CN110306044A - A kind of method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral - Google Patents
A kind of method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral Download PDFInfo
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- CN110306044A CN110306044A CN201910650599.6A CN201910650599A CN110306044A CN 110306044 A CN110306044 A CN 110306044A CN 201910650599 A CN201910650599 A CN 201910650599A CN 110306044 A CN110306044 A CN 110306044A
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- vanadium
- iron
- mineral
- oxalic acid
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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
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
- C22B3/165—Leaching with acyclic or carbocyclic agents of a single type with organic acids
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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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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention provides a kind of method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral, belongs to field of the hydro-thermal method Leaching Vanadium hercynite type containing vanadium in vanadium mineral.The present invention contains vanadium mineral as raw material using vanadium iron spinelle, and iron powder is reducing agent, and oxalic acid solution is leaching agent, its three is mixed into slurry, is reacted under hydrothermal conditions；The slurry obtained after reaction is separated by solid-liquid separation, obtain cleaning contains vanadium leachate and ferrous oxalate byproduct.This method utilize the stronger complexing of oxalate denominationby, respectively in vanadium iron spinelle vanadium and iron formed [V (C2O4)3]3‑, [Fe (C2O4)3]3‑Into solution；[Fe (the C formed2O4)3]3‑Ferrous oxalate precipitating is generated with Fe powder, to be conducive to the progress of Leach reaction, and accelerates Leach reaction rate.Method provided by the invention is realized to vanadium iron spinelle efficient vanadium extracting containing vanadium mineral, and realizes the vanadium iron separation in leaching process, simplifies processing step, and obtain the byproduct of high added value, ferrous oxalate.
Description
Technical field
The invention belongs to field of the hydro-thermal method Leaching Vanadium hercynite type containing vanadium in vanadium mineral.Grass is utilized more particularly to a kind of
The stronger complexing of acid ion and high pressure reducing condition, to accelerate Leach reaction rate, and obtain containing vanadium leachate and
A kind of method of ferrous oxalate byproduct.
Background technique
Vanadium is a kind of important metallic element, is widely used in the industries such as machinery, aviation, electronic technology, national defense industry, because
This has the title of metal " vitamin ".China's vanadium resource is mainly vanadium titano-magnetite and Rock coal containing alum, and the two is different contains
Vanadium resource can be changed by Metallurgical Means contains vanadium mineral with vanadium iron Spinel.
Currently, Pressure hydrometallurgy technique have to adaptability to raw materials it is strong, can carry out at relatively high temperatures, process power
The features such as condition is improved, and is accelerated leaching velocity, is shortened the reaction time, therefore have many workers that Pressure hydrometallurgical process is leached
Technique is applied to vanadium extraction field, for example, Chinese patent CN107236871A, CN102531056A, CN105420517A etc. are
By pressure leaching metallurgical technology from containing vanadium extraction is carried out in vanadium mineral, final obtain contains vanadium leachate.They the characteristics of are with strong
Aqueous slkali is as leaching agent, under conditions of certain temperature and pressure, is passed through oxygen, carries out the reaction of high temperature and pressure Oxidation Leaching,
And it obtains and contains vanadium leachate.But a large amount of silicon enters solution, will affect the purity of final vanadium product, therefore can be added CaO into
Row desiliconization, and make increased costs；In addition to this, strong base solution is strong to high-tension apparatus corrosivity, and maintenance cost is high, and the service life is low.Cause
This will solve the disadvantage that highly basic leaching agent is brought, and metallargist selects oxalic acid as leaching agent, and oxalic acid belongs to weak acid, corrosivity
It is weaker, there is stronger complexation property.Chinese patent CN105624435A is using fluoride and oxalic acid as leaching agent, selective leaching
Vanadium in bone coal out, but leaching rate is lower, and fluoride pollution environment, endangers people larger.Perhaps first month of spring et al. is to vanadium extraction
Tailings leaching behavior progress experimental study (experimental study [D] the Northeastern University of Xu Mengchun tailings in vanadium extraction leaching behavior,
2012.), under an increased pressure, the excessive of iron is avoided to dissolve out to control the additional amount of oxalic acid, object containing vanadium is mutually led in tailings in vanadium extraction
To be vanadium iron spinelle, inhibit the dissolution of iron, the leaching of vanadium will necessarily be prevented, so leaching rate is lower, up to 66% is left
It is right.And it leaches in residue there are also the vanadium not being leached largely and chromium, cannot arbitrarily discharge, leached tailings processing is difficult.
