CN113088724A - Method for leaching gallium in vanadium extraction tailings - Google Patents
Method for leaching gallium in vanadium extraction tailings Download PDFInfo
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- CN113088724A CN113088724A CN202110376398.9A CN202110376398A CN113088724A CN 113088724 A CN113088724 A CN 113088724A CN 202110376398 A CN202110376398 A CN 202110376398A CN 113088724 A CN113088724 A CN 113088724A
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- China
- Prior art keywords
- gallium
- leaching
- vanadium extraction
- extraction tailings
- naoh
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 51
- 238000002386 leaching Methods 0.000 title claims abstract description 46
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 42
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000605 extraction Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 71
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 description 4
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 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
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
Images
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
- C22B58/00—Obtaining gallium or indium
-
- 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
- C22B7/008—Wet processes by an alkaline or ammoniacal 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
Abstract
The invention relates to a method for leaching gallium from vanadium extraction tailings, and belongs to the technical field of extraction of gallium from vanadium extraction tailings. The method for leaching gallium in the vanadium extraction tailings comprises the following steps: uniformly mixing vanadium extraction tailings and an alkali solvent, drying for 4.5-5 h at 100-120 ℃, grinding to below 1mm, and air cooling to obtain gallium-containing residues, wherein the alkali solvent is Na2CO3NaOH, CaO, said Na2CO3CaO, NaOH: the mass ratio of the vanadium extraction tailings is as follows: 0.15-0.24: 0.4-0.45: 0.08-0.1: 0.8 to 1; roasting the obtained gallium-containing residue at 950-1100 ℃ for 1.3-1.5 h, cooling in a furnace, and grinding to be less than 0.5 mm; and mixing the roasted gallium-containing residue with a NaOH solution, and stirring and carrying out alkaline leaching for 1.2-1.5 h. The process for leaching gallium from the vanadium extraction tailings is clean and environment-friendly, and has high leaching rate.
Description
Technical Field
The invention relates to a method for leaching gallium from vanadium extraction tailings, and belongs to the technical field of extraction of gallium from vanadium extraction tailings.
Background
Gallium is one of the metal varieties with resource advantages in China. The metal gallium is the main raw material for preparing gallium nitride and gallium arsenide single crystal semiconductor materials. With the accelerated development of domestic and foreign LEDs, traditional radio frequency communication and stable development, and emerging industries such as VCSEL photoelectric chips and 5G base station construction, the demand of core materials such as gallium arsenide and gallium nitride will be continuously increased.
Vanadium titano-magnetite in Panzhihua city is listed as an important resource in western China, wherein the storage capacity of gallium is about 9.24 ten thousand tons, and accounts for over 50 percent of the gallium resource in China. The leaching process research of gallium in vanadium-titanium magnetite extraction tailings is less, the utilization technology of gallium in vanadium extraction tailings is immature, the traditional process mainly adopts an acid leaching method, a chlorination volatilization method, a pressure boiling-leaching method and a melting reduction method, but most of the methods have the defects of low extraction efficiency, resource waste or environmental pollution and the like.
To V2O5Phase structure research of the by-product vanadium extraction waste slag in the production process shows that gallium does not exist independent phase, but is dispersed and distributed in each carrier phase.
Disclosure of Invention
The invention aims to provide a novel method for leaching gallium in vanadium extraction tailings.
In order to solve the technical problem of the invention, the method for leaching gallium in the vanadium extraction tailings comprises the following steps:
A. alkali dissolution
Mixing: uniformly mixing vanadium extraction tailings and an alkali solvent, drying at 100-120 ℃ for 4.5-5 h, grinding to below 1mm, and air cooling to obtain gallium-containing residues, wherein the alkali solvent is Na2CO3NaOH, CaO, said Na2CO3CaO, NaOH: the mass ratio of the vanadium extraction tailings is as follows: 0.15-0.24: 0.4-0.45: 0.08-0.1: 0.8 to 1;
roasting: roasting the obtained gallium-containing residue at 950-1100 ℃ for 1.3-1.5 h, cooling in a furnace, and grinding to be less than 0.5 mm;
B. alkaline leaching: and C, mixing the roasted gallium-containing residue obtained in the step A with a NaOH solution, and stirring and carrying out alkaline leaching for 1.2-1.5 h.
