CN112795787A - Method for extracting vanadium and dephosphorizing phosphorus-containing vanadium slag - Google Patents
Method for extracting vanadium and dephosphorizing phosphorus-containing vanadium slag Download PDFInfo
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- CN112795787A CN112795787A CN202011304054.9A CN202011304054A CN112795787A CN 112795787 A CN112795787 A CN 112795787A CN 202011304054 A CN202011304054 A CN 202011304054A CN 112795787 A CN112795787 A CN 112795787A
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 128
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 66
- 239000011574 phosphorus Substances 0.000 title claims abstract description 63
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000002893 slag Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000002386 leaching Methods 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 21
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 16
- 150000002505 iron Chemical class 0.000 claims abstract description 15
- 239000010452 phosphate Substances 0.000 claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 230000002378 acidificating effect Effects 0.000 claims abstract description 10
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011268 mixed slurry Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 15
- 239000000292 calcium oxide Substances 0.000 claims description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 11
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 239000001099 ammonium carbonate Substances 0.000 claims description 8
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 8
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 5
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide 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
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000010703 silicon Substances 0.000 abstract description 11
- 229910052710 silicon Inorganic materials 0.000 abstract description 11
- 238000000605 extraction Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 4
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 150000003863 ammonium salts Chemical class 0.000 description 7
- 230000002308 calcification Effects 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000009628 steelmaking Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910020489 SiO3 Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 159000000013 aluminium salts Chemical class 0.000 description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 2
- 239000001164 aluminium sulphate Substances 0.000 description 2
- 235000011128 aluminium sulphate Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- JKJKPRIBNYTIFH-UHFFFAOYSA-N phosphanylidynevanadium Chemical compound [V]#P JKJKPRIBNYTIFH-UHFFFAOYSA-N 0.000 description 2
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 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 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- CFVBFMMHFBHNPZ-UHFFFAOYSA-N [Na].[V] Chemical compound [Na].[V] CFVBFMMHFBHNPZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- DIMMBYOINZRKMD-UHFFFAOYSA-N vanadium(5+) Chemical compound [V+5] DIMMBYOINZRKMD-UHFFFAOYSA-N 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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (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)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The embodiment of the application provides a method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag, which comprises the steps of roasting the phosphorus-containing vanadium slag to obtain a vanadium-containing material; mixing the vanadium-containing material, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution, wherein the pH of the mixed slurry is controlled to be 0.5-1.5 in the acid leaching process, the phosphorus concentration in the leaching solution is 0.3-4 g/L, and the vanadium concentration is 10-25 g/L; and (3) reacting the leachate with aluminum salt and iron salt, then regulating the pH value to be 3-4.5 for dephosphorization, and carrying out solid-liquid separation to obtain phosphate slag and a dephosphorization solution. The purpose of deep vanadium extraction can be achieved through the scheme, silicon and phosphorus in the acidic vanadium-containing liquid can be effectively removed, and the effect of removing silicon and phosphorus is remarkable.
Description
Technical Field
The application belongs to the field of chemical industry, and particularly relates to a method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag.
Background
Vanadium and its compounds are widely used in the fields of aerospace, steel, chemical industry, electronic energy, medicine and the like due to excellent physical and chemical properties, and are called monosodium glutamate in modern industry. The vanadium titano-magnetite is a multi-metal intergrowth ore of vanadium, titanium, iron and the like, and is an important vanadium extraction resource in China. Panzhihua-Xichang area is the most rich area of vanadium-titanium resource in China, and vanadium-titanium magnet has been proved at presentThe reserve of the mine is 67.3 million tons, the reserve of the prospect is 100 million tons, and the reserve contains vanadium (V)2O5)1475 million tons, vanadium reserve 67.3% of the whole country, third world.
