CN116103518A - Vanadium extraction method of vanadium slag by taking barium slag as additive - Google Patents
Vanadium extraction method of vanadium slag by taking barium slag as additive Download PDFInfo
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- CN116103518A CN116103518A CN202211644963.6A CN202211644963A CN116103518A CN 116103518 A CN116103518 A CN 116103518A CN 202211644963 A CN202211644963 A CN 202211644963A CN 116103518 A CN116103518 A CN 116103518A
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- barium
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 244
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 243
- 239000002893 slag Substances 0.000 title claims abstract description 147
- 229910052788 barium Inorganic materials 0.000 title claims abstract description 78
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000000605 extraction Methods 0.000 title claims abstract description 39
- 239000000654 additive Substances 0.000 title claims abstract description 29
- 230000000996 additive effect Effects 0.000 title claims abstract description 27
- 238000002386 leaching Methods 0.000 claims abstract description 70
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 26
- 239000002699 waste material Substances 0.000 abstract description 8
- DNWNZRZGKVWORZ-UHFFFAOYSA-N calcium oxido(dioxo)vanadium Chemical compound [Ca+2].[O-][V](=O)=O.[O-][V](=O)=O DNWNZRZGKVWORZ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 159000000009 barium salts Chemical class 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000002440 industrial waste Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 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 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052916 barium silicate Inorganic materials 0.000 description 1
- HMOQPOVBDRFNIU-UHFFFAOYSA-N barium(2+);dioxido(oxo)silane Chemical compound [Ba+2].[O-][Si]([O-])=O HMOQPOVBDRFNIU-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 230000002308 calcification Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 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
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910021652 non-ferrous alloy Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- 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
- 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
- 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
-
- 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)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for extracting vanadium from vanadium slag by taking barium slag as an additive, which comprises the following steps: s1: and uniformly mixing the dried and crushed barium slag and the dried and crushed vanadium slag to obtain a mixture. S2: roasting the mixture in air to oxidize trivalent vanadium into pentavalent vanadium, and obtaining clinker. S3: cooling and crushing clinker, and adding dilute sulfuric acid for leaching to obtain leaching liquid and leached tailings. The invention takes byproduct barium slag in the barium salt production process as an additive, barium carbonate in the barium slag and oxidized high-valence vanadium in the barium slag generate calcium vanadate, and leaching liquid and leached tailings are obtained through acid leaching. The leaching solution containing vanadium is used for extracting vanadium, producing vanadium products, leaching tailings can be recycled, no pollutant is generated in the whole vanadium slag vanadium extraction process, the leaching solution is very friendly to the environment, the effect of treating waste by waste can be achieved, and the efficient recycling of vanadium resources and barium resources is realized.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of industrial waste residue vanadium slag and barium slag, and particularly relates to a vanadium extraction method of vanadium slag by taking barium slag as an additive.
Background
In the modern industry vanadium is used in various fields, in particular in the fields of steel making, nonferrous alloys, chemical industry production and batteries, etc., wherein more than 80% of the vanadium yield is from vanadium slag.
The existing vanadium extraction process mainly comprises sodium oxidation roasting and calcification oxidation roasting. The sodium-modified oxidizing roasting vanadium extraction process is the main stream vanadium extraction method of vanadium slag. Although the sodium-modified oxidation roasting vanadium extraction process is relatively mature, the method has a series of advantages, and meanwhile, the problems of environmental pollution, poor raw material applicability, easy looping of the rotary kiln and difficult utilization of waste liquid tailings are also existed. The calcified oxidation roasting vanadium extraction is another vanadium extraction process applied to industrial production, has the advantages of clean and efficient roasting process, strong raw material applicability and easy recycling of waste liquid and tailings, but has the problem of low vanadium conversion rate.
Aiming at the defects of calcified roasting and sodium roasting, the prior art optimizes calcified roasting to extract vanadium by treating calcified clinker and adding oxalic acid, thereby overcoming the difficulties of low leaching rate of calcified roasting vanadium, long leaching time, difficult filtration of leached ore pulp, serious equipment corrosion, difficult utilization of tailings and the like. The prior art also provides a blank roasting technology, specifically, no additive is used during roasting, low alkali solution can be added for leaching, and then vanadium liquid and iron-rich tailings are obtained through filtration. The blank roasting method shortens the time of high-temperature roasting and oxidation, reduces energy consumption, avoids the phenomenon of looping, and improves the conversion rate of vanadium.
