CN106544514A - A kind of method of Leaching of Vanadium from Vanadium slag - Google Patents
A kind of method of Leaching of Vanadium from Vanadium slag Download PDFInfo
- Publication number
- CN106544514A CN106544514A CN201611050754.3A CN201611050754A CN106544514A CN 106544514 A CN106544514 A CN 106544514A CN 201611050754 A CN201611050754 A CN 201611050754A CN 106544514 A CN106544514 A CN 106544514A
- Authority
- CN
- China
- Prior art keywords
- vanadium
- slag
- leaching
- roasting
- intensification
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- 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
-
- 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
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to vanadium extraction chemical field, discloses a kind of method of Leaching of Vanadium from Vanadium slag, the method is comprised the following steps：(1) vanadium slag, calcium source, gas generation agent and water are mixed, obtains compound；(2) compound is carried out the first intensification roasting and the second intensification roasting successively, obtains vanadium bearing slag；(3) vanadium bearing slag is carried out, after cooling and break process, carrying out acid-leaching vanadium-extracted；Wherein, the condition of the first intensification roasting includes：Final temperature is 500 650 DEG C, and the time is 30 60min；The condition of second roasting includes：Final temperature is 800 900 DEG C, and the time is 60 120min.The Leaching of Vanadium from Vanadium slag method provided by the present invention can obtain higher V leaching rate, and the method have the advantages that roasting process need not plus residue or other inert excipients, without the need for pelletizing and not sizing, with good prospects for commercial application.
Description
Technical field
The present invention relates to vanadium extraction chemical field, in particular it relates to a kind of method of Leaching of Vanadium from Vanadium slag.
Background technology
Vanadium slag mainly has sodium roasting vanadium-extracting and calcification baking vanadium extraction at present as main vanadium extraction raw material.Calcification baking
Need to add in vanadium extraction certain residue or other inert substances dilute anti-sticks, or vanadium slag and grog cause certain pelletizing or
Granularity carries out roasting, alleviates materials from bonding；But return slag is added, causes production efficiency to reduce, and part batch mixing in roasting process
It is uneven, so as to easily cause local bonding；Pelletizing roasting, needs to add the binding agent of pelletizing, can increase and make pelletizing equipment
And the cost of binding agent etc., and pelletizing particle diameter is a scope, suppresses denser, and sintering temperature needs the relatively general powder will
Height is asked just to make pelletizing center material fully oxidized, grog is also needed to be milled down to certain particle size and could leach solvable vanadium；Pelletize is also needed
Want certain Granulation Equipments, accordingly, it would be desirable to seek it is a kind of it is new need not add any residue or inertia supplies for mitigating sintering,
Without the need for the high method of pelletizing pelletize and V leaching rate.
CN104357660A discloses a kind of method of clean manufacturing vanadic anhydride, and the method comprises the steps：Step
Rapid 1, pretreatment of raw material：Uniformly mix with roasting additive after will be high calcium vanadium slag broken, add water, raw material ball is obtained, particle diameter is 8
～12mm；Wherein, additive is CaO or CaCO3, quality by a certain percentage with addition of；Roasting：With the heating rate of 1～5 DEG C/min
Heating raw material ball is incubated 15～240min, obtains roasting grog ball to 800～950 DEG C；Step 3, diluted acid leaching：Roasting is ripe
Leached with dilution heat of sulfuric acid after material ball crushing, be filtrated to get vanadium leachate and filtering residue, filtering residue is washed with water；Step 4, vanadium liquid are net
Change：Add villiaumite to vanadium leachate, control system pH value removes impurity Ca, Mg, Al, the Si in vanadium leachate, obtains vanadium purification
Liquid；Step 5, precipitation：Vanadium scavenging solution using hydrolysis precipitation or ammonium salt precipitation, metavanadic acid or ammonium poly-vanadate are respectively obtained after filtration with
And precipitation extraction raffinate, it is dried metavanadic acid or ammonium poly-vanadate to remove Free water；Step 6, pyrolysis：Pyrolysis metavanadic acid or ammonium poly-vanadate,
Pyrolysis temperature is 200～600 DEG C, and pyrolysis time is 2～3h, obtains powder vanadic anhydride；Step 7, returns in precipitation extraction raffinate
Receive Mn：In the precipitation extraction raffinate obtained to step 5, oxalic acid or ammonium oxalate is added to obtain oxalic acid hydrate Asia manganese precipitation and filtrate.However,
The method is still needed makes raw material ball by vanadium slag and calcification additive, water, then carries out next one-step baking vanadium extraction, cumbersome.