In recent years, with the stricter requirements of users on the performance of steel, P is required to be less than or equal to 0.015 wt% for high-quality steel, and P is required to be less than or equal to 0.01 wt% for low-temperature aviation steel pipes, tin-plated plates and the like. If vanadium titano-magnetite is adopted for smelting, the P content in the molten iron is often higher and is 0.06 wt% -0.08 wt%, after desulfurization vanadium extraction or vanadium extraction desulfurization treatment, the S content can be reduced to be below 0.015 wt%, but the P content in the semi-steel is still as high as 0.060 wt% -0.090 wt%, if dephosphorization is carried out only in the semi-steel steelmaking process, the steel grade with the P content being less than or equal to 0.015 wt% or the P content being less than or equal to 0.010 wt% can not be produced in large batch.
Relevant researches show that the vanadium extraction-steel making process of the converter is similar to the dephosphorization and steel making process of a duplex converter at home and abroad in equipment and process, and the vanadium extraction converter can be adopted to extract vanadium from vanadium-containing molten iron and simultaneously realize pre-dephosphorization, so that the vanadium extraction converter has the advantages that: 1. the P content in the final molten steel is as low as 0.011 wt%, and the requirements of smelting low-phosphorus steel and even ultra-low-phosphorus steel can be met; 2. the TFe content in the obtained vanadium slag is reduced by more than 3 percent, and the economic benefit is obvious. However, the method also has the problem of high P, CaO content in the obtained vanadium slag (the dephosphorizing agent-calcium oxide needs to be added in the vanadium extraction process of the vanadium-containing molten iron), and the content is generally respectively more than 0.3 wt% and more than 10 wt% (belonging to high-calcium high-phosphorus vanadium slag), which is far higher than the level of the existing vanadium slag. Because the sodium roasting-water leaching vanadium or the calcification roasting-acid leaching vanadium has strict limitation on the phosphorus content in the vanadium slag, and the P in the vanadium slag is required to be less than or equal to 0.05 wt%, the prior sodium vanadium leaching process and the prior calcification vanadium leaching process can not be directly produced.
Disclosure of Invention
The embodiment of the application provides a method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag, which can effectively remove phosphorus in an acidic vanadium-containing liquid and has an obvious phosphorus removal effect.
The first aspect of the embodiment of the application provides a method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag, which comprises the following steps:
roasting the phosphorus-containing vanadium slag to obtain a vanadium-containing material;
mixing the vanadium-containing material, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution, wherein the pH of the mixed slurry is controlled to be 0.5-1.5 in the acid leaching process, the phosphorus concentration in the leaching solution is 0.3-4 g/L, and the vanadium concentration is 10-25 g/L;
and (3) reacting the leachate with aluminum salt and iron salt, then regulating the pH value to be 3-4.5 for dephosphorization, and carrying out solid-liquid separation to obtain phosphate slag and a dephosphorization solution.
As an optional embodiment, the vanadium-containing material contains more than 1% by mass of vanadium.
As an alternative embodiment, the aluminium salt comprises aluminium sulphate or aluminium chloride.
In an alternative embodiment, the mass ratio of the iron in the iron salt to the phosphorus in the acidic vanadium-containing liquid is 1-2.5: 1.
As an alternative embodiment, the iron salt comprises at least one of ferric sulfate, polymeric ferric sulfate, or ferric chloride.
As an alternative embodiment, the reaction time of the leachate, the aluminum salt and the iron salt is 60-120 min.
As an optional implementation mode, the pH value is adjusted to be 3-4.5, and then the mixture is stirred for 20-40 min.
As an optional embodiment, the method further comprises a standing step before the solid-liquid separation; and standing for 1-3.5 h.
As an alternative embodiment, the phosphate is at least one of aluminum phosphate and iron phosphate.
In an optional embodiment, the reagent for adjusting the PH value to 3 to 4.5 includes at least one of ammonia water, ammonium carbonate, ammonium bicarbonate, magnesium oxide, magnesium hydroxide, magnesium carbonate, calcium oxide, calcium hydroxide, and calcium carbonate.
