CN117985741A - Comprehensive recycling method of lepidolite lithium extraction slag - Google Patents
Comprehensive recycling method of lepidolite lithium extraction slag Download PDFInfo
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- CN117985741A CN117985741A CN202211332403.7A CN202211332403A CN117985741A CN 117985741 A CN117985741 A CN 117985741A CN 202211332403 A CN202211332403 A CN 202211332403A CN 117985741 A CN117985741 A CN 117985741A
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- Prior art keywords
- lithium extraction
- extraction slag
- lepidolite
- filtrate
- alkali
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 59
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052629 lepidolite Inorganic materials 0.000 title claims abstract description 42
- 238000000605 extraction Methods 0.000 title claims abstract description 39
- 239000002893 slag Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004064 recycling Methods 0.000 title claims abstract description 21
- 239000003513 alkali Substances 0.000 claims abstract description 24
- 238000002386 leaching Methods 0.000 claims abstract description 19
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 230000001376 precipitating effect Effects 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000002244 precipitate Substances 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 19
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- 239000007791 liquid phase Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 9
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 9
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 9
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 9
- 235000011151 potassium sulphates Nutrition 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000003916 acid precipitation Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- 229910052700 potassium Inorganic materials 0.000 abstract description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 9
- 238000011084 recovery Methods 0.000 description 7
- -1 silicate ions Chemical class 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 125000005624 silicic acid group Chemical group 0.000 description 4
- 229910018068 Li 2 O Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000010405 anode material Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000003469 silicate cement Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- 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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- Manufacture And Refinement Of Metals (AREA)
Abstract
A comprehensive recycling method of lepidolite lithium extraction slag comprises the following steps: (1) adding alkali for leaching; (2) adding acid to precipitate; (3) evaporating and concentrating; (4) adding alkali to remove impurities; and (5) precipitating lithium. According to the invention, a new thought is adopted to recycle valuable metal elements in the lepidolite lithium extraction slag, so that residual lithium, aluminum and potassium elements in the lepidolite lithium extraction slag are effectively recycled, and the method has higher economic value; the invention has simple process and equipment and low investment.
Description
Technical Field
The invention relates to a method for utilizing solid waste resources, in particular to a method for recycling lepidolite lithium extraction slag.
Background
With the development of new energy industry, the demand of battery anode materials is improved rapidly. Lithium batteries are favored by many battery manufacturers because of their high safety factor and high charge capacity per unit mass. The demand for lithium resources as a raw material is also greatly increasing.
Lepidolite is an important solid lithium-containing mineral. Under the current technical conditions, more than ten tons of solid waste residues can be generated in the process of preparing one ton of lithium carbonate by leaching and extracting from lepidolite ore. The stacking of the waste residues occupies space and pollutes the environment, and the waste residues contain valuable elements such as Li, K, al and the like, so that the method has certain economic value.
At present, a small amount of lepidolite lithium extraction slag is used in the field of building materials, CN103979809A discloses a method for preparing white silicate cement with little clinker by using lepidolite lithium extraction slag, CN102126838A discloses a method for preparing lightweight building material ceramsite by using lepidolite lithium extraction slag, and CN102125786A discloses a method for preparing porous ceramsite filter material by using lepidolite lithium extraction slag. The development work of comprehensively recycling lepidolite lithium extraction slag is less, and the utilization of valuable elements in the lepidolite lithium extraction slag is insufficient.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a comprehensive recycling method of lepidolite lithium extraction slag capable of recycling Li, K and Al elements.
The technical scheme adopted for solving the technical problems is as follows: a comprehensive recycling method of lepidolite lithium extraction slag comprises the following steps:
(1) Adding alkali for leaching: mixing the lepidolite lithium extraction residue raw material with an alkali solution, stirring and leaching, and filtering to obtain filtrate and filter residues;
(2) Acid precipitation: adding acid into the filtrate obtained in the step (1) until the filtrate becomes acidic, and filtering to obtain filtrate and precipitate; the sediment is silicic acid;
(3) And (3) evaporating and concentrating: evaporating and concentrating the filtrate obtained in the step (2), and performing solid-liquid separation through evaporation crystallization or cooling crystallization to obtain potassium sulfate crystals and filtrate; the step can recover potassium sulfate and improve the concentration of lithium ions at the same time;
(4) Adding alkali to remove impurities: adding alkali into the filtrate obtained in the step (3) until the filtrate is weakly acidic, neutral or weakly alkaline, and filtering to obtain filtrate and precipitate; the obtained filtrate is a high-concentration lithium-containing solution, and the precipitate is aluminum hydroxide;
(5) Precipitating lithium: and (3) adding sodium carbonate into the filtrate obtained in the step (4), and obtaining lithium carbonate precipitate after the reaction is completed.
