CN112095024B - Vanadium extraction method of sodium-modified vanadium extraction tailings - Google Patents
Vanadium extraction method of sodium-modified vanadium extraction tailings Download PDFInfo
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- CN112095024B CN112095024B CN202010807801.4A CN202010807801A CN112095024B CN 112095024 B CN112095024 B CN 112095024B CN 202010807801 A CN202010807801 A CN 202010807801A CN 112095024 B CN112095024 B CN 112095024B
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- vanadium extraction
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- 238000000605 extraction Methods 0.000 title claims abstract description 90
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 88
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium(0) Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 150000003681 vanadium Chemical class 0.000 title claims abstract description 63
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000000843 powder Substances 0.000 claims abstract description 63
- 238000002386 leaching Methods 0.000 claims abstract description 47
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 41
- VTHJTEIRLNZDEV-UHFFFAOYSA-L Magnesium hydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 30
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 29
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 18
- 239000008235 industrial water Substances 0.000 claims description 8
- GCLGEJMYGQKIIW-UHFFFAOYSA-H Sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 7
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium monoxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N Iron(III) oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- FWYVLGJBTZNHEM-UHFFFAOYSA-H Sodiumpolyphosphate Chemical compound [Na+].[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O FWYVLGJBTZNHEM-UHFFFAOYSA-H 0.000 claims description 4
- 229910000460 iron oxide Inorganic materials 0.000 claims description 4
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N Manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- GNTDGMZSJNCJKK-UHFFFAOYSA-N Vanadium(V) oxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N al2o3 Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- 229910000468 manganese oxide Inorganic materials 0.000 claims description 3
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese(II,III) oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 230000001376 precipitating Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 3
- QDOXWKRWXJOMAK-UHFFFAOYSA-N Chromium(III) oxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000001698 pyrogenic Effects 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000011112 process operation Methods 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 238000005039 chemical industry Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 7
- -1 sodium vanadium Chemical compound 0.000 description 5
- 229910001425 magnesium ion Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910001415 sodium ion Inorganic materials 0.000 description 4
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- WGLPBDUCMAPZCE-UHFFFAOYSA-N trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006011 modification reaction Methods 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N Sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N Sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 229940117975 chromium trioxide Drugs 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- XGZRAKBCYZIBKP-UHFFFAOYSA-L disodium;dihydroxide Chemical compound [OH-].[OH-].[Na+].[Na+] XGZRAKBCYZIBKP-UHFFFAOYSA-L 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052611 pyroxene Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 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
- 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
-
- 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
Abstract
The invention relates to the technical field of chemical industry and comprehensive resource utilization, and discloses a vanadium extraction method of sodium-modified vanadium extraction tailings. The method comprises the following steps: (1) adding magnesium oxide powder or magnesium hydroxide fine powder and an optional leaching aid into the sodium-modified vanadium extraction tailings, then adding water, mixing and ball-milling to form homogeneous slurry; (2) placing the slurry in a high-pressure reaction kettle for hydrothermal reaction; (3) and filtering after the reaction is finished to obtain a vanadium-containing solution and vanadium extraction residues. The invention adopts a full-wet hydrothermal extraction process, does not generate waste gas, has high degree of cleanness and is environment-friendly; compared with the traditional pyrogenic process, the method has low production cost, the leaching rate of vanadium in the sodium-modified vanadium extraction tailings can reach 69 percent at most, a large amount of vanadium can be recovered, and the economic benefit and the social benefit are better; the method has simple and feasible process operation, and the vanadium-containing solution can obtain the vanadium flakes with the grade of more than 98 percent after concentration and vanadium precipitation.
Description
Technical Field
The invention relates to the technical field of chemical engineering and comprehensive utilization of resources, in particular to a vanadium extraction method of sodium-modified vanadium extraction tailings.
Background
The existing vanadium extraction process mainly comprises a sodium vanadium extraction process and a calcium vanadium extraction process. Compared with the calcium vanadium extraction process, the sodium vanadium extraction process is relatively mature, the vanadium yield is relatively high, the cost is relatively low, but a large amount of sodium vanadium extraction tailings are generated in the production process, and the difficulty in comprehensive resource utilization is high. At present, the main treatment mode is a pyrogenic process, namely, sodium salt is added into tailings, the tailings are roasted at 600 ℃ and then leached to obtain a vanadium-containing solution, and vanadium is further precipitated after concentration.
