pressures, leachate is obtained after solid-liquor separation
And leached mud.Although the method shortens process, but acid consumption is big in vanadium extracting process and leachate impurity content is high, after being unfavorable for
The preparation of phase vanadium product.
CN105671340A discloses a kind of method of vanadium extraction of low-temperature bake containing vanadium raw materials, the method are as follows: will contain vanadium original
Material mix with manganese source after roast, obtain containing vanadium it is ripe, later, vanadium bearing slag is leached with ammonium salt solution, separation of solid and liquid, obtain contain vanadium
Liquid and tailings in vanadium extraction.Although the method shortens process, can get the vanadium product of high-quality, but ammonium salt consumption is high, and promoter manganese returns
It receives using difficult.
CN106755964A proposes a kind of method of the low direct vanadium extraction of swage vanadium titano-magnetite of high vanadium titanium, to v-ti magnetite
Sodium sulphate is added in mine miberal powder and sodium carbonate, binder and water, agglomeration successively carry out water logging after oxidizing roasting and acidleach contained
Vanadium leachate then clean and Vanadium Concentrationin, using molysite precipitation using ion exchange to leachate.The method can realize vanadium
High efficiency extraction, but tailings contains sodium, and gained tailings can not be used as smelting iron and steel raw material；Roasting process has SO2Polluted gas generates；Stream
Journey is complicated；Molysite precipitation can not obtain high-quality vanadium product.
Summary of the invention
The purpose of the present invention is to provide a kind of extraction vanadium methods at low cost and can obtaining high-quality vanadium product.
The present invention provides a kind of methods of vanadium titano-magnetite concentrate roasting extraction vanadium extraction, comprising the following steps:
A, clinker will must be roasted after the roasting of vanadium titano-magnetite concentrate, roasting clinker is sour under conditions of pH is 0.5~2.0
Leaching, is separated by solid-liquid separation to obtain leachate and leached tailings；
B, using organic amine as extractant, extraction leachate obtains organic phase a；
C, using alkali as stripping agent, extraction organic phase a obtains rich vanadium liquid and organic phase b；Rich vanadium liquid after precipitation, calcining to obtain the final product
Vanadic anhydride.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction, in step A, the roasting refers to vanadium titanium
Magnetite concentrate stops roasting, is placed in air and is cooled to room in 800~1000 DEG C of 0.5~3h of roasting after being cooled to 600 DEG C
Temperature.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction, in step A, liquid used in acidleach is dilute sulphur
The liquid-solid ratio of acid solution, dilution heat of sulfuric acid and roasting clinker is 1L~3L:1g.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction, in step A, the leached tailings are washed,
The aqueous solution that tailings directly as smelting iron and steel raw material, can be washed after drying returns to leaching process.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction, in step B, the organic amine is primary amine
7101, one or more of primary amine N11923, secondary amine 7203 or secondary amine 7206；Preferably, the organic amine is primary amine
7101 or primary amine N11923.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction, in step B, the organic amine and leachate
In vanadic anhydride molar ratio be 1:1.5~2.
Wherein, in step C, before extraction, stripping agent is made for the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction
The volume ratio of the stripping aqueous solution that mass fraction is 20%, the stripping aqueous solution and organic phase a are 2~3:1.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction, in step C, the alkali is sodium carbonate, carbonic acid
One or more of hydrogen sodium, sodium hydroxide, ammonium carbonate or ammonium hydrogen carbonate.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction,
When alkali is sodium carbonate, sodium bicarbonate or sodium hydroxide, the precipitation is directed to that ammonium salt is added in rich vanadium liquid, adjusts
PH is 2~2.5, is stirred at 95 DEG C to get ammonium poly-vanadate precipitating；
When alkali is ammonium carbonate or ammonium hydrogen carbonate, the precipitation refer to by ammonium carbonate or ammonium hydrogen carbonate crystallisation by cooling to get
Ammonium poly-vanadate precipitating.
Wherein, the method for above-mentioned vanadium titano-magnetite concentrate roasting extraction vanadium extraction, in step C, gained waste water after the precipitation
Leaching or tailings washing process are returned after neutralized.
The beneficial effects of the present invention are:
The present invention uses the direct vanadium extraction of vanadium titano-magnetite concentrate, and process is short, at low cost, vanadium high income, waste water simple process
After can be recycled, the tailings after vanadium extraction can be directly used for blast furnace ironmaking.
Specific embodiment
Specifically, a kind of method of vanadium titano-magnetite concentrate roasting extraction vanadium extraction, comprising the following steps: A, by v-ti magnetite
Clinker must be roasted after the roasting of mine concentrate, by acidleach under conditions of pH is 0.5~2.0 of roasting clinker, is separated by solid-liquid separation to obtain leachate
And leached tailings；B, using organic amine as extractant, extraction leachate obtains organic phase a；C, it using alkali as stripping agent, extracts organic
Phase a obtains rich vanadium liquid and organic phase b；Rich vanadium liquid is after precipitation, calcining up to vanadic anhydride.
