CN113088711A - Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium - Google Patents

Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium Download PDF

Info

Publication number
CN113088711A
CN113088711A CN202110357478.XA CN202110357478A CN113088711A CN 113088711 A CN113088711 A CN 113088711A CN 202110357478 A CN202110357478 A CN 202110357478A CN 113088711 A CN113088711 A CN 113088711A
Authority
CN
China
Prior art keywords
vanadium
vanadium slag
slag
blocks
roasting
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
Application number
CN202110357478.XA
Other languages
Chinese (zh)
Inventor
岳宏瑞
刘建兴
程功金
薛向新
张卫军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Northeastern University China
Original Assignee
Northeastern University China
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Northeastern University China filed Critical Northeastern University China
Priority to CN202110357478.XA priority Critical patent/CN113088711A/en
Publication of CN113088711A publication Critical patent/CN113088711A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/04Working-up slag
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/22Obtaining vanadium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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 invention relates to a method for extracting vanadium by roasting and acid leaching of a vanadium slag briquette in industrialized application, which comprises the following steps: s1, mixing and grinding the vanadium slag with the grain size of more than kilogram level and calcium peroxide to be less than 50 mu m to obtain powder; s2, briquetting the uniformly mixed vanadium slag and calcium peroxide powder under the pressure of 10-15 MPa to obtain a plurality of blocks; s3, roasting the blocks in air to oxidize trivalent vanadium in the blocks into pentavalent vanadium; and S4, grinding the blocks again to obtain clinker powder, and leaching the clinker powder in dilute sulfuric acid to obtain a vanadium-containing acid solution. According to the invention, calcium peroxide is adopted to replace traditional calcium salts such as calcium carbonate, and oxygen generated by thermal decomposition of calcium peroxide is utilized to more fully and completely oxidize low-valence vanadium in vanadium slag, so that the salt forming rate of vanadate and the recovery rate of vanadium extracted by acid leaching are improved. The method is particularly suitable for extracting vanadium from large-amount vanadium slag, reducing the vanadium slag and recycling the vanadium slag.