According to the method, phosphate is added in the acid leaching process, so that hydrolytic precipitation of vanadium can be inhibited, and vanadium loss is effectively reduced. The method can achieve the purpose of deep vanadium extraction, effectively remove silicon and phosphorus in the acidic vanadium-containing liquid, has a remarkable silicon and phosphorus removal effect, achieves the silicon and phosphorus removal rate of more than 99 percent, and has small vanadium loss.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The terms "first," "second," and the like in the description and in the claims of the present application and above, are used for distinguishing between different objects and not for describing a particular order. Furthermore, the terms "include" and "have," as well as any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those steps or elements listed, but may alternatively include other steps or elements not listed, or inherent to such process, method, article, or apparatus.
Reference in the specification to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the specification. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
The method for extracting vanadium and removing phosphorus from the phosphorus-containing vanadium slag comprises the following steps:
roasting the phosphorus-containing vanadium slag to obtain a vanadium-containing material; mixing vanadium-containing materials, phosphate and sulfuric acid, controlling the pH value of the mixed slurry to be 0.5-1.5, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution; then the leachate is mixed withMixing of aluminum and iron salts followed by the following reaction, A13++SiO3 2-→A12(SiO3)3、Fe3++PO4 3-→FePO4And then regulating the pH value to 3-4.5 for dephosphorization, and performing solid-liquid separation to obtain phosphate slag and a dephosphorization solution. Wherein the pH value of the mixed slurry is controlled to be 0.5-1.5 in the acid leaching process, the concentration of phosphorus in the leaching solution is 0.3-4 g/L, and the concentration of vanadium is 10-25 g/L.
The method for roasting the phosphorus-containing vanadium slag to obtain the vanadium-containing material specifically comprises the following steps: and (2) adding CaO: v2And carrying out calcification roasting on the vanadium slag with the molar ratio of O of 4-5 at the temperature of 800-900 ℃. The vanadium slag can be obtained by blowing molten iron in the vanadium extraction process, and meets the requirements of CaO: v2The high-calcium vanadium slag with the molar ratio of O being 4-5 can also be prepared by adding lime or limestone and other calcareous raw materials on the basis of common vanadium slag and mixing the materials to ensure that the ratio of CaO: v2And vanadium slag with the molar ratio of O being 4-5. And grinding the residual material after the calcification roasting to obtain the vanadium-containing material.
The pH value of the mixed slurry containing the phosphorus-vanadium slag is controlled to be 0.5-1.5, so that vanadium in a vanadium-containing material is fully dissolved and enters the leaching solution, and meanwhile, phosphate is added in the acid leaching process so as to improve the phosphorus concentration in the mixed slurry and the leaching solution, so that vanadium and phosphorus form a vanadium-phosphorus heteropoly acid complex, and the loss of vanadium caused by hydrolysis and precipitation of the vanadium is avoided.
After the leachate reacts with aluminum salt and iron salt, the pH value can be adjusted to 3-4.5 by using ammonium salt, if the pH value is too high after the reaction and the use amount of the ammonium salt is too large, vanadium is formed into ammonium polyvanadate and is separated out along with precipitation, so that vanadium loss is caused, the pH value is too low, the formed precipitation is not facilitated to be separated out, and the vanadium is still in the solution, so that the pH value needs to be adjusted to 3.5-4.5 by adding the ammonium salt. The ammonium salt is ammonium bicarbonate or ammonium carbonate.
As an optional embodiment, the vanadium-containing raw material with the vanadium mass content of more than 1% in the phosphorus-containing vanadium slag.
As an alternative embodiment, the aluminium salt comprises aluminium sulphate or aluminium chloride.
In an alternative embodiment, the mass ratio of the iron in the iron salt to the phosphorus in the acidic vanadium-containing liquid is 1-2.5: 1.
As an alternative embodiment, the iron salt comprises at least one of ferric sulfate, polymeric ferric sulfate, or ferric chloride.
As an alternative embodiment, the reaction time of the leachate, the aluminum salt and the iron salt is 60-120 min.
Specifically, after the leachate is obtained, sufficient aluminum salt and iron salt are added into the leachate to react for 60-120 min at the temperature of 60-80 ℃.