The ingredient of vanadium titano-magnetite concentrate used in the present invention is as follows: V2O5For 0.3~1.0%, TiO2For 10~18%, Fe
For 48.5~55.5%, SiO2It is 0.8~2.0, MgO for 3.5~5.2%, CaO be 1.0~5.0%, S is 0.2~0.6%, P
It is 0.01~0.04%, Ni for 0.002~0.006%, Co is 0.01~0.03%.Granularity is in the vanadium titano-magnetite concentrate
The weight ratio of 0.074mm is greater than 80%.
In the method for the present invention, liquid-solid ratio is too high, and vanadium concentration is low in obtained leachate, and it is low to leach production efficiency；Liquid-solid ratio
Too low, stirring is difficult, is unfavorable for production and goes on smoothly.Therefore, the present invention sets the liquid-solid ratio of dilution heat of sulfuric acid and roasting clinker
It is set to 1L~3L:1g.
The dosage of extractant efficiency and extractant in order to balance, five oxidations in step B, in the organic amine and leachate
The molar ratio of two vanadium is 1:1.5~2；In step C, before extraction, the stripping aqueous solution that mass fraction is 20% is made in stripping agent,
The volume ratio of the stripping aqueous solution and organic phase a are 2~3:1.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
1000 grams of vanadium titano-magnetite concentrate are taken to take out when 900 DEG C of roasting 1.5h, 600 DEG C in Muffle furnace cold in air
But roasting clinker is obtained to room temperature.Clinker is placed in leaching tanks, using dilute sulfuric acid as leachate, the liquid of leachate and clinker is solid
Than 1:1,2h is leached under pH=0.5, leachate is obtained by filtration, six grades are successively carried out to leachate with primary amine 7101 and extracts to have
The molar ratio of vanadic anhydride is 1.5:1 in machine phase a, primary amine 7101 and leachate, and vanadium extraction yield is 98.5%.
1h is stripped to organic phase a using 20% aqueous sodium carbonate, obtains rich vanadium liquid and organic phase b, wherein organic phase a
Volume ratio with 20% aqueous sodium carbonate is 1:2, extraction link recycling is returned to after organic phase b processing, into rich vanadium liquid
The molar ratio of addition ammonium sulfate, ammonium sulfate and vanadic anhydride is 1.5, and adjusting pH value of solution is to stir 60min at 2.2,95 DEG C, is obtained
It is precipitated to ammonium poly-vanadate, filtering, is calcined after dry and obtain vanadic anhydride product.
Every wheel leached tailings are washed by liquid-solid ratio 1:1.Tailings obtains ingredient through 150 DEG C of dry 2h and meets steel smelting
The slag of refining demand.Vanadium wastewater adds milk of lime to adjust pH~9.0, is then recycled as leaching agent and tailings wash water.
Whole process vanadium yield 72%, V in vanadic anhydride product2O5Content is 98.8%, and other impurities content meets industry
Standard requirements.
Embodiment 2
1000 grams of vanadium titano-magnetite concentrate are taken to take out when 800 DEG C of roasting 3h, 600 DEG C in Muffle furnace cooling in air
Roasting clinker is obtained to room temperature.Clinker is placed in leaching tanks, using dilute sulfuric acid as leachate, the liquid-solid ratio of leachate and clinker
1:1 leaches 2h under pH=1.0, leachate is obtained by filtration, and successively carries out six grades to leachate with primary amine N1923 and extracts to have
The molar ratio of vanadic anhydride is 1:2 in machine phase a, primary amine N1923 and leachate, and vanadium extraction yield is 99.1%.
2h is stripped to organic phase a using 20% ammonium carbonate solution, obtains rich vanadium liquid and organic phase b, wherein organic phase a
Volume ratio with 20% aqueous sodium carbonate is 1:2, extraction link recycling is returned to after organic phase b processing, into rich vanadium liquid
The molar ratio of addition ammonium sulfate, ammonium sulfate and vanadic anhydride is 1.5, and adjusting pH value of solution is to stir 60min at 2.2,95 DEG C, is obtained
It is precipitated to ammonium poly-vanadate, filtering, is calcined after dry and obtain vanadic anhydride product.
Every wheel leached tailings are washed by liquid-solid ratio 3:1.Tailings obtains ingredient through 100 DEG C of dry 6h and meets steel smelting
The slag of refining demand.Vanadium wastewater adds milk of lime to adjust pH~10.0, is then recycled as leaching agent and tailings wash water.
Whole process vanadium yield 75%, V in vanadic anhydride product2O5Content is 98.6%, and other impurities content meets industry
Standard requirements.
Embodiment 3
1000 grams of vanadium titano-magnetite concentrate are taken to take out in air when 1000 DEG C of roasting 0.5h, 600 DEG C in Muffle furnace
It is cooled to room temperature to obtain roasting clinker.Clinker is placed in leaching tanks, using dilute sulfuric acid as leachate, the liquid of leachate and clinker
Gu leaching 1h than 1:3 under pH=2.0, leachate being obtained by filtration, six grades of extractions are successively carried out to leachate with primary amine N1923
Organic phase a is obtained, the molar ratio of vanadic anhydride is 1:2 in primary amine N1923 and leachate, and vanadium extraction yield is 99.4%.