Description

Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium
Technical Field
The invention relates to the technical field of vanadium extraction from vanadium slag, in particular to a method for extracting vanadium from vanadium slag by briquetting roasting and acid leaching, which is industrially applied.
Background
The vanadium slag is a byproduct of smelting vanadium-titanium magnetite in a blast furnace-converter process, and contains a large amount of recyclable vanadium. Vanadium is mainly in low valence state (V) in the vanadium-chromium slag3+) With spinel phase (FeV)2O4) In (1). At present, the calcification roasting-leaching process is an effective vanadium slag treatment process. The main process is as follows: mixing vanadium slag with calcium salt (such as gypsum, calcium oxide or calcium carbonate), and calcining in air to obtain vanadium slag V3+Is oxidized to V5+Then the calcium vanadate reacts with calcium salt to generate calcium vanadate, and the roasted clinker is subjected to acid leaching to obtain vanadium-containing acid solution. The low-valence vanadium in the vanadium slag is oxidized to pentavalent vanadium and then subjected to salt formation (such as calcium vanadate) reaction so as to be leached in acid. The oxidation process of the vanadium slag is a limiting link of the roasting process and is also a control factor of the vanadium recovery rate in the actual production.
In actual production compared to laboratory studies, the recovery of vanadium was much lower (at least 10% lower) than in the laboratory despite similar calcination conditions. In a rotary kiln for actual production, the mass of vanadium slag can reach the level of several tons, and in a muffle furnace of a laboratory, the mass of the vanadium slag is generally between dozens of grams and 100 grams. Although the air atmosphere is the same in the rotary kiln and the muffle furnace in the macroscopic view, most of vanadium slag particles in the rotary kiln are in an oxygen-deficient state in the microscopic view, so that the overall oxidation rate of large-volume vanadium slag is too low. The laboratory vanadium slag is usually less than 100g, and the trivalent vanadium in the laboratory vanadium slag can be easily oxidized as completely as possible, while the oxidation difficulty is very high for large-amount vanadium slag. The amount of vanadium slag treated in a laboratory is very small, the vanadium slag can not be applied to the actual production process, and the recovery rate of vanadium in the actual production can be improved only by improving the integral oxidation rate of large-volume vanadium slag. In addition, the particle size and the air permeability of the vanadium slag in actual production are a pair of production parameters which are mutually restricted. When the vanadium slag particles are small, the vanadium slag can be fully oxidized during roasting, and further the recovery rate of vanadium is increased. However, when the vanadium slag particles are too small, the vanadium slag in the kiln is very densely stacked, the air permeability is very poor, and the oxidation rate of the vanadium slag located at the middle position of the stack is low, so that the overall oxidation rate of a large amount of vanadium slag in one batch is still low, and the recovery rate of vanadium is reduced.
Disclosure of Invention
Technical problem to be solved
In view of the defects and shortcomings of the prior art, the invention provides a method for extracting vanadium by roasting and acid leaching of vanadium slag briquettes for industrial application, which is used for improving the recovery rate of vanadium in large-volume vanadium slag in industrial application.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a method for extracting vanadium by roasting and acid leaching of vanadium slag briquettes for industrial application comprises the following steps:
s1, mixing and grinding the vanadium slag with the grain size of more than kilogram level and calcium peroxide to be less than 50 mu m to obtain powder;
s2, briquetting the uniformly mixed vanadium slag and calcium peroxide powder under the pressure of 10-15 MPa to obtain a plurality of blocks;
s3, roasting the blocks in air to oxidize trivalent vanadium in the blocks into pentavalent vanadium;
and S4, grinding the blocks again to obtain clinker powder, and leaching the clinker powder in dilute sulfuric acid to obtain a vanadium-containing acid solution.
Wherein, the kilogram level refers to that the amount of the vanadium slag is more than 1kg to hundreds of kg, even per ton. The method is different from laboratory pilot-scale tests, is used for reducing vanadium slag and extracting vanadium from a byproduct of smelting vanadium-titanium magnetite in a large-volume blast furnace/converter, and realizes resource utilization of the byproduct of smelting vanadium-titanium magnetite.