As an optional implementation mode, the pH value is adjusted to be 3-4.5, and then the mixture is stirred for 20-40 min.
As an optional embodiment, the method further comprises a standing step before the solid-liquid separation; and standing for 1-3.5 h.
As an alternative embodiment, the phosphate is at least one of aluminum phosphate and iron phosphate.
As an optional embodiment, the reagent for adjusting the pH value to 3 to 4.5 includes at least one of ammonia water, ammonium carbonate, ammonium bicarbonate, magnesium oxide, magnesium hydroxide, magnesium carbonate, calcium oxide, calcium hydroxide, and calcium carbonate.
According to the method, the phosphate is added in the acid leaching process, so that the hydrolytic precipitation of vanadium can be inhibited, and the loss of vanadium is effectively reduced; according to the method, acid leaching is carried out at a lower pH level with the addition of phosphate, vanadium in a vanadium-containing raw material can be fully leached, and then phosphorus in the leachate is removed by reacting the leachate with aluminum salt and iron salt and adjusting the pH. The purpose of deep vanadium extraction can be achieved through the scheme of the application; and silicon and phosphorus in the acidic vanadium-containing liquid are effectively removed, the silicon and phosphorus removal effect is remarkable, the silicon and phosphorus removal rate reaches over 99 percent, and the vanadium loss is small.
The first embodiment is as follows:
and (2) adding CaO: v2Carrying out calcification roasting on vanadium slag with the molar ratio of O of 4-5 at the temperature of 800-900 ℃ to obtain vanadium-containing material; taking roasted vanadium-containing material (V)20517.85%, P0.04%) 200g, was added to 700mL of water together with 5.8g of aluminum phosphate, and the pH of the slurry was adjusted to 0.6 to 0.8 with sulfuric acid at room temperature with stirringStirring for reaction for 70min, and performing solid-liquid separation to obtain acid leaching residue V205The content is 0.75 percent, and the vanadium leaching rate is 96.0 percent; leachate V5+The concentration is 27.46g/L, and the P concentration is 2.55 g/L; to an acidic leaching solution ([ Si ]]＝0.52g/L、[P]2.4 for 0.83g/L, pH) at Al: Si: 1.4: 1 (mass ratio); adding 4.61g of aluminum sulfate, 1.0: 1 (mass ratio) of Fe and P, 2.96g of ferric sulfate, stirring at the temperature of 60-80 ℃ for 60min, adding ammonium salt to adjust the pH value to 3.8, stirring for reacting for 50min, standing for 1h, filtering, and analyzing silicon and phosphorus by assay, wherein Si is 0.015 g/L; p is 0.005 g/L.
Example two:
and (2) adding CaO: v2Carrying out calcification roasting on vanadium slag with the molar ratio of 0 being 4-5 at the temperature of 800-900 ℃ to obtain vanadium-containing materials; taking roasted vanadium-containing material (V)20517.85%, P0.04%), 200g, and 6.4g of iron phosphate were added to 700mL of water, the pH of the slurry was adjusted to 0.6 to 0.8 with sulfuric acid at room temperature, the mixture was stirred and reacted for 70min, solid-liquid separation was performed, and V was contained in the acid leaching residue205The content is 0.8 percent, and the vanadium leaching rate is 95.0 percent; leachate V5+The concentration is 26.46g/L, and the P concentration is 2.58 g/L; to an acidic leaching solution ([ Si ]]＝0.54g/L、[P]2.4 for 0.81g/L, pH) at Al: Si: 1.4: 1 (mass ratio); adding 4.61g of aluminum sulfate, adding 2.96g of ferric sulfate into the mixture of Fe and P (in a mass ratio of 1.0 to 1), stirring the mixture at the temperature of between 60 and 80 ℃ for 60min, adding ammonium salt to adjust the pH value to 3.5, stirring the mixture to react for 50min, standing the mixture for 1h, filtering the mixture, and analyzing silicon and phosphorus by an assay, wherein Si is 0.014 g/L; p is 0.006 g/L.