However, no vanadium extraction method using barium slag as an additive is available in the prior art.
Disclosure of Invention
First, the technical problem to be solved
The invention provides a vanadium slag vanadium extraction method taking barium slag as an additive, aiming at solving the problems of high pollution and low vanadium recovery rate of the vanadium slag vanadium extraction technology in the prior art.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
a method for extracting vanadium from vanadium slag by taking barium slag as an additive comprises the following steps:
s1: uniformly mixing the dried and crushed barium slag and the dried and crushed vanadium slag to obtain a mixture;
s2: roasting the mixture in air to oxidize trivalent vanadium into pentavalent vanadium, so as to obtain clinker;
s3: cooling and crushing clinker, and adding dilute sulfuric acid for leaching to obtain leaching liquid and leached tailings.
In the step S2, the air oxidizes trivalent vanadium in the vanadium slag into pentavalent vanadium, and the barium carbonate further reacts with the high-valent vanadium to generate carbon dioxide and calcium vanadate, so that the contact between the reaction product and the air can be further increased in the process of outwards overflowing the carbon dioxide gas.
In the step S3, the leaching solution containing vanadium is used for extracting vanadium to produce vanadium products, the leached tailings can be recycled, the calcium vanadate is leached by dilute sulfuric acid to obtain the leaching solution containing vanadium and leached tailings, the leaching solution containing vanadium can be used for extracting vanadium to produce vanadium products, and the leached tailings can be recycled, so that no pollutant is generated in the whole vanadium slag vanadium extraction process, and the method is very environment-friendly.
In the invention, the barium slag and the vanadium slag belong to industrial wastes, and compared with pure substance additives, the cost of using the barium slag is very low, and the vanadium extraction cost can be obviously reduced. In addition, the synergistic treatment of the barium slag and the vanadium slag can also play a role in treating waste by waste, and the efficient recycling of vanadium resources and barium resources is realized.
In order to further improve the roasting efficiency, the vanadium slag and the barium slag are fully contacted and barium vanadate is generated, and the particle size of the vanadium slag and the barium slag particles is required to be controlled. In the vanadium extraction method of the vanadium slag, in the step S1, preferably, particles with a particle size of less than 74 μm account for 80% or more in terms of mass fraction in the barium slag, and particles with a particle size of less than 74 μm account for 80% or more in the vanadium slag. The grain diameters of the vanadium slag and the barium slag are smaller than 74 mu m, which is favorable for full contact and improves the oxidation rate and acid leaching recovery rate of vanadium in the vanadium slag.
More preferably, in step S1, in terms of mass fraction, particles with a particle size of less than 74 μm account for 100% in the barium slag, and particles with a particle size of less than 74 μm account for 100% in the vanadium slag.
In the vanadium extraction method of the vanadium slag, preferably, in the step S1, the mass fraction of the barium carbonate in the barium slag is 25-35%, and the mass fraction of the vanadium pentoxide in the vanadium slag is 5-15% calculated by the vanadium pentoxide.
The effective component of the barium slag used in the invention is barium carbonate, and the barium slag also contains barium sulfate, barium silicate, silicon dioxide, ferrous oxide, aluminum oxide and the like. The mass fraction of barium carbonate in the barium slag is generally 25-35%, wherein the presence of silica, ferrous oxide and aluminum oxide affects the leaching of vanadium.
The vanadium slag contains ferric oxide, silicon dioxide, manganese oxide, titanium dioxide, magnesium oxide, aluminum oxide, calcium oxide, chromium oxide and the like in addition to vanadium (calculated by vanadium pentoxide). The mass percentage of vanadium pentoxide in the vanadium slag is generally 5-15%, wherein the presence of ferric oxide, silicon dioxide and titanium dioxide can affect the leaching of vanadium.
In the vanadium extraction method of the vanadium slag, in the step S1, preferably, vanadium in the vanadium slag is converted into vanadium pentoxide, and the molar ratio of barium carbonate in the barium slag to the vanadium pentoxide in the vanadium slag is 0.25:1-2:1, specifically, may be 0.25:1, 0.5:1, 0.75:1, 1:1, 1.25:1, 1.5:1, 2:1, and the like. The molar ratio of the barium carbonate in the barium slag to the vanadium pentoxide in the vanadium slag can ensure that powder particles of the vanadium slag are contacted with the barium carbonate in the barium slag as much as possible, so that calcium vanadate is generated as low as possible, and the recovery rate and the subsequent leaching rate of vanadium are improved.
