CN107354304B - A kind of method of Porous Medium Adsorption separation Vanadium in Vanadium Residue resource - Google Patents
A kind of method of Porous Medium Adsorption separation Vanadium in Vanadium Residue resource Download PDFInfo
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- CN107354304B CN107354304B CN201710610645.0A CN201710610645A CN107354304B CN 107354304 B CN107354304 B CN 107354304B CN 201710610645 A CN201710610645 A CN 201710610645A CN 107354304 B CN107354304 B CN 107354304B
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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
- 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
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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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- 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
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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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
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Abstract
The invention discloses a kind of methods of Porous Medium Adsorption separation Vanadium in Vanadium Residue resource, belong to metallurgical cinder solid-liquid two-phase laminated flow field.This method comprising the following three steps: step 1: the preparation of porous media board；Step 2: 1500~1550 DEG C of melting vanadium slags are cooled to 1200~1250 DEG C with the cooling rate less than 2 DEG C/min, the heat treatment for obtaining the spinelle of vanadium iron containing solid phase melts vanadium slag；Step 3: porous media board absorption slag is carried out to the heat treatment vanadium slag and completes to be separated by solid-liquid separation, obtains smart vanadium slag and tailings of the vanadium iron Spinel grade 70~90%.The present invention utilizes the melting slag phase in porous media board capillary force absorption heat treatment vanadium slag, realize the separation and concentration of heat treatment Vanadium in Vanadium Residue hercynite solid phase, the porous media board that the vanadium iron spinelle essence vanadium slag isolated by porous media directly as wet process vanadium extraction and the raw material of pyrometallurgical smelting vanadium iron, can adsorb tailings can be used as the raw material of production cement.
Description
Technical field
The invention belongs to metallurgical cinder solid-liquid two-phase laminated flow fields, and in particular to a kind of to separate vanadium using Porous Medium Adsorption
The method of vanadium resource in slag.
Background technique
Vanadium resource is most of from vanadium titano-magnetite.Vanadium titano-magnetite enters blast furnace process after ore dressing, obtains titanium slag
With the molten iron containing vanadium 0.3% or so, vanadium-bearing hot metal is obtained by bessemerizing oxidation containing 5~15%V2O5Vanadium slag.
Currently, producing vanadium or V using v-bearing steel slag2O5Main method be that broken, oxidizing roasting, leaching remove using vanadium slag
Intermediate product ammonium vanadate is obtained by filtration in miscellaneous, precipitation, and ammonium vanadate obtains different vanadium products through subsequent processing again.Vanadium in Vanadium Residue grade with
Phase structure etc. directly determines vanadium recovery and the cost recovery of the technique.
Vanadium slag is mainly mingled with phase composition by Spinel, Binder Phase and part, and wherein to be that vanadium slag is main contain Spinel
The object phase crystallized out earliest in vanadium object phase and vanadium extracting process；Binder Phase is mainly silicate phase, last in vanadium extracting process
Solidification, is wrapped in the surface of spinelle.There is very the recovery rate of vanadium when the object phase composition of vanadium slag and structure are to the oxidizing roasting of vanadium slag
Big to influence, spinel crystal particle is bigger, and silicate phase is fewer, and exposed vanadium iron spinelle specific surface area is bigger after being crushed, then
More be conducive to the oxidation and recycling of vanadium slag when roasting.
It is above-mentioned analysis shows, realize effective enrichment of the phase containing vanadic spinel in vanadium slag, be the existing vanadium slag treatment process of optimization
Key, and solve the effective ways of low-grade vanadium slag recycling vanadium resource.ZL201310416429.4 proposes to use hypergravity
The method of method separation and concentration Vanadium in Vanadium Residue resource, this method adopt heat treatment vanadium slag under the conditions of high temperature (1200~1300 DEG C)
It is handled with hypergravity, it is high to hypergravity equipment requirement, it there is no related industries equipment at present.There are hypergravities for this method simultaneously
In treatment process, liquid vanadium slag is set in the hidden danger in centrifugation equipment, will lead to solid containing vanadic spinel in hypergravity separation vanadium slag
It can not mutually carry out.