In one embodiment, the Na2CO3CaO, NaOH: and (3) extracting vanadium tailings, namely 0.15: 0.4: 0.1: 0.8.
in a specific embodiment, water is further added into the alkali solvent in the step A, and the mass ratio of the water to the vanadium extraction tailings is 0.85-0.95: 2.8 to 2.9.
In a specific embodiment, the furnace cooling in the step A is furnace cooling to 80-100 ℃.
In a specific embodiment, the concentration of the NaOH solution in the step B is 145-155 g/L.
In a specific embodiment, the liquid-solid ratio of the NaOH solution to the alkali-soluble residue in step B is 1.0 to 1.2: 5.0 to 5.5. The liquid-solid ratio refers to the volume-mass ratio, and the unit is ml/g.
In a specific embodiment, the rotation speed of the stirring in the step B is 270-285 r/min.
In a specific embodiment, the temperature of the alkaline leaching in the step B is 85-100 ℃.
In a specific embodiment, the pressure of the alkaline leaching in the step B is 0-0.8 MPa.
In one embodiment, the leaching rate of the gallium is 98.52-99.15%.
Has the advantages that:
the process for leaching gallium from the vanadium extraction tailings is clean and environment-friendly, and has high leaching rate.
The method of the invention does not use adhesive and has low cost.
Drawings
FIG. 1 is a process diagram of an embodiment of the present invention.
Detailed Description
In order to solve the technical problem of the invention, the method for leaching gallium in the vanadium extraction tailings comprises the following steps:
A. alkali dissolution
Mixing: uniformly mixing the vanadium extraction tailings and an alkali solvent, and drying at 100-120 DEG CDrying for 4.5-5 h, grinding to below 1mm, air cooling to obtain gallium-containing residue, wherein the alkali solvent is Na2CO3NaOH, CaO, said Na2CO3CaO, NaOH: the mass ratio of the vanadium extraction tailings is as follows: 0.15-0.24: 0.4-0.45: 0.08-0.1: 0.8 to 1;
roasting: roasting the obtained gallium-containing residue at 950-1100 ℃ for 1.3-1.5 h, cooling in a furnace, and grinding to be less than 0.5 mm;
B. alkaline leaching: and C, mixing the roasted gallium-containing residue obtained in the step A with a NaOH solution, and stirring and carrying out alkaline leaching for 1.2-1.5 h.
In one embodiment, the Na2CO3CaO, NaOH: and (3) extracting vanadium tailings, namely 0.15: 0.4: 0.1: 0.8.
in a specific embodiment, water is further added into the alkali solvent in the step A, and the mass ratio of the water to the vanadium extraction tailings is 0.85-0.95: 2.8 to 2.9.
In a specific embodiment, the furnace cooling in the step A is furnace cooling to 80-100 ℃.
In a specific embodiment, the concentration of the NaOH solution in the step B is 145-155 g/L.
In a specific embodiment, the liquid-solid ratio of the NaOH solution to the alkali-soluble residue in step B is 1.0 to 1.2: 5.0 to 5.5. The liquid-solid ratio refers to the volume-mass ratio, and the unit is ml/g.
In a specific embodiment, the rotation speed of the stirring in the step B is 270-285 r/min.
In a specific embodiment, the temperature of the alkaline leaching in the step B is 85-100 ℃.
In a specific embodiment, the pressure of the alkaline leaching in the step B is 0-0.8 MPa.
In one embodiment, the leaching rate of the gallium is 98.52-99.15%.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
Mixing 100% of vanadium extraction tailings and 24%Na2CO3Uniformly mixing 40% of CaO, 8% of NaOH and 30% of water by stirring, drying for 4.5h at 100 ℃ by using drying equipment after mixing, grinding to be less than 0.8mm, placing ground gallium-containing tailings in an SX2-10-13 resistance furnace for roasting for 1.5h, and controlling the roasting temperature to be 950 ℃ by using a temperature controller of the resistance furnace. Cooling the furnace to about 85 ℃ after roasting, taking out the gallium-containing waste residue, mashing and grinding the gallium-containing waste residue to be below 0.2mm, wherein the alkaline leaching time is 1.5h, and the pressure of the alkaline leaching is 0.8 MPa. Mixing the alkali-soluble residue with 150g/L NaOH at a liquid-solid ratio of 1 ml: 5.5g of the raw materials are mixed and stirred, the stirring is carried out at the rotating speed of 270r/min, the temperature is controlled at 85 ℃ by adopting an electronic constant-temperature water bath kettle, and the mixture is stirred and leached. The leaching rate of gallium was 98.52%.