Therefore, a method for extracting vanadium, which has the advantages of simple and environment-friendly production process, low production cost and high vanadium extraction rate, is urgently needed.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a vanadium extraction method of sodium-modified vanadium extraction tailings, which comprises the following steps:
(1) adding magnesium oxide powder or magnesium hydroxide fine powder and an optional leaching aid into the sodium-modified vanadium extraction tailings, then adding water, mixing and ball-milling to form homogeneous slurry;
(2) placing the slurry in a high-pressure reaction kettle for hydrothermal reaction;
(3) and filtering after the reaction is finished to obtain a vanadium-containing solution and vanadium extraction residues.
Preferably, the sodium-modified vanadium extraction tailings contain 38-47 wt% of ferric oxide, 10.5-12 wt% of titanium dioxide, 15.5-17 wt% of silicon dioxide, 5-6 wt% of sodium oxide, 9-10 wt% of manganese oxide, 4.5-5 wt% of magnesium oxide, 3.5-4 wt% of aluminum oxide, 2-3 wt% of calcium oxide, 1-2 wt% of vanadium pentoxide and 2-3 wt% of chromium oxide.
Preferably, in the step (1), the magnesium oxide powder or the magnesium hydroxide fine powder accounts for 5-10 parts by weight and the leaching aid accounts for 0-0.5 part by weight based on 100 parts by weight of the total weight of the sodium-modified vanadium extraction tailings, the magnesium oxide powder or the magnesium hydroxide fine powder and the leaching aid.
Preferably, the leaching aid is sodium polyphosphate and/or sodium hexametaphosphate.
Preferably, the particle size of the sodium-modified vanadium extraction tailings is below 0.2 mm.
Preferably, the purity of the magnesium oxide powder or the magnesium hydroxide fine powder is more than 95%.
Preferably, the particle size of the magnesium oxide powder or the magnesium hydroxide fine powder is below 0.074 mm.
Preferably, in step (1), water is added in a volume ratio of 2-8: 1.
Preferably, the water is industrial water.
Preferably, in step (1), the ball milling time is 30 to 60 minutes.
Preferably, in step (2), the hydrothermal reaction conditions are: the reaction temperature is 60-200 ℃; the reaction time is 30-180 min.
Preferably, in step (2), the hydrothermal reaction conditions are: the reaction temperature is 120-130 ℃; the reaction time is 60-80 min.
Preferably, the method further comprises the step of concentrating and precipitating the vanadium-containing solution obtained in the step (3) to obtain the vanadium flakes with the grade of more than 98%.
Compared with the prior art, the invention has the following advantages:
1) the invention adopts a full-wet hydrothermal extraction process, does not generate waste gas, has high degree of cleanness and is environment-friendly.
2) Compared with the traditional pyrogenic process, the method has low production cost, the leaching rate of vanadium in the sodium-modified vanadium extraction tailings can reach 69 percent at most, a large amount of vanadium can be recovered, and the method has good economic and social benefits.
3) The method has simple and feasible process operation, and the vanadium-containing solution can obtain the vanadium flakes with the grade of more than 98 percent after concentration and vanadium precipitation.
Drawings
FIG. 1 is a process flow diagram of a vanadium extraction method of sodium-modified vanadium extraction tailings.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Sodium in the sodium-modified vanadium extraction tailings mainly exists in the form of sodium silicate, and vanadium mainly exists in pyroxene solid solution and iron oxide. The inventor finds that the extraction of vanadium can be realized by adding active magnesium oxide powder or magnesium hydroxide fine powder into the sodium-modified vanadium extraction tailings, and replacing magnesium ions with sodium ions through the pressurized hydrothermal action, so that sodium is dissolved out in the forms of sodium vanadate, sodium hydroxide and the like. Based on the principle, the invention provides a vanadium extraction method of sodium-modified vanadium extraction tailings.
As shown in fig. 1, the method comprises the steps of:
(1) adding magnesium oxide powder or magnesium hydroxide fine powder and an optional leaching aid into the sodium-modified vanadium extraction tailings, then adding water, mixing and ball-milling to form homogeneous slurry;
(2) placing the slurry in a high-pressure reaction kettle for hydrothermal reaction;
(3) and filtering after the reaction is finished to obtain a vanadium-containing solution and vanadium extraction residues.
In the method, the sodium-modified vanadium extraction tailings comprise 38-47 wt% of ferric oxide, 10.5-12 wt% of titanium dioxide, 15.5-17 wt% of silicon dioxide, 5-6 wt% of sodium oxide, 9-10 wt% of manganese oxide, 4.5-5 wt% of magnesium oxide, 3.5-4 wt% of aluminum oxide, 2-3 wt% of calcium oxide, 1-2 wt% of vanadium pentoxide and 2-3 wt% of chromium trioxide.