According to a preferred embodiment of the present invention, in S1, V is converted from vanadium in vanadium slag2O5V in calcium peroxide and vanadium slag2O5The molar ratio of (A) to (B) is 2-4: 1. The molar dosage of the calcium peroxide needs to ensure that powder particles of the vanadium slag can directly contact with the calcium peroxide, oxygen released by the calcium peroxide under the heating condition can directly oxidize adjacent low-valence vanadium, and the oxygen is produced in the process of outward overflowingThe green pores and channels promote the diffusion of oxygen in the air atmosphere to the central region of the interior of the block. Because the oxygen released by the calcium peroxide is quickly utilized, the overflowing amount of the oxygen is reduced, and the utilization rate of the oxygen in the calcium peroxide is improved, so that the V in the clinker is reduced2O5The calcium vanadate can be completely salified as far as possible. Too little calcium peroxide is not beneficial to improving the acid leaching rate of vanadium, too high calcium peroxide is not only wasteful, but also causes more calcium sulfate to be generated, the calcium sulfate is slightly soluble and flocculent in an aqueous solution, and more calcium vanadate is easily adsorbed, so that the vanadium yield is reduced.
According to a preferred embodiment of the present invention, in S1, it is ground to a particle size of 10 μm or less.
According to the preferred embodiment of the present invention, in S1, the particles are ground to 0.1-1 μm, and more preferably 200-300 nm.
According to a preferred embodiment of the present invention, in S1, the mixture of vanadium slag and calcium peroxide is ground using a high energy ball mill. The mixture of vanadium slag and calcium peroxide can be milled to about 200nm, even to below 100nm by using a high-energy ball mill.
Generally, the smaller the particle size, the more beneficial the improvement of the oxidation rate and the acid leaching recovery rate of vanadium in the vanadium slag, but the smaller the particle size, the fine dust is easily formed in the production process, the pollution to the production environment is easily caused, and the cost and equipment are considered, and the mixture of the vanadium slag and the calcium peroxide is preferably ground to 0.1-50 μm, and more preferably 0.1-10 μm.
According to a preferred embodiment of the present invention, in S2, the size of the block is 0.5 to 10cm, preferably 0.5 to 5 cm. The specific shape of the block is not limited, and the block can be a regular cylinder, a rectangular body, an ellipsoid, a sphere or an irregular solid shape. Wherein the pressure in the briquetting process is 10-15 MPa, and the pressing time is 5-7 min. Wherein the preferable pressure is 10MPa and the pressing time is 5 min.
Wherein the mass is preferably a mixture of irregularly shaped or different regularly geometrically shaped masses; so a large amount of vanadium slag blocks can be piled up in the kiln in a multi-gap manner, the air permeability is better, and the heat is easier to diffuse in the whole piled body, thereby being beneficial to the oxidation of the vanadium slag on the surface of the blocks.
The briquetting is prepared by filling materials in a die and continuously pressurizing for a preset time by adopting a pressure head which is adaptive to the inner cavity of the die, and the pressurizing size of the briquetting determines the compactness between vanadium slag powder particles and calcium peroxide powder particles in the block and the mass transfer and heat transfer properties in the block. The briquetting pressure is too small, the tightness between the vanadium slag particles and the calcium peroxide particles in the briquetting pressure is poor, the internal heat transfer property and the mass transfer property are poor, and trivalent vanadium in the vanadium slag is not favorably oxidized into high-valence vanadium. For example, the disk type pelletizer forms balls or agglomerates, the particles inside the pellets are loose, and the heat conductivity and the mass transfer are insufficient. The briquetting pressure should not be too big yet, and on the one hand, the compactness of block no longer changes along with pressure increase, and on the other hand, pressure is big to the equipment requirement height, and gives the increase cost of smashing once more and levigating after the calcination.
According to the preferred embodiment of the invention, in S3, the roasting temperature is 800-850 ℃, preferably 820-830 ℃, and the roasting time is 2-2.5 h, preferably 2 h. The roasting temperature has low requirement on equipment, and the energy consumption is saved.
According to the preferred embodiment of the invention, the concentration of the dilute sulfuric acid in S4 is 20-0%.
According to the preferred embodiment of the invention, in S4, the leaching temperature is 75-85 ℃.
According to the preferred embodiment of the invention, in S4, the acid leaching time is 2-2.5 h.
According to the treatment of the steps S1-S3, the clinker powder with high vanadium oxidation rate and small vanadium slag particle size can be obtained, so that the vanadium can be smoothly leached during leaching, and the high vanadium recovery rate is obtained.