In the above-mentioned vanadium extraction method of vanadium slag, preferably, in the step S2, the roasting temperature is 700-950 ℃, specifically 700 ℃, 750 ℃, 800 ℃, 825 ℃, 850 ℃, 875 ℃, 900 ℃, 950 ℃ and the like. In the invention, the roasting temperature of 700-950 ℃ can ensure that vanadium is oxidized by oxygen as much as possible, so that the recovery rate of vanadium is improved, and if the roasting temperature is lower than 700 ℃, vanadium slag can be incompletely roasted, so that the recovery rate of vanadium is lower.
In the vanadium extraction method of the vanadium slag, in the step S2, the roasting time is preferably 0.5-2.5h, and specifically may be 0.5h, 1h, 1.5h, 1.75h, 2.0h, 2.25h, 2.5h, etc.
In the vanadium extraction method of the vanadium slag, in the step S3, preferably, the mass fraction of the dilute sulfuric acid is 10-40%, and specifically may be 10%, 15%, 20%, 25%, 30%, 35%, 40%, etc. In addition, the particle size of the clinker after cooling and pulverizing is required to be kept below 74. Mu.m, that is, the clinker can be sieved by a 200-mesh sieve. In the step S3, the particle size of the crushed clinker is controlled, so that the leaching process is facilitated, and the leaching rate of vanadium is improved.
In the above vanadium extraction method of vanadium slag, preferably, in step S3, the leaching temperature is 65-95 ℃, specifically 65 ℃,70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ and the like.
(III) beneficial effects
The beneficial effects of the invention are as follows:
the invention takes byproduct barium slag in the barium salt production process as an additive, barium carbonate in the barium slag and oxidized high-valence vanadium in the vanadium slag generate calcium vanadate, and leaching liquid and leached tailings are obtained through acid leaching. The leaching solution containing vanadium is used for extracting vanadium, vanadium products are produced, and the leached tailings can be recycled.
In the invention, the barium slag and the vanadium slag belong to industrial wastes, have wide sources, have low cost compared with pure material additives, and can obviously reduce the vanadium extraction cost. In addition, the barium slag and the vanadium slag are cooperatively treated, so that the effect of treating waste by waste can be achieved, and the efficient recycling of vanadium resources and barium resources is realized.
Drawings
FIG. 1 is an XRD pattern of clinker and leached tailings of example 1;
FIGS. 2a-2f are electronic probe face scans of clinker in example 1;
FIGS. 3a-3e are electronic probe facial scans of the leached tailings of example 1.
Detailed Description
The invention will be better explained for understanding by referring to the following detailed description of the embodiments in conjunction with the accompanying drawings.
Example 1
The embodiment provides a vanadium extraction method of vanadium slag by taking barium slag as an additive, which comprises the following steps:
s1: and respectively crushing and finely grinding the dried vanadium slag and the dried barium slag until the particle size is smaller than 74 mu m, uniformly mixing the barium slag fine material and the vanadium slag fine material to ensure that the molar ratio of barium carbonate in the barium slag to vanadium pentoxide in the vanadium slag is 0.5:1, and obtaining the mixture.
S2: and (3) placing the mixture into a muffle furnace, and roasting for 2 hours at 875 ℃ to oxidize trivalent vanadium into pentavalent vanadium, so as to obtain roasting clinker.
S3: cooling clinker, pulverizing to particle size smaller than 74 μm, taking 3g of calcined clinker, and placing into a beaker according to a solid-to-liquid ratio of 10:1, adding 30ml of 25% sulfuric acid solution by mass fraction, and keeping the leaching temperature at 80 ℃ for leaching, wherein the leaching solution contains vanadium and leached tailings.
And detecting the vanadium content in the vanadium-containing leaching solution, and calculating to obtain the leaching rate of the vanadium of 98.4 percent by combining the vanadium content in the vanadium slag.