In order to replace magnesium ions with sodium ions and realize extraction of vanadium, proper amount of magnesium oxide powder or magnesium hydroxide fine powder is required to be added into the tailings of sodium-modified vanadium extraction.
In the step (1), the total weight of the tailings of sodium-modified vanadium extraction, the fine powder of magnesium oxide or magnesium hydroxide and the leaching aid is 100 parts by weight, the fine powder of magnesium oxide or magnesium hydroxide is 5-10 parts by weight, and the leaching aid is 0-0.5 part by weight.
In specific embodiments, the magnesium oxide powder or magnesium hydroxide fine powder may be 5 parts by weight, 6 parts by weight, 7 parts by weight, 8 parts by weight, 9 parts by weight, or 10 parts by weight.
In specific embodiments, the infusion aid may or may not be added. In order to improve the leaching rate of vanadium, in a preferred embodiment, a proper amount of leaching aid can be added into the sodium-modified vanadium extraction tailings.
In the method of the present invention, the leaching aid may be selected conventionally in the art, and is not particularly limited as long as the leaching rate of vanadium can be increased.
In particular embodiments, the leaching aid may be sodium polyphosphate and/or sodium hexametaphosphate. In a preferred embodiment, the leaching aid is sodium hexametaphosphate.
Before the method disclosed by the invention is adopted to extract vanadium, pretreatment needs to be carried out on the sodium-modified vanadium extraction tailings, and specifically, the operation can comprise the operations of impurity removal, crushing and the like.
In a specific embodiment, the particle size of the sodium-modified vanadium extraction tailings is less than or equal to 0.2mm through crushing. In a preferred embodiment, the particle size of the sodium-modified vanadium extraction tailings is less than or equal to 0.1 mm.
Herein, the particle size refers to the size of the particle diameter unless otherwise specified.
In the method of the invention, in order to reduce the introduction of impurities and improve the leaching rate of vanadium, the purity of the used magnesium oxide powder or magnesium hydroxide fine powder is limited to a certain extent.
In a specific embodiment, the purity of the magnesium oxide powder or magnesium hydroxide fine powder is 95% or more. In a preferred embodiment, the purity of the magnesium oxide powder or magnesium hydroxide fine powder is 98% or more.
In order to completely replace the magnesium ions with sodium ions and to increase the leaching rate of vanadium, the particle size of the magnesium oxide powder or magnesium hydroxide fine powder needs to be limited to an appropriate range.
In a specific embodiment, the particle size of the magnesium oxide powder or magnesium hydroxide fine powder is below 0.074 mm. In a preferred embodiment, the particle size of the magnesium oxide powder or magnesium hydroxide fine powder is 0.05mm or less.
In the method of the invention, in order to mix the raw materials uniformly and not waste water resources, the liquid-solid ratio needs to be controlled reasonably. In the invention, the tailings of sodium-modified vanadium extraction, the magnesium oxide powder or the magnesium hydroxide fine powder and the leaching aid are solid raw materials, and the water is a liquid raw material.
In a specific embodiment, in step (1), water may be added in a liquid-to-solid ratio of 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, or 8:1 by volume. Herein, the liquid-solid ratio is the ratio of the sum of the sodium-modified vanadium extraction tailings, the magnesium oxide powder or the magnesium hydroxide fine powder and the leaching aid to water.
In the process according to the invention, for cost saving, in a preferred embodiment the water is industrial water.
After water is added, the solid raw materials and the water can be mixed in a ball mill to form homogeneous slurry, so that conditions are created for the subsequent hydrothermal reaction.
In a specific embodiment, in step (1), the ball milling time may be any value within a range of 30 minutes, 35 minutes, 40 minutes, 45 minutes, 50 minutes, 55 minutes, 60 minutes, and any two of these points.
In a preferred embodiment, in step (1), the ball milling time is 30 minutes.
In the method, in order to completely replace magnesium ions and sodium ions and further improve the leaching rate of vanadium in the sodium-modified vanadium extraction tailings, the temperature and time of the hydrothermal reaction need to be reasonably controlled.
In the step (2), the reaction temperature of the hydrothermal reaction is 60-200 ℃; specifically, for example, the temperature may be 60 ℃, 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃ or 200 ℃.
In a preferred embodiment, in step (2), the reaction temperature of the hydrothermal reaction is 120-130 ℃.