CN103667710A discloses a kind of high calcium vanadium slag clean manufacturing vanadic anhydride technique, and the technique includes following step
Suddenly：A, pretreatment of raw material：To mix homogeneously with additive after high calcium vanadium slag broken, grinding, then pelletize；The additive is
CaO or CaCO3, additive amount is：CaO and V in high calcium vanadium slag in control additive2O5Mass ratio is 0～0.84；B, oxidation
Calcification baking：By the pellet after granulation, roasting obtains roasting grog at a constant temperature；C, dilute sulfuric acid：By roasting chamotte crushing, so
After be added to dilution heat of sulfuric acid in leached, mechanical agitation is adopted in leaching process and constant, the leaching that controls solution system pH
After be filtrated to get vanadium leachate；D, vanadium liquid purification：(NH4) is added in vanadium leachate2CO3Ca, Mg impurity is removed, adds dephosphorization
Agent removes P, Si impurity；E, precipitation：Solution after the purification of step d is respectively obtained after filtration using hydrolysis precipitation or ammonium salt precipitation
Metavanadic acid or ammonium metavanadate and vanadium wastewater, are dried vanadium metavanadic acid or ammonium metavanadate to remove Free water；F, calcining deamination：Forge
Burn metavanadic acid or ammonium metavanadate obtains powder V2O5.However, the technique is by constant temperature calcining after vanadium slag and the granulation of calcification additive
It is acid-leaching vanadium-extracted, need to carry out pelletization treatment, it is cumbersome, with certain limitation.
Therefore, it is quite necessary to find a kind of roasting process need not plus residue or other inert excipients, without the need for pelletizing, no
The higher Leaching of Vanadium from Vanadium slag method of sizing and V leaching rate.
The content of the invention
The invention aims to overcome the drawbacks described above of presence of the prior art, there is provided a kind of roasting process need not
Plus residue or other inert excipients, without the need for the higher Leaching of Vanadium from Vanadium slag method of pelletizing, not sizing and V leaching rate.
To achieve these goals, the present invention provides a kind of method of Leaching of Vanadium from Vanadium slag, and the method is comprised the following steps：(1)
Vanadium slag, calcium source, gas generation agent and water are mixed, compound is obtained；(2) compound is carried out the first intensification roasting and second liter successively
Warm roasting, obtains vanadium bearing slag；(3) vanadium bearing slag is carried out, after cooling and break process, carrying out acid-leaching vanadium-extracted；Wherein, it is described
The condition of the first intensification roasting includes：Final temperature is 500-650 DEG C, and the time is 30-60min；The second intensification roasting
Condition includes：Final temperature is 800-900 DEG C, and the time is 60-120min.
The present inventor has found that in research process gas generation agent and water can form a kind of wadding during mixing
Condensate, the flocculate can play a part of materials from bonding.In addition, obtain after vanadium slag, calcium source, gas generation agent and water are mixed
During compound carries out the first intensification roasting, as temperature is increased to 120 DEG C or so from room temperature, part water starts evaporation,
Start release from compound, so that compound produces micro-pore；Next, the continuation with temperature is raised, periphery is empty
Oxygen in gas brings it about reaction by above-mentioned micro-pore into compound；Further, gas generation agent mixes product with water
Raw flocculate also starts failure and in temperature-rise period by calcination, discharges in gaseous form, so as to cause compound the
Secondary generation hole, therefore, the oxygen in peripheral air further can be entered in compound by the hole that second produces
Portion and bring it about reaction so that there is slight cementation in compound, so as to obtain many spaces and loose material.Enter one
Step ground, by the second intensification roasting, makes the vanadium in compound be substantially oxidized and form the acid-soluble vanadium of high price, is beneficial to follow-up
Acid-leaching vanadium-extracted process.Therefore, there is the Leaching of Vanadium from Vanadium slag method that the present invention is provided roasting process residue or other inertia need not be added auxiliary
Material, without the need for the higher advantage of pelletizing, not sizing and V leaching rate, with good prospects for commercial application.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that described herein concrete
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
Herein the end points and any value of disclosed scope is not limited to the accurate scope or value, these scopes or
Value should be understood to comprising the value for being close to these scopes or value.For numerical range, between the endpoint value of each scope, respectively
Between the endpoint value of individual scope and single point value, and individually one or more can be obtained with combination with one another between point value
New numerical range, these numerical rangies should be considered concrete open herein.