Example three:
and (2) adding CaO: v2Carrying out calcification roasting on vanadium slag with the molar ratio of O of 4-5 at the temperature of 800-900 ℃ to obtain vanadium-containing material; taking roasted vanadium-containing material (V)20517.85%, P0.04%), 200g, and 6.4g of iron phosphate were added to 700mL of water, the pH of the slurry was adjusted to 0.6 to 0.8 with sulfuric acid at room temperature, the mixture was stirred and reacted for 70min, solid-liquid separation was performed, and V was contained in the acid leaching residue205The content is 0.82 percent, and the vanadium leaching rate is 95.2 percent; leachate V5+The concentration is 26.56g/L, and the P concentration is 2.68 g/L; to an acidic leaching solution ([ Si ]]＝0.55g/L、[P]0.83g/L, pH is2.4) at Al: Si: 1.4: 1 (mass ratio); adding 4.43g of aluminum chloride, adding 2.43g of iron chloride into the mixture of Fe and P (in a mass ratio of 1 to 1), stirring the mixture at the temperature of between 60 and 80 ℃ for 60min, adding ammonium salt to adjust the pH value to 3.6, stirring the mixture to react for 50min, standing the mixture for 1h, filtering the mixture, and analyzing silicon and phosphorus by an assay, wherein Si is 0.14 g/L; p is 0.007 g/L.
The foregoing detailed description of the embodiments of the present application has been presented to illustrate the principles and implementations of the present application, and the above description of the embodiments is only provided to help understand the method and the core concept of the present application; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
Claims (10)
1. A method for extracting vanadium and dephosphorizing from phosphorus-containing vanadium slag is characterized by comprising the following steps:
roasting the phosphorus-containing vanadium slag to obtain a vanadium-containing material;
mixing the vanadium-containing material, phosphate and sulfuric acid, carrying out acid leaching, and carrying out solid-liquid separation to obtain a leaching solution, wherein the pH of the mixed slurry is controlled to be 0.5-1.5 in the acid leaching process, the phosphorus concentration in the leaching solution is 0.3-4 g/L, and the vanadium concentration is 10-25 g/L;
and (3) reacting the leachate with aluminum salt and iron salt, then regulating the pH value to be 3-4.5 for dephosphorization, and carrying out solid-liquid separation to obtain phosphate slag and a dephosphorization solution.
2. The method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag according to claim 1, wherein the vanadium-containing material contains more than 1% by mass of vanadium.
3. The method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag according to claim 1, wherein the aluminum salt comprises aluminum sulfate or aluminum chloride.
4. The method for extracting vanadium and removing phosphorus from the phosphorus-containing vanadium slag according to claim 1, wherein the mass ratio of iron in the iron salt to phosphorus in the acidic vanadium-containing liquid is 1-2.5: 1.
5. The method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag according to claim 1, wherein the iron salt comprises at least one of ferric sulfate, polymeric ferric sulfate or ferric chloride.
6. The method for extracting vanadium and removing phosphorus from the phosphorus-containing vanadium slag according to claim 1, wherein the reaction time of the leachate with aluminum salt and iron salt is 60-120 min.
7. The method for extracting vanadium and removing phosphorus from the phosphorus-containing vanadium slag according to claim 1, wherein the pH value is adjusted to 3 to 4.5, and then the mixture is stirred for 20 to 40 min.
8. The method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag according to claim 1, characterized by further comprising a standing step before solid-liquid separation; and standing for 1-3.5 h.
9. The method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag according to claim 1, wherein the phosphate is at least one of aluminum phosphate and iron phosphate.
10. The method for extracting vanadium and removing phosphorus from phosphorus-containing vanadium slag according to claim 1, wherein the reagent for adjusting the pH value to 3-4.5 comprises at least one of ammonia water, ammonium carbonate, ammonium bicarbonate, magnesium oxide, magnesium hydroxide, magnesium carbonate, calcium oxide, calcium hydroxide and calcium carbonate.
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