CN117305607A - Method for recovering vanadium from vanadium slag of converter - Google Patents
Method for recovering vanadium from vanadium slag of converter Download PDFInfo
- Publication number
- CN117305607A CN117305607A CN202311407028.2A CN202311407028A CN117305607A CN 117305607 A CN117305607 A CN 117305607A CN 202311407028 A CN202311407028 A CN 202311407028A CN 117305607 A CN117305607 A CN 117305607A
- Authority
- CN
- China
- Prior art keywords
- vanadium
- slag
- recovering
- converter
- 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
Links
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 131
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000002893 slag Substances 0.000 title claims abstract description 31
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 44
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000001556 precipitation Methods 0.000 claims abstract description 19
- 230000001376 precipitating effect Effects 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910001456 vanadium ion Inorganic materials 0.000 claims abstract description 4
- 238000007598 dipping method Methods 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000000634 powder X-ray diffraction Methods 0.000 claims description 4
- 238000004846 x-ray emission Methods 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 14
- 239000002253 acid Substances 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 8
- 239000003513 alkali Substances 0.000 abstract description 5
- 238000002386 leaching Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 229910052748 manganese Inorganic materials 0.000 description 8
- 239000011572 manganese Substances 0.000 description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- VWBLQUSTSLXQON-UHFFFAOYSA-N N.[V+5] Chemical compound N.[V+5] VWBLQUSTSLXQON-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000002308 calcification Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- 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
- C22B7/001—Dry 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for recovering vanadium from vanadium slag of a converter, which comprises the following steps: s1, mixing converter vanadium slag and calcium salt according to a certain proportion, and roasting in a muffle furnace to obtain a first roasting material; s2, cooling the first roasting material to room temperature, crushing, grinding and sieving to obtain a second roasting material; s3, adding the mixture into sulfuric acid solution for soaking, filtering to obtain filtrate and filter residue dissolved with vanadium ions, and adding a vanadium precipitating agent into the vanadium-containing filtrate to obtain vanadium-containing precipitate and filtrate; and S4, calcining the vanadium-containing precipitate in a muffle furnace to obtain vanadium pentoxide. The invention adopts cheap and easily available acid and alkali, the steps of precipitation and separation are easy to grasp, and the invention has the advantages of simple process, convenient operation and low cost.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for recovering vanadium from converter vanadium slag.
Background
Vanadium belongs to a high-melting-point rare metal, has good ductility, high hardness and no magnetism, and can be widely applied to the fields of metallurgy, aviation, batteries and catalysis in the form of alloys or compounds. Sodium roasting and calcification roasting processes are two most mature vanadium extraction processes which take converter vanadium slag as raw materials at present.
At present, the prior art for precipitating vanadium from acidic vanadium liquid mainly comprises the following steps: the patent with the publication number of CN107541599B discloses a preparation method for preparing high-purity vanadium by using an acidic high-manganese vanadium-containing leaching solution, and belongs to the technical field of metallurgical production processes. Provides a preparation method for preparing high-purity vanadium by using an acidic high-manganese vanadium-containing leaching solution, which has low production cost and good preparation effect. The preparation method comprises the steps of firstly removing impurity manganese under the strong alkaline condition, then precipitating under the strong acid condition, washing vanadium precipitate, and finally calcining the vanadium precipitate to obtain the high-purity vanadium. The patent with publication number CN111592042B discloses a method for preparing high-purity vanadium pentoxide by ammonium-free vanadium precipitation of vanadium liquid, which comprises the following steps: step a: carrying out hydrolysis vanadium precipitation on vanadium liquid by using an ammonium-free vanadium precipitation agent, and carrying out solid-liquid separation to obtain a hydrolysis vanadium precipitation product; step b: purifying the hydrolyzed vanadium precipitation product by utilizing an organic acid dilute solution, and obtaining the purified hydrolyzed vanadium precipitation product after solid-liquid separation and washing; step c: calcining the purified hydrolyzed precipitated vanadium product to obtain high-purity vanadium pentoxide. The vanadium pentoxide prepared by the method can reach a vanadium precipitation rate of more than 98%, and the purity of the vanadium pentoxide reaches more than 99.9%. The Chinese patent document with publication number of CN112239806A discloses a method for extracting vanadium from acidic high-phosphorus vanadium liquid, which comprises the following specific processes: (1) Adding an oxidant into the acidic high-phosphorus vanadium liquid to react, and then filtering to obtain filtered vanadium liquid; (2) Adjusting the pH value of the filtered vanadium liquid obtained in the step (1), heating, adding a vanadium precipitating agent, reacting, and filtering to obtain a vanadium-rich precipitate; (3) Calcining the vanadium-rich precipitate obtained in the step (2) to obtain vanadium pentoxide; in the step (1), the oxidant is at least one of ammonium persulfate, sodium chlorate, potassium chlorate and hydrogen peroxide.