The present invention provides a kind of method of Leaching of Vanadium from Vanadium slag, and the method is comprised the following steps：
(1) vanadium slag, calcium source, gas generation agent and water are mixed, obtains compound；
(2) compound is carried out the first intensification roasting and the second intensification roasting successively, obtains vanadium bearing slag；
(3) vanadium bearing slag is carried out, after cooling and break process, carrying out acid-leaching vanadium-extracted；
Wherein, the condition of the first intensification roasting includes：Final temperature is 500-650 DEG C, and the time is 30-60min；Institute
The condition for stating the second intensification roasting includes：Final temperature is 800-900 DEG C, and the time is 60-120min.
According to the present invention, in step (1), the vanadium slag is with V2O5Use of the consumption of meter with the calcium source in terms of calcium constituent
The weight ratio of amount can be 1：0.3-1.5, preferably 1：0.5-1.
According to the present invention, in step (1), the calcium source can be the various materials that can provide calcium ion, for example, institute
It can be calcium oxide and/or Calcium Carbonate to state calcium source, it is preferable that the calcium source is calcium oxide and Calcium Carbonate.
In situations where it is preferred, the calcium source is calcium oxide and Calcium Carbonate, and the calcium oxide and the Calcium Carbonate are rubbed
You are than being 1：0.1-10, preferably 1：0.1-6.
According to the present invention, in step (1), relative to the vanadium slag of 100g, the consumption of the gas generation agent can be
0.05-0.5g, preferably 0.05-0.2g；The consumption of the water can be 1-10mL, preferably 1-5mL.
According to the present invention, the gas generation agent can in polyacrylamide, ammonium carbonate, ammonium hydrogen carbonate and Polyethylene Glycol extremely
Few one kind, preferably polyacrylamide and/or Polyethylene Glycol.
According to the present invention, to the source of vanadium slag, there is no particular limitation, can be the conventional selection of this area, for example, vanadium
The source of slag can be at least one in vanadium extraction by converter blowing vanadium slag, the slag containing vanadium and/or the dead catalyst containing vanadium；Preferred
In the case of, the content of the Vanadium in Vanadium Residue element is more preferably 5-20 weight % more than or equal to 5 weight %, further preferably
For 5.2-8.5 weight %.
In situations where it is preferred, the granularity of the vanadium slag is less than or equal to 80 mesh and granularity containing in the vanadium slag of 100-200 mesh
Amount is more than 80 weight %.
In the present invention, granularity refers to the size of granule, and specifically, the granularity of spheroidal particle can use the straight of spheroidal particle
Footpath is representing；The granularity of aspherical particle can be used as this by the diameter of a certain spheroidal particle with which with identical behavior
The equivalent diameter of grain is representing.In the present invention, " mesh " refers to the empty eye number on screen cloth per square inch, and for example, 200 mesh are
The eyelet that finger is gone up per square inch is 200, and mesh number is higher, and eyelet is more, and then, particle diameter is less.Therefore, " mesh " is while be used for
Expression can be by the particle diameter of the granule (such as vanadium slag) of screen cloth.In the present invention, 200 mesh=74 micron.
According to the present invention, in step (1), there is no particular limitation for condition of the present invention to the mixing, for example, described
The condition of mixing can include：Temperature is 20-60 DEG C, and the time is 30-90min；Preferably, temperature is 20-40 DEG C, and the time is
30-60min。
In the present invention, in step (1), there is no particular limitation for mode of the present invention to the mixing, as long as material
Can be with mix homogeneously, for example, the mixing can be carried out under conditions of stirring, and the present invention does not have to the condition of the stirring
There is special restriction, can be the conventional selection of this area, as long as material mix homogeneously can be made, it is for instance possible to use
The mode of magnetic agitation, mechanical agitation or Gas Stirring.In situations where it is preferred, the speed of the stirring is 120-300rpm.
In the present invention, in step (1), the order by merging to each material is not particularly required, it is preferable that first by hair engaging aperture
Agent and water mixing, then the material for obtaining is mixed with vanadium slag and calcium source.
According to the present invention, in step (2), compound is carried out the first intensification roasting and the second intensification roasting successively, is obtained
To vanadium bearing slag, wherein, the condition of the first intensification roasting can include：Final temperature is 500-650 DEG C, and the time is 30-
60min；The condition of the second intensification roasting can include：Final temperature is 800-900 DEG C, and the time is 60-120min.