Summary of the invention
In view of the deficiency of the prior art, the technical problem to be solved in the present invention is to provide one kind efficiently to connect
Concentration and separation phase containing vanadic spinel in continuous slave vanadium slag mentions to reduce influence of the Binder Phase to vanadium extraction production efficiency in vanadium slag
High product V2O5The processing method of recovery rate.
In order to solve the above technical problems, the present invention is achieved by the following technical programs.
A kind of method of Porous Medium Adsorption separation Vanadium in Vanadium Residue resource of the present invention, specifically includes the following steps:
(1) preparation of porous media board
Quick lime or lime stone are sieved after crushing, obtain particle of the size between 10~60 mesh, then through briquetting at
Type obtains thick porous media board, and dielectric-slab is heated to 600~1200 DEG C in heating furnace and is kept the temperature；The porous media plate thickness
Degree is 60~150 millimeters, and aperture is 30~80 microns.
Or sieve quick lime or lime stone after crushing, particle of the size between 10~60 mesh is obtained, then through pressing
Formation of lots obtains the thin porous media board of room temperature, spare in room temperature state；The porous media board is with a thickness of 20~60 millimeters, aperture
It is 60~100 microns.
(2) in vanadium slag the Selective separation-out of rich vanadium phase with grow up
1500~1550 DEG C of melting vanadium slags are cooled to 1200~1250 DEG C with the cooling rate less than 2 DEG C/min, heat preservation
20~40 minutes, the heat treatment for obtaining the spinelle of vanadium iron containing solid phase melted vanadium slag.
(3) adsorbing separation of porous media board
Using 3~10 drainage trough shunting devices, the vanadium slag that solid phase vanadium iron spinelle is precipitated in step (2) is uniformly quickly fallen
Porous media plate surface to step (1) preparation carries out capillary absorption, and after waiting vanadium slags to solidify, porous media plate surface is Vanadium Concentrationin
The smart vanadium slag of hercynite phase, porous media intralamellar part are absorption melting slag phase and the tailings for being cooled to solid phase.
Further, the fluxing agent no more than its total weight 3% is added in step (2) the melting vanadium slag before cooling.
Further, the fluxing agent is sodium carbonate or boric acid.
Further, the porous media board of the absorption tailings can be directly used for the raw material of manufacture of cement.
Further, the smart vanadium slag of the Vanadium Concentrationin hercynite phase can be directly used for wet process vanadium extraction or pyrometallurgical smelting vanadium iron
Raw material.
Compared with prior art, the present invention has following technical effect that
1, the melting slag phase in heat treatment vanadium slag is adsorbed using porous media board capillary force, effectively realizes heat treatment vanadium
The separation and concentration of vanadium iron spinelle solid phase in slag；
2, vanadium slag sensible heat and latent heat are made full use of, control cooling velocity completes the precipitation the controlling growth of vanadium iron spinelle, point
From the raw material that gained vanadium iron spinelle can be used as vanadium iron smelting and wet process vanadium extraction；
3, using cheap quick lime or lime stone as Porous Medium Adsorption plate material, after the completion of adsorbing separation, tail is adsorbed
The porous media board of slag can be directly used for cement producting material；
4, the continuous batch processing of heat treatment vanadium slag, process flow can be achieved in Porous Medium Adsorption separation of the present invention
It is short, technological operation is simple, environmental pollution is small, can effectively solve the problem of complex utilization of all kinds of resources in vanadium slag.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 is porous media board of the present invention preparation and treatment process schematic diagram.
Fig. 3 is porous media board adsorbing separation vanadium slag process schematic representation of the present invention.
Specific embodiment
As shown in Figures 1 to 3, the specific embodiment of Porous Medium Adsorption separation Vanadium in Vanadium Residue resource allocation method of the present invention includes
The following three steps:
(1) preparation and processing of porous media board
Preparation method one: quick lime or lime stone are sieved after crushing, obtain particle of the size between 10~60 mesh,
Again through compound stalk forming, thick porous media board is obtained, dielectric-slab is heated to 600-1200 DEG C in heating furnace and is kept the temperature.This is porous
Media plate thickness are 60~150 millimeters, and aperture is 30~80 microns.