The defects of the acid ammonium salt vanadium precipitation in the prior art are expressed as the following two points: (1) The concentration of the precipitated vanadium is limited by the concentration of sodium sulfate in the solution, vanadium and sodium in the solution exist in a certain proportion, hydrolysate or heteropolyacid and other precipitates are easy to generate in the process of regulating the pH value, (2) the ammonia nitrogen content in the precipitated vanadium wastewater is high, and the mixed salt of sodium sulfate and ammonium sulfate is obtained through the subsequent evaporation concentration process, so that the separation and purification are difficult, and the utilization value is low. The ammonium-free precipitation method needs a large amount of sulfuric acid and high-temperature heating, has high industrial production cost and serious corrosion to equipment, and partial manganese in the vanadium precipitation process can form manganese vanadate precipitate to influence the purity of the subsequent vanadium pentoxide.
The vanadium leaching solution prepared from the vanadium titano-magnetite by using the acid vanadium extraction process contains high manganese content, and conventional manganese removal methods comprise a contact oxidation method, a hydrogen peroxide oxidation method, a potassium permanganate oxidation method and an electrochemical oxidation method. However, these methods are suitable for environments with higher pH and are generally not suitable for strong acid systems. The ozone oxidation method is easy to oxidize bivalent manganese into permanganate, the amount of ozone is difficult to control, the solubility of ozone in water is low, an ozone generating device is expensive, the operation is complex, the power consumption is high, and the operation cost is high.
In view of this, improvements should be made over the prior art.
Disclosure of Invention
The invention mainly aims to provide a method for recovering vanadium from vanadium slag of a converter, which comprises the steps of selecting acid and alkali which are cheap and easy to obtain, and then carrying out precipitation and separation to obtain vanadium pentoxide with purity of more than 99 percent.
According to one aspect of the present invention, a method for recovering vanadium from converter vanadium slag is presented, comprising the steps of:
s1, mixing converter vanadium slag and calcium salt according to a certain proportion, and roasting in a muffle furnace to obtain a first roasting material;
s2, cooling the first roasting material to room temperature, crushing, grinding and sieving to obtain a second roasting material;
s3, adding the mixture into sulfuric acid solution for soaking, filtering to obtain filtrate and filter residue dissolved with vanadium ions, and adding a vanadium precipitating agent into the vanadium-containing filtrate to obtain vanadium-containing precipitate and filtrate;
and S4, calcining the vanadium-containing precipitate in a muffle furnace to obtain vanadium pentoxide.
According to one embodiment of the invention, the temperature of the calcination in step S1 is 400-900 ℃.
According to one embodiment of the invention, the particles of the second calcine are below 200 mesh.
According to one embodiment of the invention, the mass concentration of the sulfuric acid solution is 10-50%, and the mass concentration of the sulfuric acid solution and the second roasting material are=1-5L/1 Kg.
According to one embodiment of the invention, in step S3, the rotation speed of the stirring paddle is 100-500 rpm; the dipping temperature is 30-90 ℃ and the dipping time is 1-4h.
According to one embodiment of the invention, the vanadium precipitating agent is an amino group containing compound.
According to one embodiment of the invention, the molar ratio of the vanadium precipitating agent to vanadium is 0.1-1.0.
According to one embodiment of the invention, in step S4, the rotation speed of the stirring paddle is 100-500 rpm; the precipitation temperature is 30-90 ℃ and the soaking time is 0.2-1h.