In the present invention, to the initial temperature of the first intensification roasting, there is no particular limitation, can be by step (1)
The temperature of the compound for obtaining, it is generally the case that the initial temperature of the first intensification roasting can be 20-40 DEG C.In addition, this
Also there is no particular limitation for heating rate of the invention to the first intensification roasting, as long as can be in the first intensification roasting
The final temperature (that is, 500-650 DEG C) of the first intensification roasting, for example, institute are warming up in time (that is, 30-60min)
The heating rate for stating the first intensification roasting can be 10-21 DEG C/min.
In the present invention, to the initial temperature of the second intensification roasting, there is no particular limitation, can be first liter of Jing
The temperature of the material that warm roasting is obtained, for example, the initial temperature of the second intensification roasting can be 500-650 DEG C.In addition, this
Also there is no particular limitation for heating rate of the invention to the second intensification roasting, as long as can be in the second intensification roasting
The final temperature (that is, 800-900 DEG C) of the second intensification roasting is warming up in time (that is, 60-120min), for example,
The heating rate of the second intensification roasting can be 8-15 DEG C/min.
The present invention one preferred embodiment in, the condition of the first intensification roasting includes：Initial temperature is
20-40 DEG C, final temperature is 500-650 DEG C, and the time is 30-60min；The condition of the second intensification roasting includes：Initial temperature
Spend for 500-650 DEG C, final temperature is 800-900 DEG C, and the time is 60-120min.
In addition, inventor is surprised to find that in research process：Obtain after vanadium slag, calcium source, gas generation agent and water are mixed
Compound carry out the first intensification roasting during, as temperature is increased to 120 DEG C or so from room temperature, part water start steam
Send out, start release from compound, so that compound produces micro-pore；Next, the continuation with temperature is raised, periphery
Oxygen in air brings it about reaction by above-mentioned micro-pore into compound；Further, gas generation agent is mixed with water
The flocculate of generation also starts to fail and by calcination in temperature-rise period, discharges in gaseous form, so as to cause compound
Produce hole for second, therefore, the hole that the oxygen in peripheral air further can be produced by second enters compound
It is internal and bring it about reaction so that the slight cementation of compound generation, so as to obtain many spaces and loose material.Enter
One step ground, by the second intensification roasting, makes the vanadium in compound be substantially oxidized and form the acid-soluble vanadium of high price, is beneficial to follow-up
Acid-leaching vanadium-extracted process.
According to the present invention, in step (3), it is described cooling allow cool down after vanadium bearing slag temperature be 200-400
℃。
According to the present invention, in step (3), the break process causes the particle diameter≤30mm of vanadium bearing slag, preferably 3-
20mm.There is no particular limitation to the broken mode for the present invention, as long as crush can dried compound, example
Such as, it is possible to use Glass rod turns over broken, or is smashed using hammer, or broken using disintegrating machine commonly used in the art
It is broken.Wherein, the particle diameter of the material can be controlled by way of broken.In the present invention, particle diameter refers to the diameter of granule, tool
Body ground, the particle diameter of spheroidal particle are the diameter of spheroidal particle；The particle diameter of aspherical particle is have a certain of identical behavior with which
The diameter of spheroidal particle.
According to the present invention, in step (3), the acid-leaching vanadium-extracted condition can be the conventional selection of this area, for example,
The acid-leaching vanadium-extracted condition can include：PH value is 2.4-4, and temperature is 30-60 DEG C, and the time is 30-60min.
In the present invention, it is described it is acid-leaching vanadium-extracted during, it is possible to use dilute acid for adjusting pH value be 2.4-4, wherein, institute
State the conventional selection that diluted acid can be this area, for example, the diluted acid can in dilute sulfuric acid, dilute hydrochloric acid and dust technology at least
It is a kind of.The present invention to it is described it is acid-leaching vanadium-extracted during the consumption of diluted acid there is no particular limitation, can be the routine of this area
Select, as long as being leached the vanadium in material completely, for example, for the material of 100g, it is possible to use 200-500mL's
Diluted acid carries out leaching vanadium extraction.
The present invention it is a kind of preferred embodiment in, the method comprising the steps of：
A gas generation agent and water are mixed by ()；
B () will be mixed with vanadium slag and calcium source by the material that step (a) is obtained, obtain compound；
C () compound is carried out the first intensification roasting and the second intensification roasting successively, obtain vanadium bearing slag；
D vanadium bearing slag is carried out, after cooling and break process, carrying out acid-leaching vanadium-extracted by ()；
Wherein, the condition of the first intensification roasting includes：Final temperature is 500-650 DEG C, and the time is 30-60min；Institute
The condition for stating the second intensification roasting includes：Final temperature is 800-900 DEG C, and the time is 60-120min.In the preferred implementation
In, cooling and other conditions such as break process can be with as it was previously stated, will not be described here.