In the step (2), the reaction time of the hydrothermal reaction is 30-180 min; specifically, it may be 30min, 40min, 60min, 80min, 100min, 120min, 140min, 160min, or 180min, for example.
In a preferred embodiment, in step (2), the reaction time of the hydrothermal reaction is 60 to 80 min.
In a preferred embodiment, the method for extracting vanadium from the sodium-modified vanadium extraction tailings provided by the invention comprises the following steps:
(1) adding 10 wt% of magnesium oxide powder and 0.2 wt% of sodium hexametaphosphate into the sodium-modified vanadium extraction tailings, then adding industrial water according to the volume ratio of 8:1, and mixing and ball-milling in a ball mill for 30min to form homogeneous slurry, wherein the particle size of the sodium-modified vanadium extraction tailings is below 0.1mm, the purity of the magnesium oxide powder is above 98%, and the particle size of the magnesium oxide powder is below 0.05 mm;
(2) placing the slurry in a high-pressure reaction kettle to perform hydrothermal reaction at 120 ℃ for 60 min;
(3) and filtering after the reaction is finished to obtain a vanadium-containing solution and vanadium extraction residues.
In the method of the invention, after the vanadium-containing solution is obtained, the vanadium-containing solution can be further processed by adopting the operation commonly used in the field to obtain the vanadium product.
In a preferred embodiment, the vanadium-containing solution obtained in step (3) can be concentrated and precipitated to obtain vanadium flakes with a grade of more than 98%.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
In the method, the specific measurement method for the leaching rate of vanadium in the sodium-modified vanadium extraction tailings comprises the following steps: firstly detecting the content of all vanadium in the sodium-modified vanadium extraction tailings, then leaching part of vanadium in the sodium-modified vanadium extraction tailings by adopting the method of the invention, detecting the content of residual vanadium in the vanadium extraction residues, and calculating the leaching rate of vanadium according to a formula, wherein,
the vanadium leaching rate is (the content of all vanadium in the sodium-modified vanadium extraction tailings-the content of residual vanadium in the vanadium extraction residue)/the content of all vanadium in the sodium-modified vanadium extraction tailings is multiplied by 100 percent.
Example 1
Adding 5 wt% of magnesium oxide powder and 0.5 wt% of sodium hexametaphosphate into the sodium-modified vanadium extraction tailings, then adding industrial water according to the volume ratio of 6:1, and carrying out ball milling for 45min in a ball mill to ensure that magnesium oxide, a leaching aid and the sodium-modified vanadium extraction tailings are fully and uniformly mixed to form homogeneous slurry, wherein the particle size of the sodium-modified vanadium extraction tailings is below 0.2mm, the purity of the magnesium oxide powder is above 95%, and the particle size of the magnesium oxide powder is below 0.074 mm; putting the slurry into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 200 ℃ for 30 min; and filtering the slurry after reaction to obtain a vanadium-containing solution and vanadium-extracted residues. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is up to 62 percent.
Example 2
Adding 10 wt% of magnesium oxide powder and 0.2 wt% of sodium hexametaphosphate into the sodium-modified vanadium extraction tailings, then adding industrial water according to the volume ratio of 8:1, and carrying out ball milling in a ball mill for 30min to ensure that magnesium oxide, a leaching aid and the sodium-modified vanadium extraction tailings are fully and uniformly mixed to form homogeneous slurry, wherein the particle size of the sodium-modified vanadium extraction tailings is below 0.15mm, the purity of the magnesium oxide powder is above 98%, and the particle size of the magnesium oxide powder is below 0.05 mm; putting the slurry into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 120 ℃ for 60 min; and filtering the slurry after reaction to obtain a vanadium-containing solution and vanadium-extracted residues. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is up to 69 percent.
Example 3
Adding 8 wt% of magnesium hydroxide fine powder into the sodium-modified vanadium extraction tailings, then adding industrial water according to the volume ratio of 2:1, and carrying out ball milling in a ball mill for 60min to ensure that the magnesium hydroxide fine powder and the sodium-modified vanadium extraction tailings are fully and uniformly mixed and form homogeneous slurry, wherein the particle size of the sodium-modified vanadium extraction tailings is below 0.2mm, the purity of the magnesium hydroxide fine powder is above 95%, and the particle size of the magnesium hydroxide fine powder is below 0.074 mm; putting the slurry into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 60 ℃ for 180 min; and filtering the slurry after reaction to obtain a vanadium-containing solution and vanadium-extracted residues. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is measured to be up to 52 percent.