According to one embodiment of the invention, the calcium salt is one or more of calcium sulfate, calcium carbonate and calcium oxide.
According to one embodiment of the invention, step S4 further comprises, after obtaining vanadium pentoxide, determining its purity and crystalline form by X-ray fluorescence spectroscopy analysis and X-ray powder diffraction analysis.
In a method for recovering vanadium from converter vanadium slag according to an embodiment of the invention, comprising the steps of: the invention obtains vanadium pentoxide with purity up to 99% by selecting cheap and easily available acid and alkali and then carrying out precipitation and separation, has the advantages of simple process, convenient operation and low cost, and solves the problems of high operation cost and complex process of the existing vanadium extraction process.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a process flow diagram of a method for recovering vanadium from converter vanadium slag according to the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
The vanadium slag of the converter is an important raw material for recovering vanadium in the metallurgical process. At present, vanadium is separated and recovered from vanadium slag of a converter in a large number, wherein sodium roasting-leaching (water leaching, acid leaching and alkaline leaching) -precipitation-calcination are one of the most traditional vanadium extraction processes, and the process has higher vanadium extraction efficiency, but has serious problems of waste gas, waste water and waste residue pollution. In order to reduce the three wastes, calcium salt is adopted to replace sodium salt to develop the calcified roasting process. In the roasting process, the oxidation products of the low-valence vanadium have various forms due to different usage amounts of the added auxiliary agents. In addition, as the roasted material is easy to form a liquid phase, the problems of material aggregation, wrapping, bonding, sintering, furnace burden looping, material balling and the like are caused, the vanadium-containing spinel phase is wrapped by the silicate phase and is not easy to expose, and the oxidation conversion rate of vanadium is not high.
In order to solve the above problems, as shown in fig. 1, the present invention provides a method for recovering vanadium from vanadium slag of a converter, comprising the steps of:
s1, mixing converter vanadium slag and calcium salt according to a certain proportion, and roasting in a muffle furnace to obtain a first roasting material;
s2, cooling the first roasting material to room temperature, crushing, grinding and sieving to obtain a second roasting material;
s3, adding the mixture into sulfuric acid solution for soaking, filtering to obtain filtrate and filter residue dissolved with vanadium ions, and adding a vanadium precipitating agent into the vanadium-containing filtrate to obtain vanadium-containing precipitate and filtrate;
and S4, calcining the vanadium-containing precipitate in a muffle furnace to obtain vanadium pentoxide.
In the method for recovering vanadium from the vanadium slag of the converter, according to the embodiment of the invention, the vanadium pentoxide with the purity of more than 99% is obtained by selecting the acid and the alkali which are low in cost and easy to obtain and then carrying out precipitation and separation, so that the method has the advantages of simple process, convenient operation and low cost, and solves the problems of high operation cost and complex process of the existing vanadium extraction process.
The production process flow of the invention is as follows: roasting, grinding, sieving, dipping, precipitating and calcining, wherein:
and (2) roasting in the step (S1) at the temperature of 400-900 ℃, and oxidizing low-valence vanadium in the vanadium slag of the converter into high-valence vanadium through roasting. In some embodiments, the firing temperature is 400-600 ℃.
The first roasting material is crushed, ground and sieved after being cooled to room temperature, and the pretreatment of the first roasting material is used for facilitating subsequent leaching.
The particles of the pretreated second roasting material are below 200 meshes.
The mass concentration of the sulfuric acid solution is 10-50%, and the mass concentration of the sulfuric acid solution and the second roasting material is=1-5L to 1Kg. Leaching the second roasting material by sulfuric acid, and dissolving vanadium in the vanadium slag roasting material of the converter.
In the step S3, the rotating speed of the stirring paddle is 100-500 rpm; the dipping temperature is 30-90 ℃ and the dipping time is 1-4h.
In some embodiments, the agitation speed is 400-500 rpm; the mass concentration of the sulfuric acid solution is 20-30%, and the mass concentration of the sulfuric acid solution to the second roasting material=2-4L to 1Kg; the dipping temperature is 70-90 ℃ and the dipping time is 1-2h.
