CN114053993A - Preparation method of aluminum-based layered lithium adsorbent - Google Patents
Preparation method of aluminum-based layered lithium adsorbent Download PDFInfo
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- CN114053993A CN114053993A CN202110424404.3A CN202110424404A CN114053993A CN 114053993 A CN114053993 A CN 114053993A CN 202110424404 A CN202110424404 A CN 202110424404A CN 114053993 A CN114053993 A CN 114053993A
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 56
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 46
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 8
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 15
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical group Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 238000003756 stirring Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- 238000001035 drying Methods 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 230000003213 activating effect Effects 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000012267 brine Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910007857 Li-Al Inorganic materials 0.000 description 1
- 229910008447 Li—Al Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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Abstract
The invention provides a preparation method of an aluminum-based layered lithium adsorbent, which comprises the following steps: uniformly mixing a lithium source and an aluminum source in water, adjusting the pH value, heating to 80-120 ℃ at a first rate of 3-8 ℃/min under the condition of microwave, carrying out heat preservation treatment for 1-5 min, heating to 150-170 ℃ at a second rate of 5-15 ℃/min, and carrying out heat preservation treatment for 1-3 h to obtain an aluminum-based layered lithium adsorbent; wherein the first rate is less than the second rate. The aluminum-based layered lithium adsorbent is prepared by a microwave hydrothermal method in two steps, the aluminum-based layered lithium adsorbent can be prepared in a short time, and the obtained aluminum-based layered lithium adsorbent is high in adsorption speed and adsorption capacity and can be repeatedly used.
Description
Technical Field
The invention relates to the technical field of wet metallurgy, in particular to a preparation method of an aluminum-based layered lithium adsorbent.
Background
The adsorption method is one of effective methods for extracting lithium from brine, and the aluminum hydroxide-based lithium adsorbent is the only adsorbent industrially applied when the adsorption method is adopted to extract lithium from brine. Regardless of the method used to prepare the adsorbent, the main component of the basic framework of the adsorbent is aluminum hydroxide, and thus the adsorbent is referred to herein as an aluminum hydroxide-based lithium adsorbent. The adsorbent has low preparation cost, and the cost is low no matter the raw materials or the preparation process are adopted.
The aluminum hydroxide-based lithium adsorbent is generally prepared by a hydrothermal synthesis method, but in the traditional hydrothermal synthesis or medium heat transfer process, the temperature rise process is slow and low in efficiency, and meanwhile, a temperature gradient exists between a reaction container and a reactant, so that the synthesis process is long, and the adsorption capacity of the obtained adsorbent is low.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide a method for preparing an aluminum-based layered lithium adsorbent, which can rapidly prepare the aluminum-based layered lithium adsorbent, and the obtained adsorbent has high adsorption capacity.
The invention provides a preparation method of an aluminum-based layered lithium adsorbent, which comprises the following steps:
uniformly mixing a lithium source and an aluminum source in water, adjusting the pH value, heating to 80-120 ℃ at a first rate of 3-8 ℃/min under the condition of microwave, carrying out heat preservation treatment for 1-5 min, heating to 150-170 ℃ at a second rate of 5-15 ℃/min, and carrying out heat preservation treatment for 1-3 h to obtain an aluminum-based layered lithium adsorbent;
wherein the first rate is less than the second rate.
In one embodiment, the lithium source is selected from one or more of lithium chloride, lithium hydroxide, or lithium nitrate; the aluminum source is selected from aluminum chloride.
In one embodiment, the pH is adjusted to a value of 5.6 to 7.5.
In one embodiment, the frequency of the microwave is 500 to 800W.
In one embodiment, the molar ratio of the lithium source to the aluminum source is 1 to 3: 1.
in one embodiment, the molar ratio of the lithium source to the aluminum source is 1.4: 1.
in one embodiment, the incubation treatment is carried out at a first rate of 6.7 ℃/min up to 100 ℃ for 3min, and then at a second rate of 10 ℃/min up to 160 ℃ for 2 h.