Preparation method two: quick lime or lime stone are sieved after crushing, obtain particle of the size between 10~60 mesh,
Again through compound stalk forming, the thin porous media board of room temperature is obtained, it is spare in room temperature state.The porous media board is with a thickness of 20~60 millis
Rice, aperture are 60~100 microns.
(2) in vanadium slag the Selective separation-out of rich vanadium phase with grow up
To guarantee the efficient absorption separation containing vanadium slag, it is necessary first to measure analysis with temperature to vanadium slag ingredient is come out of the stove.
By melting vanadium slag ingredient real-time detection, FeO, SiO in vanadium slag are learnt rapidly2、V2O5Equal size, and examined using high-temperature measurement instrument
Survey clinker real time temperature.
According to the detection and analysis of ingredient and temperature, the fluxing dosage such as sodium carbonate, the boric acid being added in melting vanadium slag are determined, with
Adjust the relevant physical properties of vanadium slag.
Pretreated vanadium slag completes the Selective separation-out and length that rich vanadium phase is realized in cooling procedure control in electric furnace
Big heat treatment process.Equipment for Heating Processing is using graphite electrode heating adjustment and control slag slow cooling speed, using bottom blown gas
Stir evenly in-furnace slag temperature.1500~1550 DEG C of melting vanadium slags are cooled to 1200 with the cooling rate less than 2 DEG C/min
~1250 DEG C, 20~40 minutes are kept the temperature, the heat treatment for obtaining the spinelle of vanadium iron containing solid phase melts vanadium slag.
(3) adsorbing separation of porous media board
Using multiple drainage trough shunting devices, the vanadium slag of vanadium iron spinelle solid phase will be precipitated uniformly quickly down to porous media
Plate surface carries out capillary absorption, and after waiting vanadium slags to solidify, porous media plate surface is the smart vanadium slag of Vanadium Concentrationin hercynite phase, porous
Slag phase is melted for absorption inside dielectric-slab and is cooled to the tailings that can be used for cement producting material of solid phase.
Below in conjunction with specific embodiment, the invention will be further elaborated, but the present invention is not limited to following embodiments.
Embodiment 1
Certain v-bearing steel slag, through detecting, chemical composition are as follows: 6.8%CaO, 20.5%SiO2, 1.2%Al2O3,5.8%
MgO, 8.2%MnO, 3.5%TiO2,8.5%V2O5, Quan Tiewei 32.2%.It is the 1560 DEG C melting vanadium slag big by temperature
Heat treatment vanadium slag electric furnace is poured under gas atmosphere, topples over while being added the sodium carbonate fluxing agent of vanadium slag quality 1%, keeps the temperature 20 minutes,
Ensure that contents temperature is evenly distributed.1240 DEG C then are cooled to the cooling rate of 2 DEG C/min, keeps the temperature 30 minutes, is obtained containing solid
The heat treatment of phase vanadium iron spinelle melts vanadium slag.After vanadium slag is heat-treated, by gained vanadium slag down to adding by the way of drainage
Adsorbed in heat to 1000 DEG C of porous lime dielectric-slab, porous lime dielectric-slab with a thickness of 100 millimeters.Porous media board
After the completion of adsorbing separation, smart vanadium slag (the vanadium iron Spinel rich in vanadium iron spinelle being separated and recovered from above porous stone hawk
Grade is 75%), to be collected simultaneously the porous media board of absorption tailings.
Embodiment 2
Certain v-bearing steel slag, through detecting, chemical composition are as follows: 5.7%CaO, 21.4%SiO2,1.1%Al2O3,6.2%
MgO, 8.6%MnO, 3.8%TiO2,7.9%V2O5, Quan Tiewei 29.8%.It is the 1570 DEG C melting vanadium slag big by temperature
Heat treatment vanadium slag electric furnace is poured under gas atmosphere, topples over while being added the diboron trioxide fluxing agent of vanadium slag quality 0.8%, heat preservation 20
Minute, it is ensured that contents temperature is evenly distributed.1230 DEG C then are cooled to the cooling rate of 1.8 DEG C/min, 30 minutes is kept the temperature, obtains
The heat treatment melting vanadium slag of solid phase vanadium iron spinelle must be contained.After vanadium slag is heat-treated, by gained vanadium slag by the way of drainage
It is adsorbed on down to the porous lime dielectric-slab of room temperature with a thickness of 50 millimeters, after the completion of porous media board adsorbing separation, separation
And recycle and be rich in vanadium iron spinelle essence vanadium slag (vanadium iron Spinel grade is 79%) above porous stone hawk, it is collected simultaneously suction
The porous media board of attached tailings.