In order to precipitate vanadium in the filtrate, a vanadium precipitating agent is added into the vanadium-containing filtrate, wherein the vanadium precipitating agent is an amino-containing compound.
The molar ratio of the vanadium precipitating agent to vanadium is 0.1-1.0.
In the step S4, the rotating speed of the stirring paddle is 100-500 rpm; the precipitation temperature is 30-90 ℃ and the soaking time is 0.2-1h.
In some embodiments, the molar ratio of vanadium precipitating agent to vanadium is from 0.2 to 0.5; stirring at 400-500 rpm; the precipitation temperature is 30-50 ℃, and the soaking time is 0.2-0.5h.
Further, in order to leach as much vanadium as possible from the vanadium slag of the converter, the calcium salt is one or more of calcium sulfate, calcium carbonate and calcium oxide.
Step S4 also comprises the steps of determining the purity and the crystal form of the vanadium pentoxide through X-ray fluorescence spectrometry analysis and X-ray powder diffraction analysis after the vanadium pentoxide is obtained.
The invention is proved by experiments, after the vanadium pentoxide is obtained, the purity and the crystal form of the vanadium pentoxide are determined by X-ray fluorescence spectrometry analysis and X-ray powder diffraction analysis, and the purity of the obtained vanadium pentoxide is found to be more than 99 percent.
The test results are shown in the following table:
the invention provides a method for recovering vanadium from vanadium slag of a converter, which comprises the steps of selecting acid and alkali which are cheap and easy to obtain, and then carrying out precipitation and separation to obtain vanadium pentoxide with purity of more than 99 percent.
The foregoing is an exemplary embodiment of the present disclosure, and the order in which the embodiments of the present disclosure are disclosed is merely for the purpose of description and does not represent the advantages or disadvantages of the embodiments. It should be noted that the above discussion of any of the embodiments is merely exemplary and is not intended to suggest that the scope of the disclosure of embodiments of the invention (including the claims) is limited to these examples and that various changes and modifications may be made without departing from the scope of the invention as defined in the claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
Those of ordinary skill in the art will appreciate that: the above discussion of any embodiment is merely exemplary and is not intended to imply that the scope of the disclosure of embodiments of the invention, including the claims, is limited to such examples; combinations of features of the above embodiments or in different embodiments are also possible within the idea of an embodiment of the invention, and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, equivalent substitutions, improvements, and the like, which are made within the spirit and principles of the embodiments of the invention, are included within the scope of the embodiments of the invention.
Claims (10)
1. A method for recovering vanadium from vanadium slag of a converter, comprising the steps of:
s1, mixing converter vanadium slag and calcium salt according to a certain proportion, and roasting in a muffle furnace to obtain a first roasting material;
s2, cooling the first roasting material to room temperature, crushing, grinding and sieving to obtain a second roasting material;
s3, adding the mixture into sulfuric acid solution for soaking, filtering to obtain filtrate and filter residue dissolved with vanadium ions, and adding a vanadium precipitating agent into the vanadium-containing filtrate to obtain vanadium-containing precipitate and filtrate;
and S4, calcining the vanadium-containing precipitate in a muffle furnace to obtain vanadium pentoxide.
2. The method for recovering vanadium from vanadium slag in converter according to claim 1, wherein the roasting temperature in step S1 is 400-900 ℃.
3. The method for recovering vanadium from vanadium slag of a converter according to claim 1, wherein the particles of the second roasting material are below 200 mesh.
4. The method for recovering vanadium from vanadium slag of a converter according to claim 1, wherein the mass concentration of the sulfuric acid solution is 10-50%, and the sulfuric acid solution is 1-5L/1 Kg.
5. The method for recovering vanadium from vanadium slag of a converter according to claim 1, wherein in step S3, the rotation speed of the stirring paddle is 100 to 500 rpm; the dipping temperature is 30-90 ℃ and the dipping time is 1-4h.
6. The method for recovering vanadium from vanadium slag of a converter according to claim 1, wherein the vanadium precipitating agent is an amino-containing compound.