The method comprises the steps of preparing the aluminum-based layered lithium adsorbent by a microwave hydrothermal method in two steps, mixing a lithium source and an aluminum source uniformly in water, adjusting the pH value, heating to 80-120 ℃ at a first rate of 3-8 ℃/min under the condition of microwave, carrying out heat preservation treatment for 1-5 min, heating to 150-170 ℃ at a second rate of 5-15 ℃/min, carrying out heat preservation treatment for 1-3 h, and thus obtaining the aluminum-based layered lithium adsorbent. The method provided by the invention can prepare the aluminum-based layered lithium adsorbent in a short time, and the obtained aluminum-based layered lithium adsorbent has high adsorption speed and high adsorption capacity and can be repeatedly used for many times. Experimental results show that when the adsorbent provided by the invention is used for adsorbing a lithium-containing solution, the adsorption capacity of the adsorbent can reach 5.5 mg/g. After 5 times of repeated adsorption and elution tests, the adsorption amount is stabilized at 2.35 mg/g.
Drawings
FIG. 1 is an XRD pattern of an adsorbent provided by an embodiment of the present invention;
FIG. 2 is a graph showing the adsorption capacity obtained in example 1 of the present invention.
Detailed Description
The preparation method provided by the invention is described in detail by combining the following examples.
Example 1
Mixing AlCl3And LiCl in a molar ratio of Al to Li of 1.4: 1 are respectively dissolved in deionized water, stirred evenly, added with 1mol/L sodium hydroxide while stirring until the pH value is 6, and stirred for 30 min; placing the obtained mixture in a microwave hydrothermal parallel synthesizer, heating to 100 ℃ at the speed of 6.7 ℃/min with the microwave power of 600W, preserving heat for 3min, heating to 160 ℃ at the speed of 10 ℃/min, preserving heat for 2h, cooling, washing the obtained reaction product with deionized water for 3 times, drying at 60 ℃, stirring in the deionized water, activating, extracting lithium, and drying to obtain the aluminum-based layered adsorbent.
The aluminum-based layered lithium adsorbent was characterized by X-ray diffraction (XRD), and referring to fig. 1, fig. 1 is an XRD pattern of the adsorbent provided by the embodiment of the present invention. The results show that the product has a highly crystalline Li-Al LDH phase with no significant impure phases.
Weighing 1g of the aluminum-based layered adsorbent, putting the aluminum-based layered adsorbent into 200mL of LiCl solution with the lithium ion concentration of 1000mg/L, performing adsorption experiments under the conditions of normal temperature and stirring, sampling at different time points, and measuring Li in the solution at the moment+The adsorption capacity was calculated from the concentration, and the experimental results are shown in FIG. 2, and FIG. 2 is a graph showing the adsorption capacity obtained in example 1 of the present invention. As can be seen from FIG. 2, when the lithium-containing solution is adsorbed by the adsorbent provided by the invention, the adsorption is nearly saturated after 2h, and at the moment, the LiCl solution Li is adsorbed by the adsorbent+The adsorption capacity reached 5.5 mg/g.
After the adsorption elution test is repeated for 5 times, the adsorption quantity of the aluminum-based layered lithium adsorbent is stabilized at 2.35 mg/g.
Example 2
Mixing AlCl3And LiCl in a molar ratio of Al to Li of 1.6: 1 are respectively dissolved in deionized water, stirred evenly, added with 1mol/L sodium hydroxide while stirring until the pH value is 6, and stirred for 30 min; placing the obtained mixture in a microwave hydrothermal parallel synthesizer, heating to 100 ℃ at the speed of 6.7 ℃/min with the microwave power of 600W, preserving heat for 3min, heating to 1600 ℃ at the speed of 10 ℃/min, preserving heat for 2h, cooling, washing the obtained reaction product with deionized water for 3 times, drying at 60 ℃, stirring in the deionized water, activating, extracting lithium, and drying to obtain the aluminum-based layered adsorbent.