Hereinafter will be described the present invention by embodiment.
In the following Examples and Comparative Examples, the leaching rate of the content and vanadium of v element is obtained using following methods：
1) concentration of v element in vanadium leachate is analyzed using Atomic Emission Spectrometer AES (ICP)；
2) after leaching rate %=water logging vanadium extraction in leachate the content/Vanadium in Vanadium Residue element of v element content × 100%.
Compound used in following examples and comparative example can be obtained by conventional commercially available mode.
Embodiment 1
The method that the present embodiment is used for the Leaching of Vanadium from Vanadium slag for illustrating that the application is provided.
The content of vanadium slag 100g, wherein v element (is converted to V for 5.2 weight %2O5Content be 9.28 weight %), grain
Spend all to cross 80 mesh (wherein 85% belongs to -120 mesh of mesh～+200).
By vanadium slag and Calcium Carbonate 12.26g (purity of Calcium Carbonate be 98 weight %, granular, technical grade) mixing, then by poly- third
Mix 30min at 20 DEG C in the mixture of acrylamide 0.05g and water 1mL mixing incorporation vanadium slag and Calcium Carbonate, obtain compound.
Compound being entered into roasting apparatus, 650 DEG C being warming up to from 20 DEG C first, the heating-up time is 30min；900 are warming up to from 650 DEG C again
DEG C, the heating-up time is 60min, obtains vanadium bearing slag (roasting process is without the viscous wall of material).Then vanadium bearing slag is cooled to into 200
DEG C, into crusher in crushing so that broken particle diameter≤30mm, Jing 200mL dilute sulfuric acids are leached, and pH value is 4, are leached at 30 DEG C
60min, filters, and washing, wash water are integrated with leachate, obtains vanadium leachate 295mL altogether.
Jing is checked, and in vanadium leachate, the concentration of v element is 16.88g/L, is computed drawing that the leaching rate of vanadium is
95.76%.
Embodiment 2
The method that the present embodiment is used for the Leaching of Vanadium from Vanadium slag for illustrating that the application is provided.
The content of vanadium slag 1000g, wherein v element (is converted to V for 8.5 weight %2O5Content be 15.2 weight %), grain
Spend all to cross 80 mesh (wherein 80% belongs to -100 mesh of mesh～+200).
By vanadium slag and Calcium Carbonate 221g (purity of Calcium Carbonate be 98 weight %, granular, technical grade), calcium oxide 21g (carbonic acid
The purity of calcium is 98 weight %, granular, technical grade) mixing, then polyacrylamide 1g and water 30mL mixing is mixed into vanadium slag and carbon
Mix 45min at 40 DEG C in sour calcium, the mixture of calcium oxide, obtain compound.Compound is entered into roasting apparatus, first from
40 DEG C are warming up to 600 DEG C, and the heating-up time is 45min；850 DEG C are warming up to from 650 DEG C again, the heating-up time is 90min, is obtained containing vanadium
Grog (roasting process is without the viscous wall of material).Then vanadium bearing slag is cooled to into 200 DEG C, into crusher in crushing so that broken kernel
Footpath≤30mm, Jing 2000mL dilute hydrochloric acid are leached, and pH value is 2.4, and 30min is leached at 60 DEG C, filter, and washing, wash water are integrated with
In leachate, vanadium leachate 3000mL is obtained altogether.
Jing is checked, and in vanadium leachate, the concentration of v element is 27.35g/L, is computed drawing that the leaching rate of vanadium is
96.53%.
Embodiment 3
The method that the present embodiment is used for the Leaching of Vanadium from Vanadium slag for illustrating that the application is provided.
The content of vanadium slag 100kg, wherein v element (is converted to V for 8.5 weight %2O5Content be 15.2 weight %), grain
Spend all to cross 80 mesh (wherein 80% belongs to -100 mesh of mesh～+200).