(III) advantageous effects
The invention has the beneficial effects that:
(1) the method adopts calcium peroxide to replace the traditional calcium salts such as calcium sulfate, calcium carbonate and the like, utilizes oxygen generated by the thermal decomposition of the calcium peroxide to oxidize low-valence vanadium in vanadium slag, and then utilizes calcium oxide generated by the decomposition of the calcium peroxide and high-valence vanadium to produce calcium vanadate so as to be dissolved out in the acid leaching extraction process.
(2) The vanadium slag and the calcium peroxide are ground to be very fine, then the vanadium slag particles and the calcium peroxide particles are pressed into blocks under specific pressure, the vanadium slag particles and the calcium peroxide particles are fully mixed and closely contacted, the calcium peroxide with fine particle size can be rapidly decomposed and release oxygen, the oxygen is contacted with the peripheral vanadium slag particles and rapidly oxidizes low-valence vanadium into high-valence vanadium, the efficiency of oxidizing the vanadium slag by the calcium peroxide is improved, the probability of overflowing the oxygen generated by thermal decomposition of the calcium peroxide is reduced, and the recovery rate of the vanadium in the vanadium slag is improved.
(3) The pressed blocks are accumulated in the kiln, so that the transmission and the diffusion of ventilation and heat in the whole kiln are facilitated, the conflict between the granularity of the material and the overall ventilation property is solved, the low-valence vanadium on the surfaces of the blocks is effectively ensured to be fully oxidized into high-valence vanadium, and the recovery rate of the vanadium in the vanadium slag is improved.
Drawings
FIG. 1 is an EPMA image of a fired block of example 1 of the present invention.
FIG. 2 is data of vanadium leaching rates in examples 1 to 3 of the present invention.
FIG. 3 is data of vanadium leaching rates in examples 2, 4, 5 of the present invention and comparative example 5.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
In each of the following examples and comparative examples, the mass fraction of vanadium in an acid solution was measured using ICP-OES (inductively coupled plasma emission spectrometer).
Example 1
The embodiment provides a method for extracting vanadium from vanadium slag briquettes through roasting and acid leaching, which is applied industrially, and the method comprises the following steps:
s1, adding 330 g of CaO2The powder was mixed with 5kg of vanadium slag (containing V as the amount of vanadium)2O5Calculated as 8.34%) and mixed in a mixing bowl for 10 hours to mix the two powders uniformly. And (3) ball-milling the mixed powder in a high-energy ball mill for 10 hours to ensure that the particle size of the powder is 200-400 nm.
And S2, pressing the mixture into blocks in a stainless steel die with the inner diameter of 3cm, wherein the pressure in the pressing process is 10MPa, and the pressing time is 5 min. After demoulding, a block with a diameter of 3cm and a thickness of about 1cm is obtained.
And S3, raising the temperature of the muffle furnace to 800 ℃, keeping the temperature constant, and putting the block in the S2 into the muffle furnace to start roasting. After keeping the temperature for 2h, the block is taken out and rapidly cooled in the air. The block was cut in the radial direction and the cut surface was polished smooth using sandpaper. Sections were characterized using EPMA, resulting in EPMA images of the mass shown in fig. 1.
S4, crushing the roasted blocks in a sampling machine for 120S to obtain clinker powder, and leaching the clinker powder for 2h at 80 ℃ in 25% dilute sulfuric acid. The vanadium content in the acid leachate was measured and the recovery rate was calculated to be 77% in combination with the vanadium content in the vanadium slag (first point on the left as shown in fig. 2).
Example 2
The embodiment provides a method for extracting vanadium from vanadium slag briquettes through roasting and acid leaching, which is applied industrially, and the method comprises the following steps:
s1, adding 500 g of CaO2The powders were mixed with 5kg of vanadium slag and mixed in a mixing tank for 10h to mix the two powders uniformly. And (3) ball-milling the mixed powder in a high-energy ball mill for 10 hours to ensure that the particle size of the powder is 200-400 nm.
And S2, pressing the mixture into blocks in a stainless steel die with the inner diameter of 3cm, wherein the pressure in the pressing process is 10MPa, and the pressing time is 5 min. After demoulding, a block with a diameter of 3cm and a thickness of about 1cm is obtained.
And S3, raising the temperature of the muffle furnace to 800 ℃, keeping the temperature constant, and putting the block in the S2 into the muffle furnace to start roasting. After keeping the temperature for 2h, the block is taken out and rapidly cooled in the air.