Embodiment 3
Certain v-bearing steel slag, through detecting, chemical composition are as follows: 6.3%CaO, 22.5%SiO2,1.5%Al2O3,5.4%
MgO, 7.2%MnO, 3.6%TiO2,7.6%V2O5, Quan Tiewei 30.4%.It is the 1540 DEG C melting vanadium slag big by temperature
Heat treatment vanadium slag electric furnace is poured under gas atmosphere, topples over while being added the diboron trioxide fluxing agent of vanadium slag quality 1.1%, heat preservation 20
Minute, it is ensured that contents temperature is evenly distributed.1250 DEG C then are cooled to the cooling rate of 2 DEG C/min, keeps the temperature 30 minutes, is obtained
The heat treatment of the spinelle of vanadium iron containing solid phase melts vanadium slag.After vanadium slag is heat-treated, gained vanadium slag is fallen by the way of drainage
To with a thickness of being adsorbed on 40 millimeters of the porous lime stone dielectric-slab of room temperature, after the completion of porous media board adsorbing separation, separate
And recycle and be rich in vanadium iron spinelle essence vanadium slag (vanadium iron Spinel grade is 85%) above porous stone hawk, it is collected simultaneously suction
The porous media board of attached tailings.
Claims (3)
1. a kind of method of Porous Medium Adsorption separation Vanadium in Vanadium Residue resource, it is characterised in that the following steps are included:
(1) preparation of porous media board
Quick lime or lime stone are sieved after crushing, obtain particle of the size between 10~60 mesh, then through compound stalk forming, obtain
To thick porous media board, dielectric-slab is heated to 600~1200 DEG C in heating furnace and is kept the temperature；The porous media board is with a thickness of 60
~150 millimeters, aperture is 30~80 microns；
Or quick lime or lime stone are sieved after crushing, obtain particle of the size between 10~60 mesh, then through briquetting at
Type obtains the thin porous media board of room temperature, spare in room temperature state；The porous media board is with a thickness of 20~60 millimeters, aperture 60
~100 microns；
(2) in vanadium slag the Selective separation-out of rich vanadium phase with grow up
1500~1550 DEG C of melting vanadium slags are cooled to 1200~1250 DEG C with the cooling rate less than 2 DEG C/min, heat preservation 20~
40 minutes, the heat treatment for obtaining the spinelle of vanadium iron containing solid phase melted vanadium slag；The melting vanadium slag is added before cooling is no more than it
The fluxing agent of total weight 3%；The fluxing agent is sodium carbonate or boric acid；
(3) adsorbing separation of porous media board
Using 3~10 drainage trough shunting devices, the vanadium slag of solid phase vanadium iron spinelle is precipitated uniformly quickly down to step in step (2)
Suddenly the porous media plate surface of (1) preparation carries out capillary absorption, and after waiting vanadium slags to solidify, porous media plate surface is enrichment vanadium iron point
The smart vanadium slag of spar phase, porous media intralamellar part are absorption melting slag phase and the tailings for being cooled to solid phase.
2. the method for Porous Medium Adsorption separation Vanadium in Vanadium Residue resource as described in claim 1, which is characterized in that the absorption
The porous media board of tailings can be directly used for the raw material of manufacture of cement.
3. the method for Porous Medium Adsorption separation Vanadium in Vanadium Residue resource as described in claim 1, which is characterized in that the enrichment
The smart vanadium slag of vanadium iron Spinel can be directly used for the raw material of wet process vanadium extraction or pyrometallurgical smelting vanadium iron.
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| CN110016376B (en) * | 2018-01-09 | 2020-12-22 | 宝山钢铁股份有限公司 | Utilization method of cold rolling magnetic filtration waste |
| CN112456550B (en) * | 2020-11-09 | 2022-06-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium slag with high acidolysis rate |
| CN115044738B (en) * | 2022-05-11 | 2023-07-04 | 东北大学 | Method for improving resource utilization level of stainless steel slag of electric furnace |
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