1h is stripped to organic phase a using 20% ammonium carbonate solution, obtains rich vanadium liquid and organic phase b, wherein organic phase a
Volume ratio with 20% aqueous sodium carbonate is 1:3, and extraction link recycling is returned after organic phase b processing, and rich vanadium liquid is direct
Crystallisation by cooling obtains ammonium metavanadate precipitate, filtering, calcines after dry and obtains vanadic anhydride product.
Every wheel leached tailings are washed by liquid-solid ratio 2:1.Tailings obtains ingredient through 200 DEG C of dry 1h and meets steel smelting
The slag of refining demand.Vanadium wastewater adds milk of lime to adjust pH~7.0, is then recycled as leaching agent and tailings wash water.
Whole process vanadium yield 71%, V in vanadic anhydride product2O5Content is 98.2%, and other impurities content meets industry
Standard requirements.
Claims (10)
1. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction, which comprises the following steps:
A, clinker will must be roasted after the roasting of vanadium titano-magnetite concentrate, clinker acidleach under conditions of pH is 0.5~2.0 will be roasted,
It is separated by solid-liquid separation to obtain leachate and leached tailings；
B, using organic amine as extractant, extraction leachate obtains organic phase a；
C, using alkali as stripping agent, extraction organic phase a obtains rich vanadium liquid and organic phase b；Rich vanadium liquid is after precipitation, calcining up to five oxygen
Change two vanadium.
2. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step A, institute
It states roasting to refer to vanadium titano-magnetite concentrate in 800~1000 DEG C of 0.5~3h of roasting, stops roasting after being cooled to 600 DEG C, be placed in
It is cooled to room temperature in air.
3. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step A, acid
Soaking liquid used is dilution heat of sulfuric acid, and dilution heat of sulfuric acid and the liquid-solid ratio for roasting clinker are 1L~3L:1g.
4. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step A, institute
State leached tailings it is washed, it is dry after the aqueous solution of tailings directly as smelting iron and steel raw material, can be washed return to leaching process.
5. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step B, institute
Stating organic amine is one or more of primary amine 7101, primary amine N11923, secondary amine 7203 or secondary amine 7206；Preferably, institute
Stating organic amine is primary amine 7101 or primary amine N11923.
6. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step B, institute
The molar ratio for stating the vanadic anhydride in organic amine and leachate is 1:1.5~2.
7. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step C, extraction
Before taking, the stripping aqueous solution that mass fraction is 20% is made in stripping agent, the volume ratio of the stripping aqueous solution and organic phase a is
2~3:1.
8. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step C, institute
Stating alkali is one or more of sodium carbonate, sodium bicarbonate, sodium hydroxide, ammonium carbonate or ammonium hydrogen carbonate.
9. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 8, which is characterized in that
When alkali is sodium carbonate, sodium bicarbonate or sodium hydroxide, the precipitation is directed to that ammonium salt is added in rich vanadium liquid, adjusts pH and is
2~2.5, it is stirred at 95 DEG C to get ammonium poly-vanadate precipitating；
When alkali is ammonium carbonate or ammonium hydrogen carbonate, the precipitation refers to ammonium carbonate or ammonium hydrogen carbonate crystallisation by cooling to get more vanadium
Sour ammonia-sinking is formed sediment.
10. the method for vanadium titano-magnetite concentrate roasting extraction vanadium extraction according to claim 1, which is characterized in that in step C,
Leaching or tailings washing process are returned after gained waste water is neutralized after the precipitation.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110387463A (en) * | 2019-09-03 | 2019-10-29 | 昆明禾丰环境研究所 | A method of vanadic anhydride is produced using vanadium ferrotianium mineral intergrowth |
| CN110735032A (en) * | 2019-09-03 | 2020-01-31 | 昆明禾丰环境研究所 | vanadium-titanium-iron paragenetic ore treatment process |
| CN112080651A (en) * | 2020-09-23 | 2020-12-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
| CN112250110A (en) * | 2020-10-09 | 2021-01-22 | 中南大学 | Preparation method of ammonium metavanadate without wastewater discharge |
| CN115478178A (en) * | 2022-08-30 | 2022-12-16 | 广东省科学院资源利用与稀土开发研究所 | Method for efficiently extracting vanadium and manganese from vanadium precipitation mother liquor obtained by calcium roasting, acid leaching and vanadium extraction of vanadium slag |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110735032B (en) * | 2019-09-03 | 2021-04-06 | 昆明禾丰环境研究所 | Vanadium-titanium-iron paragenetic ore treatment process |
| CN112080651A (en) * | 2020-09-23 | 2020-12-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting |
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| CN112250110A (en) * | 2020-10-09 | 2021-01-22 | 中南大学 | Preparation method of ammonium metavanadate without wastewater discharge |
| CN115478178A (en) * | 2022-08-30 | 2022-12-16 | 广东省科学院资源利用与稀土开发研究所 | Method for efficiently extracting vanadium and manganese from vanadium precipitation mother liquor obtained by calcium roasting, acid leaching and vanadium extraction of vanadium slag |
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Application publication date: 20190716 |