S4, crushing the roasted blocks in a sampling machine for 120S to obtain clinker powder, and leaching the clinker powder in 25% dilute sulfuric acid at 80 ℃ for 2 h. The vanadium content in the acid leachate was measured and the recovery rate was calculated to be 79% in combination with the vanadium content in the vanadium slag (middle point shown in fig. 2, 3).
Example 3
The embodiment provides a method for extracting vanadium from vanadium slag briquettes through roasting and acid leaching, which is applied industrially, and the method comprises the following steps:
s1, adding 661 g of CaO2The powders were mixed with 5kg of vanadium slag and mixed in a mixing tank for 10h to mix the two powders uniformly. The mixed powder is put into a high-energy ball millGrinding for 10 hours to ensure that the particle size of the powder is 200-400 nm.
And S2, pressing the mixture into blocks in a stainless steel die with the inner diameter of 3cm, wherein the pressure in the pressing process is 10MPa, and the pressing time is 5 min. After demoulding, a block with a diameter of 3cm and a thickness of about 1cm is obtained.
And S3, raising the temperature of the muffle furnace to 800 ℃, keeping the temperature constant, and putting the block in the S2 into the muffle furnace to start roasting. After keeping the temperature for 2h, the block is taken out and rapidly cooled in the air.
S4, crushing the roasted blocks in a sampling machine for 120S to obtain clinker powder, and leaching the clinker powder in 25% dilute sulfuric acid at 80 ℃ for 2 h. The vanadium content in the acid leachate was measured and the recovery rate was calculated to be 81% in combination with the vanadium content in the vanadium slag (right-hand point shown in fig. 2).
Example 4
The embodiment provides a method for extracting vanadium from vanadium slag briquettes through roasting and acid leaching, which is applied industrially, and the method comprises the following steps:
s1, adding 500 g of CaO2The powders were mixed with 5kg of vanadium slag and mixed in a mixing tank for 10h to mix the two powders uniformly. And (3) ball-milling the mixed powder in a high-energy ball mill for 10 hours to ensure that the particle size of the powder is 200-400 nm.
And S2, pressing the mixture into blocks in a stainless steel die with the inner diameter of 3cm, wherein the pressure in the pressing process is 10MPa, and the pressing time is 5 min. After demoulding, a block with a diameter of 3cm and a thickness of about 1cm is obtained.
And S3, raising the temperature of the muffle furnace to 850 ℃, keeping the constant temperature, and putting the block in the S2 into the muffle furnace to start roasting. After keeping the temperature for 2h, the block is taken out and rapidly cooled in the air.
S4, crushing the roasted blocks in a sampling machine for 120S to obtain clinker powder, and leaching the clinker powder in 25% dilute sulfuric acid at 80 ℃ for 2 h. The vanadium content in the acid leachate was measured and the recovery rate was calculated as about 81% in combination with the vanadium content in the vanadium slag (as shown in fig. 3).
Example 5
The embodiment provides a method for extracting vanadium from vanadium slag briquettes through roasting and acid leaching, which is applied industrially, and the method comprises the following steps:
s1, adding 500 g of CaO2Powder and 5kAnd g, mixing the vanadium slag, and mixing the materials in a mixing tank for 10 hours to uniformly mix the two kinds of powder. And (3) ball-milling the mixed powder in a high-energy ball mill for 10 hours to ensure that the particle size of the powder is 200-400 nm.
And S2, pressing the mixture into blocks in a stainless steel die with the inner diameter of 3cm, wherein the pressure in the pressing process is 15MPa, and the pressing time is 5 min. After demoulding, a block with a diameter of 3cm and a thickness of about 1cm is obtained.
And S3, raising the temperature of the muffle furnace to 900 ℃, keeping the temperature, and putting the block in the S2 into the muffle furnace to start roasting. After keeping the temperature for 2h, the block is taken out and rapidly cooled in the air.
S4, crushing the roasted blocks in a sampling machine for 120S to obtain clinker powder, and leaching the clinker powder in 25% dilute sulfuric acid at 80 ℃ for 2 h. The vanadium content in the acid leachate was measured and the recovery was calculated as approximately 80% in combination with the vanadium content in the vanadium slag (right-hand point shown in fig. 3).
Comparative example 1
Comparative example CaO is prepared on the basis of example 22The powder was adjusted to 85g, which was associated with V in the vanadium slag2O5The molar ratio is about 0.5: 1. Other conditions were the same as in example 2.
And detecting the content of vanadium in the acid leaching solution, and calculating the recovery rate of vanadium in the vanadium slag to be 67.4%.
Comparative example 2
Comparative example CaO is prepared on the basis of example 22The powder was adjusted to 240g, which was associated with V in the vanadium slag2O5The molar ratio is about 1.5: 1. Other conditions were the same as in example 2. And detecting the content of vanadium in the acid leaching solution, and calculating the recovery rate of vanadium in the vanadium slag to be 69.2%.