Example 4
The procedure of example 2 was followed, except that the leaching aid added was sodium polyphosphate. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is up to 65 percent.
Example 5
The process of example 2 was followed, except that the slurry was placed in an autoclave and the hydrothermal reaction was carried out at 130 ℃. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is up to 68 percent.
Example 6
The process of example 2 was followed, except that the slurry was placed in an autoclave for hydrothermal reaction for 80 min. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is up to 69 percent.
Example 7
The method is implemented according to the method of the embodiment 2, and is different from the method that the vanadium-containing solution is concentrated and precipitated to obtain the vanadium flakes with the grade of more than 98%.
Comparative example 1
The method is implemented according to the method of the example 2, except that no magnesia powder is added into the sodium-modified vanadium extraction tailings. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is measured to be 31 percent.
Comparative example 2
The method of example 2 was followed, except that 3 wt% of magnesium oxide powder was added to the tailings of sodium-modified vanadium extraction. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is 47 percent.
Comparative example 3
The process was carried out as in example 3, except that industrial water was added in a volume ratio of 1: 1. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is measured to be 45%.
Comparative example 4
The process of example 3 was followed, except that the slurry was placed in an autoclave and the hydrothermal reaction was carried out at 250 ℃. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is measured to be 46%.
Comparative example 5
The process of example 3 was followed, except that the slurry was placed in an autoclave for hydrothermal reaction for 20 min. The leaching rate of vanadium in the sodium-modified vanadium extraction tailings is measured to be 45%.
It can be seen from the results in the above examples and comparative examples that the vanadium of the tailings obtained by sodium treatment vanadium extraction according to the method of the present invention has a leaching rate of vanadium of more than 52%, and the leaching rate of vanadium can reach 69% at most, and the vanadium-containing solution is concentrated and precipitated to obtain vanadium flakes with a grade of more than 98%; and the leaching rate of vanadium in the comparative example is below 50 percent, so that the method can obviously improve the leaching rate of vanadium in the sodium-modified vanadium extraction tailings.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (7)
1. A vanadium extraction method of sodium-modified vanadium extraction tailings is characterized by comprising the following steps:
(1) adding magnesium oxide powder or magnesium hydroxide fine powder and an auxiliary leaching agent into the sodium-modified vanadium extraction tailings, then adding water, mixing and ball-milling to form homogeneous slurry, wherein the granularity of the sodium-modified vanadium extraction tailings is below 0.2mm, the magnesium oxide powder or magnesium hydroxide fine powder accounts for 5-10 parts by weight and the auxiliary leaching agent accounts for 0-0.5 part by weight based on 100 parts by weight of the total weight of the sodium-modified vanadium extraction tailings, the magnesium oxide powder or the magnesium hydroxide fine powder and the auxiliary leaching agent;
(2) placing the slurry in a high-pressure reaction kettle to carry out hydrothermal reaction, wherein the hydrothermal reaction conditions are as follows: the reaction temperature is 120-130 ℃; the reaction time is 60-80 min;
(3) filtering after the reaction is finished to obtain a vanadium-containing solution and vanadium extraction residues;
the sodium-modified vanadium extraction tailings contain 38-47 wt% of ferric oxide, 10.5-12 wt% of titanium dioxide, 15.5-17 wt% of silicon dioxide, 5-6 wt% of sodium oxide, 9-10 wt% of manganese oxide, 4.5-5 wt% of magnesium oxide, 3.5-4 wt% of aluminum oxide, 2-3 wt% of calcium oxide, 1-2 wt% of vanadium pentoxide and 2-3 wt% of chromium sesquioxide;
in the step (1), water is added according to the volume ratio of liquid to solid of 2-8: 1.
2. The method according to claim 1, wherein the leaching aid is sodium polyphosphate and/or sodium hexametaphosphate.
3. The method according to claim 1, wherein the purity of the magnesium oxide powder or the magnesium hydroxide fine powder is 95% or more.
4. The method of claim 1, wherein the particle size of the magnesium oxide powder or magnesium hydroxide fine powder is below 0.074 mm.
5. The method according to claim 1, wherein in step (1), the water is industrial water.
6. The method of claim 1, wherein in step (1), the ball milling time is 30 to 60 minutes.
7. The method according to claim 1, characterized by further comprising the step of concentrating and precipitating the vanadium-containing solution obtained in the step (3) to obtain the vanadium flakes with a grade of more than 98%.
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