7. The method for recovering vanadium from vanadium slag of a converter according to claim 1, wherein the molar ratio of the vanadium precipitating agent to vanadium is 0.1 to 1.0.
8. The method for recovering vanadium from vanadium slag of a converter according to claim 1, wherein in step S4, the rotation speed of the stirring paddle is 100 to 500 rpm; the precipitation temperature is 30-90 ℃ and the soaking time is 0.2-1h.
9. The method of recovering vanadium from converter vanadium slag of claim 1, wherein the calcium salt is one or more of calcium sulfate, calcium carbonate, and calcium oxide.
10. The method for recovering vanadium from vanadium slag of claim 1, wherein step S4 further comprises determining the purity and crystal form of vanadium pentoxide by X-ray fluorescence spectroscopy analysis and X-ray powder diffraction analysis after obtaining the vanadium pentoxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311407028.2A CN117305607A (en) | 2023-10-26 | 2023-10-26 | Method for recovering vanadium from vanadium slag of converter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311407028.2A CN117305607A (en) | 2023-10-26 | 2023-10-26 | Method for recovering vanadium from vanadium slag of converter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117305607A true CN117305607A (en) | 2023-12-29 |
Family
ID=89255296
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311407028.2A Pending CN117305607A (en) | 2023-10-26 | 2023-10-26 | Method for recovering vanadium from vanadium slag of converter |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117305607A (en) |
-
2023
- 2023-10-26 CN CN202311407028.2A patent/CN117305607A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109666789B (en) | Method for preparing vanadium pentoxide by using vanadium-chromium slag and manganese carbonate | |
| CN114684801B (en) | Method for preparing high-purity ferric phosphate by using pyrite cinder | |
| CN107954474B (en) | Method for producing vanadium product and basic chromium sulfate by using vanadium-chromium solution | |
| CN102628111B (en) | Method for extracting rhenium from rhenium-rich concentrates | |
| CN106848473B (en) | Method for selectively recovering lithium in waste lithium iron phosphate batteries | |
| CN111057876B (en) | Method for preparing high-purity vanadium pentoxide by microemulsion extraction | |
| CN112430740B (en) | Method for strengthening vanadium-chromium separation by cooperatively roasting vanadium slag through calcium salt and manganese salt | |
| CN112080651B (en) | Method for extracting vanadium by high-calcium low-sodium ammonium composite roasting | |
| CN1800422A (en) | Method for processing cobalt copper alloy | |
| HU231497B1 (en) | Method for purifying nickel-cobalt-manganese leaching solution | |
| CN108754186A (en) | The method for preparing vfanadium compound containing vanadium solution | |
| CN114058851A (en) | Method for recycling tungsten, molybdenum and titanium from waste denitration catalyst | |
| CN111020234A (en) | Method for preparing APT (ammonium paratungstate) by utilizing tungsten-containing waste | |
| CN111575502A (en) | Method for extracting nickel element from nickel ore | |
| WO2012113263A1 (en) | Method for removing iron and aluminum from iron-based waste material containing high-value elements through natural oxidation | |
| JP2023152896A (en) | Method of preparing high-purity lithium carbonate through reduction calcining of waste cathode material | |
| CN114988485A (en) | Method for synchronously producing manganous-manganic oxide and ferric oxide for soft magnetism by using marine polymetallic nodule | |
| CN111560518B (en) | Treatment method of copper-containing molybdenum concentrate | |
| CN115744991B (en) | Method for preparing tungsten oxide from tungsten-containing waste | |
| CN102849782B (en) | Method for producing high-purity zinc oxide by steel mill smoke dust ash ammonia method decarburization | |
| WO2020138137A1 (en) | Method for purifying vanadium oxide | |
| CN117305607A (en) | Method for recovering vanadium from vanadium slag of converter | |
| CN105983707A (en) | Method for preparing high-purity rhenium powder from rhenium-containing high-arsenic copper sulfide | |
| CN111020233B (en) | Method for preparing vanadium pentoxide by ammonium-free vanadium precipitation | |
| CN110629043B (en) | Bismuth extraction method based on phase transformation of bismuth sulfide ore |
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 |