XRD detection is performed on the roasted clinker obtained in the step S2 and the leached tailings obtained in the step S3, and the results are shown in figure 1, wherein substances possibly occurring in the roasted clinker and the leached tailings are shown in figure 1. As can be seen from fig. 1, the diffraction peak of barium vanadate is detected in the clinker generated by roasting the barium slag and the vanadium slag, and after sulfuric acid leaching, the diffraction peak of barium vanadate disappears, which indicates that barium vanadate is generated in the clinker, and the leaching treatment enriches the barium vanadate in the leaching solution.
The roasting clinker obtained in step S2 and the leached tailings obtained in step S3 are subjected to electron probe detection, the results of which are shown in fig. 2a-2f and fig. 3a-3e, wherein the area where vanadium and barium are simultaneously present is marked as shown in fig. 2 a.
As can be seen from fig. 2a-2f and fig. 3a-3e, the areas where the vanadium element is present in the calcined clinker have a barium element distribution, which indicates that vanadium forms barium vanadate with barium, which verifies the XRD analysis results. In addition, only barium element and no vanadium element are detected in the leached tailings, which also proves that under the optimal conditions of the embodiment, vanadium in the roasted clinker is enriched into the leaching solution.
The components and contents of the barium slag used in this example are shown in Table 1, and those of the vanadium slag are shown in Table 2.
TABLE 1 composition and content of barium slag
TABLE 2 composition and content of vanadium slag
As is clear from Table 1, the barium slag contains BaCO in an amount of 30.92% by mass 3 24.33% SiO 2 6.83% Al 2 O 3 2.71% FeO. The vanadium slag contains 8.387% of V by mass 2 O 5 43.49% of Fe 2 O 3 14.62% SiO 2 10.27% TiO 2 。
Example 2
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S1, the molar ratio of barium carbonate in the barium slag to vanadium pentoxide in the vanadium slag is 0.25:1.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 91.2% by combining the vanadium content in the vanadium slag.
Example 3
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S1, the molar ratio of barium carbonate in the barium slag to vanadium pentoxide in the vanadium slag is 1.5:1.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 92.5% by combining the vanadium content in the vanadium slag.
Example 4
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S2, the roasting temperature is 800 ℃.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 92.2% by combining the vanadium content in the vanadium slag.
Example 5
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S2, the roasting temperature is 950 ℃.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 95.9% by combining the vanadium content in the vanadium slag.
Example 6
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S2, the roasting time period is 1.5h.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 96.8% by combining the vanadium content in the vanadium slag.
Example 7
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S2, the roasting time period is 2.5h.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 98.1% by combining the vanadium content in the vanadium slag.
Example 8
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S3, the leaching temperature is 65 ℃.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 97.6% by combining the vanadium content in the vanadium slag.
Example 9
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S3, the leaching temperature is 95 ℃.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 98.1% by combining the vanadium content in the vanadium slag.
Example 10
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S3, the mass fraction of dilute sulfuric acid is 15%.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 96.3% by combining the vanadium content in the vanadium slag.
Example 11
The embodiment provides a vanadium extraction method using barium slag as an additive, which is different from embodiment 1 in that in step S3, the mass fraction of dilute sulfuric acid is 40%.
The vanadium content in the vanadium-containing leaching solution prepared in the embodiment is detected, and the leaching rate of the vanadium is calculated to be 97.9% by combining the vanadium content in the vanadium slag.
Comparative example 1
The comparative example provides a vanadium extraction method of vanadium slag by taking barium slag as an additive, which comprises the following steps:
s1: and respectively crushing and finely grinding the dried vanadium slag and the dried barium slag until the particle size is smaller than 74 mu m, uniformly mixing the barium slag fine material and the vanadium slag fine material to ensure that the molar ratio of barium carbonate in the barium slag to vanadium pentoxide in the vanadium slag is 2.5:1, and obtaining the mixture.
S2: and (3) placing the mixture into a muffle furnace, and roasting for 2 hours at 800 ℃ to oxidize trivalent vanadium into pentavalent vanadium, so as to obtain roasting clinker.
S3: cooling clinker, pulverizing to particle size smaller than 74 μm, taking 3g of calcined clinker, and placing into a beaker according to a solid-to-liquid ratio of 10:1, adding 30ml of 25% sulfuric acid solution by mass fraction, and keeping the leaching temperature at 80 ℃ for leaching, wherein the leaching solution contains vanadium and leached tailings.