By vanadium slag and calcium oxide 19kg (purity of calcium oxide be 98 weight %, granular, technical grade), Calcium Carbonate 5.6kg (carbon
The purity of sour calcium be 98 weight %, granular, technical grade) mixing, then by polyacrylamide 0.2kg and water 5L mixing mix vanadium slag and
Mix 60min at 30 DEG C in Calcium Carbonate, the mixture of calcium oxide, obtain compound.Compound is entered into roasting apparatus, first
650 DEG C are warming up to from room temperature (25 DEG C), the heating-up time is 60min；900 DEG C are warming up to from 650 DEG C again, the heating-up time is
120min, obtains vanadium bearing slag (roasting process is without the viscous wall of material).Then vanadium bearing slag is cooled to into 400 DEG C, into disintegrating machine
It is broken so that broken particle diameter≤30mm, Jing 200L dust technologies are leached, and pH value is 3, and 45min is leached at 45 DEG C, are filtered, washing,
Wash water is integrated with leachate, obtains vanadium leachate 300L altogether.
Jing is checked, and in vanadium leachate, the concentration of v element is 27.65g/L, is computed drawing that the leaching rate of vanadium is
97.58%.
Embodiment 4
The method that the present embodiment is used for the Leaching of Vanadium from Vanadium slag for illustrating that the application is provided.
The content of vanadium slag 100g, wherein v element (is converted to V for 5.2 weight %2O5Content be 9.28 weight %), grain
Spend all to cross 80 mesh (wherein 85% belongs to -120 mesh of mesh～+200).
By vanadium slag and Calcium Carbonate 12.26g (purity of Calcium Carbonate be 98 weight %, granular, technical grade) mixing, then by poly- second
Mix 30min at 20 DEG C in the mixture of glycol 0.05g and water 1mL mixing incorporation vanadium slag and calcium oxide, obtain compound.Will
Compound enters roasting apparatus, is warming up to 500 DEG C from 20 DEG C first, and the heating-up time is 30min；800 are warming up to from 500 DEG C again
DEG C, the heating-up time is 60min, obtains vanadium bearing slag (roasting process is without the viscous wall of material).Then vanadium bearing slag is cooled to into 200
DEG C, into crusher in crushing so that broken particle diameter≤30mm, Jing 200mL dilute sulfuric acids are leached, and pH value is 4, are leached at 30 DEG C
60min, filters, and washing, wash water are integrated with leachate, obtains vanadium leachate 295mL altogether.
Jing is checked, and in vanadium leachate, the concentration of v element is 16.68g/L, is computed drawing that the leaching rate of vanadium is
94.63%.
Embodiment 5
The method that the present embodiment is used for the Leaching of Vanadium from Vanadium slag for illustrating that the application is provided.
Leaching of Vanadium from Vanadium slag is carried out according to method same as Example 1, wherein, except that, using the oxygen of identical weight
Changing calcium replaces Calcium Carbonate as calcium source, and roasting process does not observe that material glues wall.
Jing is checked, and in vanadium leachate, the concentration of v element is 16.90g/L, is computed drawing that the leaching rate of vanadium is
95.88%.
Comparative example 1
Leaching of Vanadium from Vanadium slag is carried out according to method same as Example 1, wherein, except that, polyacrylamide is not added,
Obtain vanadium leachate 295mL.
Jing is checked, and in vanadium leachate, the concentration of v element is 16.00g/L, is computed drawing that the leaching rate of vanadium is
90.75%.
Comparative example 2
Leaching of Vanadium from Vanadium slag is carried out according to method same as Example 1, wherein, except that, compound is entered into roasting
Equipment, is warming up to 650 DEG C from 20 DEG C of temperature first, and the heating-up time is 65min；900 DEG C are warming up to from 650 DEG C again, the heating-up time is
25min, obtains vanadium leachate 295mL.
Jing is checked, and in vanadium leachate, the concentration of v element is 16.31g/L, is computed drawing that the leaching rate of vanadium is
92.52%.
Comparative example 3
Leaching of Vanadium from Vanadium slag is carried out according to method same as Example 1, wherein, except that, compound is once roasted
Directly cooled down after burning, compound is warming up to into 650 DEG C from 20 DEG C into after roasting apparatus, the heating-up time is 30min, is obtained
Vanadium leachate 295mL.
Jing is checked, and in vanadium leachate, the concentration of v element is 13.21g/L, is computed drawing that the leaching rate of vanadium is
74.94%.
Comparative example 4
Leaching of Vanadium from Vanadium slag is carried out according to method same as Example 1, wherein, except that, compound is entered into roasting
Equipment, is warming up to 700 DEG C from 20 DEG C of temperature first, and the heating-up time is 30min；900 DEG C are warming up to from 700 DEG C again, the heating-up time is
60min, obtains vanadium leachate 295mL.
Jing is checked, and in vanadium leachate, the concentration of v element is 16.02g/L, is computed drawing that the leaching rate of vanadium is
90.89%.