Preferably, in the step (1), the particle size of the lepidolite lithium extraction slag raw material is 100-500 meshes. The lithium extraction slag is seriously agglomerated, so that raw materials with smaller granularity are preferable; if the particles of the lepidolite lithium extraction slag raw material are larger, the lepidolite lithium extraction slag raw material can be crushed in advance.
Preferably, in step (1), the alkali solution is a sodium hydroxide solution and/or a potassium hydroxide solution.
Preferably, in the step (1), the concentration of the alkali solution is 1-10 mol/L.
Preferably, in the step (1), the ratio of the lepidolite lithium extraction slag raw material to the hydroxyl in the alkali solution is 1 kg:1-10 mol. Under the condition, the unstable structure of the lithium extraction slag with volcanic ash activity in alkaline solution is destroyed, and lithium ions, potassium ions, metaaluminate ions and silicate ions are released.
Preferably, in the step (1), the temperature during the stirring leaching is 20-95 ℃, and the time of the stirring leaching is 30-600 min.
Preferably, in step (2), the acid is sulfuric acid.
Preferably, in the step (2), the pH of the reaction end point of the acid addition is 3 to 6. In this process, silicate ions combine with hydrogen ions to form silicic acid precipitates, and metaaluminate ions react with hydrogen ions to form aluminum ions.
Preferably, in the step (3), the temperature of the evaporation concentration is 60-90 ℃.
Preferably, in the step (3), the concentration multiple of evaporation concentration is 15-50 times, and then the temperature is reduced to 20-30 ℃ for crystallization.
Preferably, in step (4), the base is sodium hydroxide.
Preferably, in the step (4), the reaction end point pH value of the alkali addition is 6.8-7.5. The aluminum ions are completely precipitated into aluminum hydroxide, and the aluminum hydroxide and filtrate are obtained by filtration.
Preferably, in step (5), sodium carbonate is added by adding a saturated sodium carbonate solution.
Preferably, in the step (5), the reaction time is 0.2 to 3 hours, and the reaction temperature is 60 to 100 ℃.
Preferably, in step (5), the remaining liquid phase after the completion of the reaction is returned to step (4) for use as a saturated sodium carbonate solution.
The invention has the beneficial effects that:
1. According to the invention, a new thought is adopted to recycle valuable metal elements in the lepidolite lithium extraction slag, so that residual lithium, aluminum and potassium elements in the lepidolite lithium extraction slag are effectively recycled, and the method has higher economic value;
2. The invention has simple process and equipment and low investment.
Detailed Description
The invention is further illustrated by the following examples.
The starting materials used in the examples of the present invention were all obtained by conventional commercial means.
Example 1
The comprehensive recycling method of lepidolite lithium extraction slag in the embodiment comprises the following steps:
Crushing and preprocessing raw materials: aiming at lepidolite leaching residues, wherein the content of SiO 2 is 44.3%, the content of Al 2O3 is 10.4%, the content of CaO is 25.1%, the content of Li 2 O is 0.57% and the content of K 2 O is 5.5%. Crushing the raw materials to below 200 meshes, namely below 74 μm.
(1) Adding alkali for leaching: adding 2mol/L sodium hydroxide solution into the crushed raw materials at a solid-to-liquid ratio of 1:3, leaching at 60 ℃ for 90min, and filtering to obtain filtrate and filter residues;
(2) Acid precipitation: adding sulfuric acid into the filtrate obtained in the step (1), controlling the pH of the reaction end point to be 3.5, and filtering to obtain filtrate and precipitate, wherein the precipitate is silicic acid precipitate;
(3) And (3) evaporating and concentrating: heating the filtrate obtained in the step (2) to 90 ℃, evaporating and concentrating for 25 times, cooling to 20 ℃, and filtering to obtain potassium sulfate precipitate and filtrate;
(4) Adding alkali to remove impurities: adding sodium hydroxide into the filtrate obtained in the step (3), and filtering to obtain an aluminum hydroxide precipitate and a lithium-containing liquid phase, wherein the pH of the reaction end point is 7;
(5) Precipitating lithium: adding an excessive saturated sodium carbonate solution into a lithium-containing liquid phase, reacting for 1h at 90 ℃, and filtering to obtain lithium carbonate; the filtered liquid phase is returned to the step (4) and used as saturated sodium carbonate solution.