The vanadium content in the vanadium-containing leaching solution prepared in the comparative example is detected, and the leaching rate of the vanadium is calculated to be 90.6 percent by combining the vanadium content in the vanadium slag.
Comparative example 2
This comparative example provides a vanadium extraction method using barium slag as an additive, which is different from example 1 in that in step S2, the roasting temperature is 650 ℃.
The vanadium content in the vanadium-containing leaching solution prepared in the comparative example is detected, and the leaching rate of the vanadium is calculated to be 89.8% by combining the vanadium content in the vanadium slag.
Comparative example 3
This comparative example provides a vanadium extraction method using barium slag as an additive, which is different from example 1 in that in step S2, the mass concentration of dilute sulfuric acid is 5%.
The vanadium content in the vanadium-containing leaching solution prepared in the comparative example is detected, and the leaching rate of the vanadium is calculated to be 82.3 percent by combining the vanadium content in the vanadium slag.
Comparative example 4
This comparative example provides a vanadium extraction method of vanadium slag using barium carbonate as an additive, which is different from example 1 in that barium carbonate having a purity of 99.5% is used as an additive, finely ground to a particle size of less than 74 μm, and then mixed with barium slag.
The vanadium content in the vanadium-containing leaching solution prepared in the comparative example is detected, and the leaching rate of the vanadium is calculated to be 88.4 percent by combining the vanadium content in the vanadium slag.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any person skilled in the art may make modifications or alterations to the above disclosed technical content to equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (9)
1. The vanadium extraction method of the vanadium slag with the barium slag as the additive is characterized by comprising the following steps of:
s1: uniformly mixing the dried and crushed barium slag and the dried and crushed vanadium slag to obtain a mixture;
s2: roasting the mixture in air to oxidize trivalent vanadium into pentavalent vanadium, so as to obtain clinker;
s3: cooling and crushing clinker, and adding dilute sulfuric acid for leaching to obtain leaching liquid and leached tailings.
2. The method according to claim 1, wherein in step S1, particles with a particle size of less than 74 μm in the barium slag account for 80% or more, and particles with a particle size of less than 74 μm in the vanadium slag account for 80% or more, in terms of mass fraction.
3. The method according to claim 2, wherein in step S1, in terms of mass fraction, particles with a particle size of less than 74 μm in the barium slag account for 100%, and particles with a particle size of less than 74 μm in the vanadium slag account for 100%.
4. The method for extracting vanadium from vanadium slag according to claim 1, wherein in the step S1, the mass fraction of barium carbonate in the barium slag is 25-35%, and the mass fraction of vanadium pentoxide in the vanadium slag is 5-15% in terms of vanadium pentoxide.
5. The method for extracting vanadium from vanadium slag according to claim 1, wherein in step S1, vanadium in the vanadium slag is converted into vanadium pentoxide, and the molar ratio of barium carbonate in the barium slag to the vanadium pentoxide in the vanadium slag is 0.25:1-2:1.
6. The method for extracting vanadium from vanadium slag according to claim 1, wherein in step S2, the roasting temperature is 700-950 ℃.
7. The method for extracting vanadium from vanadium slag according to claim 1, wherein in step S2, the roasting time is 0.5-2.5h.
8. The method according to claim 1, wherein in the step S3, the mass fraction of the dilute sulfuric acid is 10-40%.
9. The method according to claim 1, wherein in step S3, the leaching temperature is 65-95 ℃.
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| WO2011018799A2 (en) * | 2009-08-10 | 2011-02-17 | Aditya Birla Science & Technology Co. Ltd | A process for preparing vanadium oxide from vanadate sludge |
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| CN112111661A (en) * | 2020-09-24 | 2020-12-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for extracting vanadium by calcium-manganese composite roasting of vanadium slag |
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| WO2011018799A2 (en) * | 2009-08-10 | 2011-02-17 | Aditya Birla Science & Technology Co. Ltd | A process for preparing vanadium oxide from vanadate sludge |
| CN101892380A (en) * | 2010-07-02 | 2010-11-24 | 淅川县玉典钒业有限责任公司 | Method for preparing vanadium pentoxide and roasting additive used therein |
| CN103667710A (en) * | 2013-12-04 | 2014-03-26 | 四川省川威集团有限公司 | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag |
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