Example 2
Similar to example 1, except that Na2CO3CaO, NaOH: and (3) extracting vanadium tailings, namely 0.15: 0.4: 0.1: 0.8. the leaching rate of gallium is 99.15%.
Comparative example 1
Similar to example 1, except that NaOH, CaO, vanadium extraction tailings are added in a ratio of 0.4:1: 1; and placing the ground gallium-containing tailings in an SX2-10-13 resistance furnace for roasting for 1.5 h. The leaching rate of gallium was 67.9%.
Claims (10)
1. The method for leaching gallium in vanadium extraction tailings is characterized by comprising the following steps:
A. alkali dissolution
Mixing: uniformly mixing vanadium extraction tailings and an alkali solvent, drying at 100-120 ℃ for 4.5-5 h, grinding to below 1mm, and air cooling to obtain gallium-containing residues, wherein the alkali solvent is Na2CO3NaOH, CaO, said Na2CO3CaO, NaOH: the mass ratio of the vanadium extraction tailings is as follows: 0.15-0.24: 0.4-0.45: 0.08-0.1: 0.8 to 1;
roasting: roasting the obtained gallium-containing residue at 950-1100 ℃ for 1.3-1.5 h, cooling in a furnace, and grinding to be less than 0.5 mm;
B. alkaline leaching: and C, mixing the roasted gallium-containing residue obtained in the step A with a NaOH solution, and stirring and carrying out alkaline leaching for 1.2-1.5 h.
2. According to claimThe method for leaching gallium in vanadium extraction tailings of claim 1, wherein the Na is2CO3CaO, NaOH: and (3) extracting vanadium tailings, namely 0.15: 0.4: 0.1: 0.8.
3. the method for leaching gallium in vanadium extraction tailings according to claim 1 or 2, wherein water is further added to the alkali solvent in the step A, and the mass ratio of the water to the vanadium extraction tailings is 0.85-0.95: 2.8 to 2.9.
4. The method for leaching gallium in vanadium extraction tailings according to any one of claims 1 to 3, wherein the furnace cooling in the step A is furnace cooling to 80-100 ℃.
5. The method for leaching gallium in vanadium extraction tailings according to any one of claims 1 to 4, wherein the concentration of the NaOH solution in the step B is 145 to 155 g/L.
6. The method for leaching gallium in vanadium extraction tailings according to any one of claims 1 to 5, wherein the liquid-solid ratio of the NaOH solution to the alkali-soluble residue in the step B is 1.0-1.2: 5.0 to 5.5.
7. The method for leaching gallium from vanadium extraction tailings according to any one of claims 1 to 6, wherein the rotation speed of stirring in the step B is 270 to 285 r/min.
8. The method for leaching gallium in vanadium extraction tailings according to any one of claims 1 to 7, wherein the temperature of the alkaline leaching in the step B is 85 to 100 ℃.
9. The method for leaching gallium in vanadium extraction tailings according to any one of claims 1 to 8, wherein the pressure of the alkaline leaching in the step B is 0 to 0.8 MPa.
10. The method for leaching gallium from vanadium extraction tailings according to any one of claims 1 to 8, wherein the leaching rate of gallium is 98.52 to 99.15%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113667840A (en) * | 2021-08-24 | 2021-11-19 | 安徽工业大学 | Method for extracting gallium metal by wet processing gallium nitride waste |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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2021
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113667840A (en) * | 2021-08-24 | 2021-11-19 | 安徽工业大学 | Method for extracting gallium metal by wet processing gallium nitride waste |
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Application publication date: 20210709 |