The test shows that the main content of potassium sulfate is 92.13%, and the recovery rate is 70.65%. The main content of aluminum hydroxide is 89.03 percent, and the recovery rate is 97.72 percent. The main content of the dried lithium carbonate is 98.63%, the single-time yield is 85.00%, and the continuous reaction yield is 95.50%.
Example 2
The comprehensive recycling method of lepidolite lithium extraction slag in the embodiment comprises the following steps:
Crushing and preprocessing raw materials: aiming at lepidolite leaching residues, the content of SiO 2 is 50.2%, the content of Al 2O3 is 8.5%, the content of CaO is 24.7%, the content of Li 2 O is 1.12% and the content of K 2 O is 7.0%. Crushing the raw materials to below 300 meshes, namely below 48 mu m.
(1) Adding alkali for leaching: adding 1mol/L potassium hydroxide solution into the crushed raw materials at a solid-to-liquid ratio of 1:1, leaching for 120min at 90 ℃, and filtering to obtain filtrate and filter residues;
(2) Acid precipitation: adding sulfuric acid into the filtrate obtained in the step (1), controlling the pH of the reaction end point to be 4, and filtering to obtain filtrate and precipitate, wherein the precipitate is silicic acid precipitate;
(3) And (3) evaporating and concentrating: heating the filtrate obtained in the step (2) to 90 ℃, evaporating and concentrating for 20 times, cooling to 25 ℃, and filtering to obtain potassium sulfate precipitate and filtrate;
(4) Adding alkali to remove impurities: adding sodium hydroxide into the filtrate obtained in the step (3), and filtering to obtain an aluminum hydroxide precipitate and a lithium-containing liquid phase, wherein the pH of the reaction end point is 7.2;
(5) Precipitating lithium: adding an excessive saturated sodium carbonate solution into a lithium-containing liquid phase, reacting for 1.5 hours at 80 ℃, and filtering to obtain lithium carbonate; the filtered liquid phase is returned to the step (4) and used as saturated sodium carbonate solution.
The test shows that the main content of potassium sulfate is 92.50%, and the recovery rate is 89.65%. The main content of aluminum hydroxide is 89.57 percent, and the recovery rate is 98.00 percent. The main content of the dried lithium carbonate is 98.76%, the single reaction recovery rate is 85.55%, and the continuous reaction yield is 95.50%.
Example 3
The comprehensive recycling method of lepidolite lithium extraction slag in the embodiment comprises the following steps:
Crushing and preprocessing raw materials: aiming at lepidolite leaching residues, the content of SiO 2 is 48.2%, the content of Al 2O3 is 9.4%, the content of CaO is 23.5%, the content of Li 2 O is 0.85% and the content of K 2 O is 6.7%. The raw materials are crushed to 140 meshes or less, namely, 106 μm or less.
(1) Adding alkali for leaching: adding 2mol/L sodium hydroxide solution into the crushed raw materials at a solid-to-liquid ratio of 1:3.5, leaching at 80 ℃ for 45min, and filtering to obtain filtrate and filter residues;
(2) Acid precipitation: adding sulfuric acid into the filtrate obtained in the step (1), controlling the pH of the reaction end point to be 4.5, and filtering to obtain filtrate and precipitate, wherein the precipitate is silicic acid precipitate;
(3) And (3) evaporating and concentrating: heating the filtrate obtained in the step (2) to 87 ℃, evaporating and concentrating for 22 times, cooling to 22 ℃, and filtering to obtain potassium sulfate precipitate and filtrate;
(4) Adding alkali to remove impurities: adding sodium hydroxide into the filtrate obtained in the step (3), and filtering to obtain an aluminum hydroxide precipitate and a lithium-containing liquid phase, wherein the pH of the reaction end point is 7.4;
(5) Precipitating lithium: adding an excessive saturated sodium carbonate solution into a lithium-containing liquid phase, reacting for 2 hours at 85 ℃, and filtering to obtain lithium carbonate; the filtered liquid phase is returned to the step (4) and used as saturated sodium carbonate solution.