In order to solve above-mentioned problems faced, the present invention proposes completely new slave metallurgy routes of the vanadium iron spinelle containing vanadium extraction in vanadium mineral,
Using oxalic acid as leaching agent, iron powder is reducing agent, and vanadium iron spinelle is raw material containing vanadium mineral, its three is mixed into slurry, low
Under warm pressurized conditions, by vanadium iron spinelle vanadium and iron leach jointly, under the action of iron powder, the ferric iron that is dipped into solution
Under the action of reduced iron powder, ferrous oxalate precipitating is formed, realizes the vanadium iron separation in leachate, and obtain soaking containing vanadium for cleaning
Liquid out.
Summary of the invention
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of hydro-thermal oxalic acid complexation leaching vanadium iron points
Method of the spar containing vanadium in vanadium mineral contains vanadium mineral as raw material using vanadium iron spinelle, iron powder is reducing agent, and oxalic acid solution is leaching
Its three is mixed into slurry, is reacted under low temperature pressurized conditions by agent out；The slurry obtained after reaction is separated by solid-liquid separation,
Obtain cleaning contains vanadium leachate and ferrous oxalate byproduct.
For existing high-pressure oxidation leaches vanadium extraction, this method utilizes the stronger complexing of oxalate denominationby,
Respectively in vanadium iron spinelle vanadium and iron formed [V (C2O4)3]3-, [Fe (C2O4)3]3-Into solution；[the Fe formed
(C2O4)3]3-Ferrous oxalate precipitating is generated with Fe powder, to be conducive to the progress of Leach reaction, and accelerates Leach reaction rate.
A kind of method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral, it is characterised in that including following step
It is rapid:
(1) vanadium iron spinelle is mixed containing the mixture of vanadium mineral, iron powder with oxalic acid solution, forms slurry, is placed in reaction
In kettle, reacted under pressure；
(2) slurry obtained after step (1) reaction is separated by solid-liquid separation, is obtained containing vanadium leachate and filter cake, and to filter
Cake is dried；
(3) to step (2) drying after filter cake be rinsed with deionized water, according to ferrous oxalate with leaching residue it is close
Degree is different, obtains ferrous oxalate byproduct and leaches residue.
Further, step (1) the vanadium iron spinel-type is 0.074mm or less containing its granularity of vanadium mineral；The iron powder
As reducing agent；For oxalic acid solution as leaching agent, mass concentration is 10%~40%.
Further, step (1) iron powder and mass ratio of the vanadium iron spinelle containing vanadium mineral are (2-5): 1.
Further, the temperature of step (1) described reaction is 105 DEG C~135 DEG C, the pressure of the reaction be 1Mpa~
5Mpa, the time of the reaction are 15min~120min, and the reaction mixing speed is 500rpm.In step (1) reaction process
Following reaction may occur:
2Fe2VO4+8H2C2O4+Fe→5FeC2O4↓+V2(C2O4)3+8H2O
Fe+8H2C2O4→FeC2O4↓+H2
H2C2O4→CO+CO2+H2O
Further, step (2) is described after reaction, and the temperature of separation of solid and liquid is 30 DEG C~40 DEG C.
The technical solution adopted by the present invention has the advantage that compared with prior art
1. the present invention provides a kind of method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral, this method benefit
With the stronger complexing of oxalate denominationby, respectively in vanadium iron spinelle vanadium and iron form [V (C2O4)3]3-, [Fe
(C2O4)3]3-Into solution.
2. under the action of reduced iron powder, [Fe (C2O4)3]3-Ferrous oxalate precipitating is formed with iron powder, thus in leaching process
Middle realization vanadium iron separation, simplifies process, and accelerate Leach reaction rate.
3. this method required temperature is low, to reduce energy consumption；In addition, obtaining ferrous oxalate byproduct, it can be used for battery
The raw material of LiFePO 4 of anode material.
4. this method is compared with traditional pressure oxidation extract technology, without being passed through for oxidizing gas, equipment is simple, cost
It is low；Without the addition of oxidant, leachate is clean；Reduced iron powder of the present invention is nontoxic and tailings processing is simple.