Comparative example 3
Comparative example CaO is prepared on the basis of example 22The powder and vanadium slag are ground to a particle size of 100 to 150 mesh (about 100 to 150 μm) by a common grinder. Other conditions were the same as in example 2. And detecting the content of vanadium in the acid leaching solution, and calculating the recovery rate of vanadium in the vanadium slag to be 71.8%.
Comparative example 4
Comparative example CaO is prepared on the basis of example 22Powder and vanadium slag are higherThe powder can be ball-milled for 10 hours in a ball mill to ensure that the particle size of the powder is 200-400 nm. Pressing into blocks in a stainless steel mold with an inner diameter of 3cm, wherein the pressure in the pressing process is 2MPa, and the pressing time is 5 min. Other conditions were the same as in example 2. And detecting the content of vanadium in the acid leaching solution, and calculating the recovery rate of vanadium in the vanadium slag to be 63.7%.
In addition, when balls with a diameter of 3cm were prepared using a disc tumbler instead of the briquettes in comparative example 4, the recovery rate of vanadium in the vanadium slag was less than 60% under the same conditions as in example 2.
Comparative example 5
The comparative example is based on example 2, the roasting temperature is reduced to 700 ℃, and the constant temperature roasting is carried out for 2 hours. Other conditions were the same as in example 2. The vanadium content in the acid leachate was measured and the recovery of vanadium in the vanadium slag was calculated to be 68% (first point on the left as shown in fig. 3).
As can be seen from FIG. 1, pores appear in the briquette-fired block, and these pores are formed by CaO2Decomposition by heating to give O2And the result is that. O is2When the vanadium slag is diffused to the outside of the block sample, the vanadium slag can be oxidized along the way. CaO (CaO)2V in vanadium slag2O5The molar ratio of (A) to (B) is within a range of 2:1 to 4:1, and the recovery rate of vanadium is not greatly changed. The roasting temperature is increased from 700 ℃ to 800 ℃, and the recovery rate of vanadium is obviously increased; the recovery rate of vanadium is basically kept unchanged by continuously increasing the roasting temperature.
In the present invention, CaO2V in vanadium slag2O5The parameters such as the molar ratio, the particle fineness, the briquetting pressure, the roasting temperature, the roasting time and the like have certain influence on the vanadium recovery rate.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The method for extracting vanadium by roasting and acid leaching of the vanadium slag briquettes in industrial application is characterized by comprising the following steps:
s1, mixing and grinding the vanadium slag with the grain size of more than kilogram level and calcium peroxide to be less than 50 mu m to obtain powder;
s2, briquetting the uniformly mixed vanadium slag and calcium peroxide powder under the pressure of 10-15 MPa to obtain a plurality of blocks;
s3, roasting the blocks in air to oxidize trivalent vanadium in the blocks into pentavalent vanadium;
and S4, grinding the blocks again to obtain clinker powder, and leaching the clinker powder in dilute sulfuric acid to obtain a vanadium-containing acid solution.
2. The method according to claim 1, wherein in S1, V is converted from vanadium in vanadium slag2O5V in calcium peroxide and vanadium slag2O5The molar ratio of (A) to (B) is 2-4: 1.
3. The method according to claim 1, wherein in S1, the particles are ground to a particle size of 10 μm or less.
4. The method of claim 3, wherein in S1, the particles are ground to 200-300 nm.
5. The method according to claim 4, characterized in that the mixture of vanadium slag and calcium peroxide is finely ground using a high energy ball mill.
6. The method according to claim 1, wherein in S2, the size of the block is 0.3-5 cm; the pressure in the briquetting process is 10-15 MPa, and the pressing time is 5-7 min.
7. The method of claim 1, wherein in S2, the mass is a mixture of irregularly shaped or different regularly geometrically shaped masses.
8. The method according to claim 1, wherein in S3, the roasting temperature is 800-850 ℃ and the roasting time is 2-2.5 h.
9. The method according to claim 1, wherein the concentration of dilute sulfuric acid in S4 is 20-30%.
10. The method of claim 1, wherein in S4, the leaching temperature is 75-85 ℃, and the acid leaching time is 2-2.5 h.
CN202110357478.XA 2021-04-01 2021-04-01 Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium Pending CN113088711A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110357478.XA CN113088711A (en) 2021-04-01 2021-04-01 Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110357478.XA CN113088711A (en) 2021-04-01 2021-04-01 Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium

Publications (1)

Publication Number Publication Date
CN113088711A true CN113088711A (en) 2021-07-09

Family

ID=76672802

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110357478.XA Pending CN113088711A (en) 2021-04-01 2021-04-01 Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium

Country Status (1)

Country Link
CN (1) CN113088711A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1952192A (en) * 2005-10-18 2007-04-25 孙世凡 Process for extracting vanadium from peroxide sintered ore and furnace slag
CN102296192A (en) * 2011-09-20 2011-12-28 武汉工程大学 Composite roasting additive for extracting vanadium pentoxide from vanadium-containing stone coal and application of composite roasting additive
CN108707747A (en) * 2018-05-31 2018-10-26 攀枝花恒弘球团有限公司 The method for producing vanadium bearing slag is roasted containing vanadium raw materials
CN110184452A (en) * 2019-06-11 2019-08-30 北京科技大学 A kind of method of vanadium in extraction solid
CN110343855A (en) * 2019-08-20 2019-10-18 攀钢集团攀枝花钢铁研究院有限公司 The method of efficient calcification vanadium extraction
CN110643838A (en) * 2019-11-12 2020-01-03 四川大学 Method for roasting vanadium slag by adopting calcium sulfate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1952192A (en) * 2005-10-18 2007-04-25 孙世凡 Process for extracting vanadium from peroxide sintered ore and furnace slag
CN102296192A (en) * 2011-09-20 2011-12-28 武汉工程大学 Composite roasting additive for extracting vanadium pentoxide from vanadium-containing stone coal and application of composite roasting additive
CN108707747A (en) * 2018-05-31 2018-10-26 攀枝花恒弘球团有限公司 The method for producing vanadium bearing slag is roasted containing vanadium raw materials
CN110184452A (en) * 2019-06-11 2019-08-30 北京科技大学 A kind of method of vanadium in extraction solid
CN110343855A (en) * 2019-08-20 2019-10-18 攀钢集团攀枝花钢铁研究院有限公司 The method of efficient calcification vanadium extraction
CN110643838A (en) * 2019-11-12 2020-01-03 四川大学 Method for roasting vanadium slag by adopting calcium sulfate

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
何志军等: "《微波冶金新技术》", 30 September 2017, 冶金工业出版社 *
廖世明等: "《国外钒冶金》", 28 February 1985, 冶金工业出版社 *

Similar Documents

Publication Publication Date Title
JP4984204B2 (en) Indium oxide powder and method for producing the same
TWI654140B (en) Lithium metal composite oxide powder
CN108359792B (en) Acid oxidation pellet of titanium concentrate and vanadium iron concentrate bulk concentrate and preparation method thereof
CN113896182B (en) Green lithium iron phosphate precursor and preparation method and application thereof
CN113526894B (en) Method for strengthening sintering decarburization of coal gangue
CN106517201A (en) Method for producing vanadium carbide through vertical medium-frequency induction furnace
CN112430108A (en) Method for preparing refractory material by using copper smelting slag as raw material
CN113429136B (en) Coal gangue layered distribution sintering decarburization process
CN113333770B (en) Preparation method of powder metallurgy iron powder
CN113088711A (en) Method for industrially applying vanadium slag briquetting roasting acid leaching vanadium
CN113957240A (en) Preparation method of manganese-containing vanadium-titanium magnetite pellet
CN113088712A (en) Method for extracting vanadium from vanadium slag by water leaching through large-scale treatment of vanadium slag
KR102405107B1 (en) Manufacturing method and manufacturing apparatus of lithium transition metal oxide
CN109369191B (en) Preparation method of yttrium-containing boron nitride-aluminum nitride composite powder
CN110627513A (en) Magnesium-calcium-iron sand prepared by using flotation magnesite concentrate powder as raw material and preparation method thereof
CN115172718A (en) Method for preparing lithium iron manganese phosphate by solid-phase coating method
CN109384468B (en) Preparation method of boron nitride-aluminum nitride composite powder
CN109517994B (en) Method for purifying mangano-manganic oxide from manganese steel plant smoke dust and product
CN113101942A (en) Molecular sieve composite catalytic material for catalytic oxidation of ozone and preparation method thereof
CN110669925B (en) Alkaline bentonite for pellets
CN117776701B (en) Method for preparing permanent magnetic ferrite pre-sintering material by taking iron scales as raw materials
KR102396972B1 (en) Method and apparatus for preparing transition metal lithium oxide
JP3651911B2 (en) Method for producing metallic chromium
CN116732357A (en) Method for preparing birnessite from pyrolusite
CN116103518A (en) Vanadium extraction method of vanadium slag by taking barium slag as additive

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
RJ01 Rejection of invention patent application after publication

Application publication date: 20210709