The test shows that the main content of potassium sulfate is 92.90 percent and the recovery rate is 68.55 percent. The main content of aluminum hydroxide is 89.45 percent, and the recovery rate is 98.20 percent. The main content of the dried lithium carbonate is 98.86%, the single-time yield is 85.12%, and the continuous reaction yield is 95.50%.
Claims (10)
1. The comprehensive recycling method of the lepidolite lithium extraction slag is characterized by comprising the following steps of:
(1) Adding alkali for leaching: mixing the lepidolite lithium extraction residue raw material with an alkali solution, stirring and leaching, and filtering to obtain filtrate and filter residues;
(2) Acid precipitation: adding acid into the filtrate obtained in the step (1) until the filtrate becomes acidic, and filtering to obtain filtrate and precipitate;
(3) And (3) evaporating and concentrating: evaporating and concentrating the filtrate obtained in the step (2), and performing solid-liquid separation through evaporation crystallization or cooling crystallization to obtain potassium sulfate crystals and filtrate;
(4) Adding alkali to remove impurities: adding alkali into the filtrate obtained in the step (3) until the filtrate is weakly acidic, neutral or weakly alkaline, and filtering to obtain filtrate and precipitate;
(5) Precipitating lithium: and (3) adding sodium carbonate into the filtrate obtained in the step (4), and obtaining lithium carbonate precipitate after the reaction is completed.
2. The method for comprehensively recycling lepidolite lithium extraction slag according to claim 1, wherein in the step (1), the granularity of the lepidolite lithium extraction slag raw material is 100-500 meshes; the alkali solution is sodium hydroxide solution and/or potassium hydroxide solution; the concentration of the alkali solution is 1-10 mol/L.
3. The method for comprehensively recycling lepidolite lithium extraction slag according to claim 1 or 2, wherein in the step (1), the ratio of lepidolite lithium extraction slag raw material to hydroxide in the alkaline solution is 1 kg:1-10 mol.
4. The method for comprehensively recycling lepidolite lithium extraction slag according to any one of claims 1 to 3, wherein in the step (1), the temperature during the stirring leaching is 20 to 95 ℃, and the time of the stirring leaching is 30 to 600min.
5. The method for comprehensively recycling lepidolite lithium extraction slag according to any one of claims 1 to 4, wherein in the step (2), the acid is sulfuric acid; the pH value of the reaction end point of the acid addition is 3-6.
6. The method for comprehensively recycling lepidolite lithium extraction slag according to any one of claims 1 to 5, wherein in the step (3), the evaporating concentration temperature is 60 to 90 ℃.
7. The method for comprehensively recycling lepidolite lithium extraction slag according to any one of claims 1 to 6, wherein in the step (3), the concentration multiple of evaporation concentration is 15 to 50 times, and then the temperature is reduced to 20 to 30 ℃ for crystallization.
8. The method for comprehensively recycling lepidolite lithium extraction slag according to any one of claims 1 to 7, wherein in the step (4), the alkali is sodium hydroxide; the pH value of the reaction end point of the alkali addition is 6.8-7.5.
9. The comprehensive recycling method of lepidolite lithium extraction slag according to any one of claims 1 to 8, characterized in that in step (5), sodium carbonate is added by adding saturated sodium carbonate solution; the reaction time is 0.2-3 h, and the reaction temperature is 60-100 ℃.
10. The comprehensive recycling method of lepidolite lithium extraction slag according to any one of claims 1 to 9, characterized in that in the step (5), the residual liquid phase after the completion of the reaction is returned to the step (4) to be used as a saturated sodium carbonate solution.
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| CN202211332403.7A CN117985741A (en) | 2022-10-28 | 2022-10-28 | Comprehensive recycling method of lepidolite lithium extraction slag |
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| CN202211332403.7A CN117985741A (en) | 2022-10-28 | 2022-10-28 | Comprehensive recycling method of lepidolite lithium extraction slag |
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