Detailed description of the invention
Fig. 1 is vanadium extraction flow chart of the invention.
Fig. 2 is the XRD spectrum of ferrous oxalate obtained.
Specific embodiment
In order to verify feasibility of the invention, below with reference to the example content that the present invention is further explained, but it is of the invention
Content is not limited solely to following example.The simple modification that substantive content according to the present invention is made, should all cover in this hair
Within bright protection scope.
Embodiment 1:
Using vanadium trioxide and di-iron trioxide as initial feed, under reducing atmosphere, temperature is to roast at 1200 DEG C
Pure Fe is made in 48h2VO4.Pure Fe will be obtained2VO4Grind size is to 0.074mm hereinafter, and weighing the vanadium after 0.2g ball milling
The reduced iron powder of hercynite and 0.6g is placed in reaction kettle after being mixed together, and the oxalic acid of 20ml mass fraction 30% is added
Solution forms mixed slurry in reaction kettle, at 135 DEG C of reaction temperature, time 120min, the condition of mixing speed 500rpm
Under, it carries out Leach reaction and is separated by solid-liquid separation after reaction, obtain and contain vanadium leachate and filter cake, filter cake is washed,
Ferrous oxalate byproduct is obtained according to elutriation method and leaches residue.It is finally by the concentration that ICP-AES measures vanadium in leachate
2.2g/L, the concentration for measuring iron in leachate is 95mg/L.
Embodiment 2:
According to the method for Chinese patent CN106011456A and CN107641723A, using bone coal as initial feed, three oxidations
Two iron are as additive, and under reducing atmosphere, temperature is 1200 DEG C of roastings, and obtaining after magnetic separation, there is vanadium iron spinel-type to contain
Vanadium concentrate.By the vanadium iron spinel-type ball milling granularity of concentrate containing vanadium of acquisition to 0.074mm hereinafter, vanadium after weighing the ball milling of 0.2g
The reduced iron powder of concentrate and 0.6g, after being mixed together be placed in reaction kettle in, be added 20ml mass fraction 30% oxalic acid solution in
In reaction kettle, mixed slurry is formed, under conditions of 135 DEG C of reaction temperature, time 120min, mixing speed 500rpm, is carried out
Leach reaction is separated by solid-liquid separation after reaction, is obtained and is contained vanadium leachate and filter cake, washs to filter cake, according to elutriation
Method obtains ferrous oxalate byproduct and leaches residue.It is 637.5mg/ finally by the concentration that ICP-AES measures vanadium in leachate
L, leaching rate 98%, the concentration for measuring iron in leachate is 80.5mg/L.
Embodiment 3:
Using vanadium slag as initial feed, by vanadium slag ball milling granularity to 0.074mm or less.Vanadium slag after weighing the ball milling of 0.2g,
It with the reduced iron powder of 0.6g, is placed in reaction kettle after being mixed together, the oxalic acid solution of 20ml mass fraction 30% is added in reaction
In kettle, forms mixed slurry and leached under conditions of 135 DEG C of reaction temperature, time 120min, mixing speed 500rpm
Reaction, after reaction, is separated by solid-liquid separation, and is obtained and is contained vanadium leachate and filter cake, washs to filter cake, obtained according to elutriation method
It obtains ferrous oxalate byproduct and leaches residue.It is 497mg/L, leaching finally by the concentration that ICP-AES measures vanadium in leachate
Extracting rate is 89%, and the concentration for measuring iron in leachate is 75mg/L.
Claims (5)
1. a kind of method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral, it is characterised in that including following step
It is rapid:
(1) vanadium iron spinelle is mixed containing the mixture of vanadium mineral, iron powder with oxalic acid solution, forms slurry, is placed in reaction kettle,
It is reacted under pressure；
(2) obtained slurry after step (1) reaction is separated by solid-liquid separation, is obtained containing vanadium leachate and filter cake, and to filter cake into
Row drying；
(3) filter cake after step (2) drying is rinsed with deionized water, according to ferrous oxalate and leaches the density of residue not
Together, it obtains ferrous oxalate byproduct and leaches residue.