Comparative example 5
Leaching of Vanadium from Vanadium slag is carried out according to method same as Example 1, wherein, except that, compound is entered into roasting
Equipment, is warming up to 450 DEG C from 20 DEG C first, and the heating-up time is 30min；800 DEG C are warming up to from 450 DEG C again, the heating-up time is
60min, obtains vanadium leachate 295mL.
Jing is checked, and in vanadium leachate, the concentration of v element is 16.05g/L, is computed drawing that the leaching rate of vanadium is
91.05%.
Embodiment 1-5 that the present invention is provided is compared with the result of comparative example 1-5 and is understood, the vanadium provided by the present invention
Slag extraction vanadium method can obtain higher V leaching rate, and there is the method roasting process residue or other inertia need not be added auxiliary
Material, without the need for pelletizing and the not advantage of sizing, with good prospects for commercial application.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means.In order to avoid unnecessary repetition, the present invention to it is various can
The compound mode of energy is no longer separately illustrated.
Additionally, combination in any between a variety of embodiments of the present invention, can also be carried out, as long as which is without prejudice to this
The thought of invention, which should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of method of Leaching of Vanadium from Vanadium slag, it is characterised in that the method is comprised the following steps：
(1) vanadium slag, calcium source, gas generation agent and water are mixed, obtains compound；
(2) compound is carried out the first intensification roasting and the second intensification roasting successively, obtains vanadium bearing slag；
(3) vanadium bearing slag is carried out, after cooling and break process, carrying out acid-leaching vanadium-extracted；
Wherein, the condition of the first intensification roasting includes：Final temperature is 500-650 DEG C, and the time is 30-60min；Described
The condition of two intensification roastings includes：Final temperature is 800-900 DEG C, and the time is 60-120min.
2. method according to claim 1, wherein, in step (1), the vanadium slag is with V2O5The consumption of meter and the calcium
The weight ratio of the consumption that source is counted with calcium constituent is as 1：0.3-1.5, preferably 1：0.5-1.
3. method according to claim 1, wherein, in step (1), relative to the vanadium slag of 100g, the gas generation agent
Consumption is 0.05-0.5g, preferably 0.05-0.2g；The consumption of the water is 1-10mL, preferably 1-5mL.
4. the method according to any one in claim 1-3, wherein, in step (1), the calcium source is calcium oxide
And/or Calcium Carbonate, preferably calcium oxide and Calcium Carbonate；The gas generation agent is polyacrylamide, ammonium carbonate, ammonium hydrogen carbonate and poly- second
At least one in glycol, preferably polyacrylamide and/or Polyethylene Glycol.
5. the method according to any one in claim 1-3, wherein, the content of the Vanadium in Vanadium Residue element be more than etc.
In 5 weight %；Preferably, the granularity of the vanadium slag is less than or equal to the content of 80 mesh and granularity in the vanadium slag of 100-200 mesh 80
It is more than weight %.
6. method according to claim 1, wherein, in step (1), the condition of the mixing includes：Temperature is 20-60
DEG C, the time is 30-90min；Preferably, temperature is 20-40 DEG C, and the time is 30-60min.
7. method according to claim 1, wherein, in step (3), the cooling causes the temperature of vanadium bearing slag after cooling
Spend for 200-400 DEG C.
8. method according to claim 1, wherein, in step (3), the break process causes the particle diameter of vanadium bearing slag
≤30mm。
9. method according to claim 1, wherein, in step (3), the acid-leaching vanadium-extracted condition includes：PH value is
2.4-4, temperature are 30-60 DEG C, and the time is 30-60min.
10. the method according to any one in claim 1-9, wherein, the method comprising the steps of：
A gas generation agent and water are mixed by ()；
B () will be mixed with vanadium slag and calcium source by the material that step (a) is obtained, obtain compound；
C () compound is carried out the first intensification roasting and the second intensification roasting successively, obtain vanadium bearing slag；
D vanadium bearing slag is carried out, after cooling and break process, carrying out acid-leaching vanadium-extracted by ()；
Wherein, the condition of the first intensification roasting includes：Final temperature is 500-650 DEG C, and the time is 30-60min；Described
The condition of two intensification roastings includes：Final temperature is 800-900 DEG C, and the time is 60-120min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611050754.3A CN106544514A (en) | 2016-11-25 | 2016-11-25 | A kind of method of Leaching of Vanadium from Vanadium slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611050754.3A CN106544514A (en) | 2016-11-25 | 2016-11-25 | A kind of method of Leaching of Vanadium from Vanadium slag |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106544514A true CN106544514A (en) | 2017-03-29 |
Family
ID=58395010
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611050754.3A Pending CN106544514A (en) | 2016-11-25 | 2016-11-25 | A kind of method of Leaching of Vanadium from Vanadium slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106544514A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842054A (en) * | 2018-08-21 | 2018-11-20 | 成渝钒钛科技有限公司 | The method of roasting and roasting clout of a kind of high calcium slag and application |
| CN112195347A (en) * | 2020-09-27 | 2021-01-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of calcified vanadium slag |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4666512A (en) * | 1985-04-18 | 1987-05-19 | U.S. Vanadium Corp. | Method for recovering vanadium from vanadium-containing ore |
| CN103667710A (en) * | 2013-12-04 | 2014-03-26 | 四川省川威集团有限公司 | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag |
| CN104152673A (en) * | 2014-07-31 | 2014-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Calcification roasting method of vanadium/phosphorus-containing material |
| CN104178639A (en) * | 2014-07-31 | 2014-12-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from chrome vanadium slag |
-
2016
- 2016-11-25 CN CN201611050754.3A patent/CN106544514A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4666512A (en) * | 1985-04-18 | 1987-05-19 | U.S. Vanadium Corp. | Method for recovering vanadium from vanadium-containing ore |
| CN103667710A (en) * | 2013-12-04 | 2014-03-26 | 四川省川威集团有限公司 | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag |
| CN104152673A (en) * | 2014-07-31 | 2014-11-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Calcification roasting method of vanadium/phosphorus-containing material |
| CN104178639A (en) * | 2014-07-31 | 2014-12-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium from chrome vanadium slag |
Non-Patent Citations (1)
| Title |
|---|
| 洛光林主编: "《印刷包装材料》", 31 March 2002, 中国轻工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108842054A (en) * | 2018-08-21 | 2018-11-20 | 成渝钒钛科技有限公司 | The method of roasting and roasting clout of a kind of high calcium slag and application |
| CN112195347A (en) * | 2020-09-27 | 2021-01-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of calcified vanadium slag |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103194603B (en) | Preparation method of high-purity vanadium pentoxide | |
| CN100359025C (en) | Method of extracting vanadium pentoxide from vanadium ore | |
| CN107058764B (en) | A method of recycling vanadium from corundum slag | |
| CN109913660A (en) | A method of rich vanadium richness iron charge is prepared using v-bearing steel slag | |
| CN105776333A (en) | Preparation method of vanadium pentoxide | |
| CN103031445A (en) | Method for effectively roasting and leaching vanadium slag | |
| JP5862919B2 (en) | Nickel oxide fine powder and method for producing the same | |
| CN111705226B (en) | Method for removing impurities from high-titanium slag | |
| CN107267766A (en) | A kind of method of Selective Separation vanadium, titanium, iron from modified vanadium slag | |
| CN106544514A (en) | A kind of method of Leaching of Vanadium from Vanadium slag | |
| CN112410561A (en) | Treatment method for neutralizing gypsum slag in vanadium precipitation wastewater | |
| JP5168070B2 (en) | Nickel oxide powder and method for producing the same | |
| CN109402380A (en) | A method of the vanadium extraction from vanadium slag | |
| US4069295A (en) | Treating raw materials containing titanium components | |
| CN102220499B (en) | Roasting-leaching method of fine vanadium slags | |
| JP6159306B2 (en) | Nickel oxide powder | |
| CN110306065A (en) | A kind of method that vanadium slag prepares ammonium metavanadate | |
| JP5733101B2 (en) | Method for producing nickel oxide powder | |
| CN106544516A (en) | A kind of method of Leaching of Vanadium from Vanadium slag | |
| CN106006701B (en) | A kind of preparation method of micrometer-submicrometer grade RE oxide powder | |
| RU2390572C1 (en) | Method of processing quartz-leucoxene concentrates | |
| CN107663585A (en) | The method of low-quality vanadium slag upgrading | |
| CN111378846A (en) | Method for extracting vanadium from manganese vanadium slag prepared based on vanadium blowing of converter | |
| CN109913661A (en) | A method of from extraction sulphur and vanadium in desulfurization slag containing vanadium | |
| RU2793681C2 (en) | Method for extracting vanadium from vanadium slag by roasting with a composite based on calcium and manganese |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170329 |
|
| RJ01 | Rejection of invention patent application after publication |