2. method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral as described in claim 1, which is characterized in that
Step (1) the vanadium iron spinel-type is 0.074mm or less containing its granularity of vanadium mineral；The iron powder is as reducing agent；Oxalic acid is molten
For liquid as leaching agent, mass concentration is 10%~40%.
3. method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral as described in claim 1, which is characterized in that
Step (1) iron powder and mass ratio of the vanadium iron spinelle containing vanadium mineral are (2-5): 1.
4. method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral as described in claim 1, which is characterized in that
The temperature of step (1) described reaction is 105 DEG C~135 DEG C, and the pressure of the reaction is 1Mpa~5Mpa, the time of the reaction
For 15min~120min, the reaction mixing speed is 500rpm.
5. method of the hydro-thermal oxalic acid complexation leaching vanadium iron spinelle containing vanadium in vanadium mineral as described in claim 1, which is characterized in that
Step (2) is described after reaction, and the temperature of separation of solid and liquid is 30 DEG C~40 DEG C.
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| CN201910650599.6A CN110306044B (en) | 2019-07-18 | 2019-07-18 | Method for leaching vanadium from vanadium-containing mineral of vanadium-iron spinel by hydrothermal oxalic acid complexation |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110747358A (en) * | 2019-10-16 | 2020-02-04 | 北京科技大学 | Method for precipitating vanadium from vanadium-containing oxalic acid leaching mother liquor by hydrothermal method |
| CN111041200A (en) * | 2019-11-18 | 2020-04-21 | 北京科技大学 | Method for leaching vanadium, titanium and chromium from vanadium, titanium and chromium raw materials by organic acid through hydrothermal method |
| CN111519026A (en) * | 2020-04-30 | 2020-08-11 | 西安建筑科技大学 | Method for leaching secondary coated gold hematite |
| CN112342399A (en) * | 2020-10-16 | 2021-02-09 | 北京科技大学 | Method for simultaneously extracting vanadium, titanium and chromium from vanadium slag |
| CN112941327A (en) * | 2021-03-09 | 2021-06-11 | 河南理工大学 | Method for selectively separating vanadium and iron from red mud |
| CN115463935A (en) * | 2021-10-14 | 2022-12-13 | 中钢集团马鞍山矿山研究总院股份有限公司 | Method for preparing lithium battery anode material lithium iron phosphate by using iron-rich solid wastes in metallurgical industry |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110747358A (en) * | 2019-10-16 | 2020-02-04 | 北京科技大学 | Method for precipitating vanadium from vanadium-containing oxalic acid leaching mother liquor by hydrothermal method |
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| CN111041200A (en) * | 2019-11-18 | 2020-04-21 | 北京科技大学 | Method for leaching vanadium, titanium and chromium from vanadium, titanium and chromium raw materials by organic acid through hydrothermal method |
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| CN111519026A (en) * | 2020-04-30 | 2020-08-11 | 西安建筑科技大学 | Method for leaching secondary coated gold hematite |
| CN111519026B (en) * | 2020-04-30 | 2022-01-18 | 西安建筑科技大学 | Method for leaching secondary coated gold hematite |
| CN112342399A (en) * | 2020-10-16 | 2021-02-09 | 北京科技大学 | Method for simultaneously extracting vanadium, titanium and chromium from vanadium slag |
| CN112941327A (en) * | 2021-03-09 | 2021-06-11 | 河南理工大学 | Method for selectively separating vanadium and iron from red mud |
| CN112941327B (en) * | 2021-03-09 | 2022-06-10 | 河南理工大学 | Method for selectively separating vanadium and iron from red mud |
| CN115463935A (en) * | 2021-10-14 | 2022-12-13 | 中钢集团马鞍山矿山研究总院股份有限公司 | Method for preparing lithium battery anode material lithium iron phosphate by using iron-rich solid wastes in metallurgical industry |
| WO2023060889A1 (en) * | 2021-10-14 | 2023-04-20 | 中钢集团马鞍山矿山研究总院股份有限公司 | Method for extracting fe, zn and pb from electric furnace dedusting ash and high value utilization of same |
| CN115463935B (en) * | 2021-10-14 | 2023-07-28 | 中钢集团马鞍山矿山研究总院股份有限公司 | Method for preparing lithium battery anode material lithium iron phosphate by using iron-rich solid waste in metallurgical industry |
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