Weighing 1g of the aluminum-based layered adsorbent, putting the aluminum-based layered adsorbent into 200mL of LiCl solution with the lithium ion concentration of 1000mg/L, and performing an adsorption experiment under the conditions of normal temperature and stirring, wherein the adsorbent is used for adsorbing LiCl solution Li+The adsorption capacity was 4.8 mg/g.
Example 3
Mixing AlCl3And LiCl in a molar ratio of Al to Li of 1.8: 1 are respectively dissolved in deionized water, stirred evenly, added with 1mol/L sodium hydroxide while stirring until the pH value is 5.5, and stirred for 30 min; placing the obtained mixture in a microwave hydrothermal parallel synthesizer, heating to 100 deg.C at a speed of 6.7 deg.C/min with a microwave power of 800W, holding for 3min, and heating to 10 deg.CHeating to 160 ℃ at a speed of/min, preserving heat for 2h, cooling, washing the obtained reaction product with deionized water for 3 times, drying at 60 ℃, stirring in the deionized water for activating and extracting lithium, and drying to obtain the aluminum-based layered adsorbent.
Weighing 1g of the aluminum-based layered adsorbent, putting the aluminum-based layered adsorbent into 200mL of LiCl solution with the lithium ion concentration of 1000mg/L, and performing an adsorption experiment under the conditions of normal temperature and stirring, wherein the adsorbent is used for adsorbing LiCl solution Li+The adsorption capacity was 3.6 mg/g.
Example 4
Mixing AlCl3And LiCl in a molar ratio of Al to Li of 2: 1 are respectively dissolved in deionized water, stirred evenly, added with 1mol/L sodium hydroxide while stirring until the pH value is 5.5, and stirred for 30 min; placing the obtained mixture in a microwave hydrothermal parallel synthesizer, heating to 100 ℃ at the speed of 6.7 ℃/min with the microwave power of 800W, preserving heat for 3min, heating to 160 ℃ at the speed of 10 ℃/min, preserving heat for 2h, cooling, washing the obtained reaction product with deionized water for 3 times, drying at 60 ℃, stirring in the deionized water, activating, extracting lithium, and drying to obtain the aluminum-based layered adsorbent.
Weighing 1g of the aluminum-based layered adsorbent, putting the aluminum-based layered adsorbent into 200mL of LiCl solution with the lithium ion concentration of 1000mg/L, and performing an adsorption experiment under the conditions of normal temperature and stirring, wherein the adsorbent is used for adsorbing LiCl solution Li+The adsorption capacity was 2.1 mg/g.
Example 5
Mixing AlCl3And LiCl in a molar ratio of Al to Li of 1.4: 1 are respectively dissolved in deionized water, stirred evenly, added with 1mol/L sodium hydroxide while stirring until the pH value is 6, and stirred for 30 min; placing the obtained mixture in a microwave hydrothermal parallel synthesizer, heating to 100 ℃ at the speed of 6.7 ℃/min with the microwave power of 600W, preserving heat for 3min, heating to 160 ℃ at the speed of 15 ℃/min, preserving heat for 2h, cooling, washing the obtained reaction product with deionized water for 3 times, drying at 60 ℃, stirring in the deionized water, activating, extracting lithium, and drying to obtain the aluminum-based layered adsorbent.
Weighing 1g of the aluminum-based layered adsorbent, putting the aluminum-based layered adsorbent into 200mL of LiCl solution with the lithium ion concentration of 1000mg/L, and adsorbing the aluminum-based layered adsorbent under the conditions of normal temperature and stirringAdsorption experiment, adsorbent to LiCl solution Li+The adsorption capacity was 3.9 mg/g.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of an aluminum-based layered lithium adsorbent comprises the following steps:
uniformly mixing a lithium source and an aluminum source in water, adjusting the pH value, heating to 80-120 ℃ at a first rate of 3-8 ℃/min under the condition of microwave, carrying out heat preservation treatment for 1-5 min, heating to 150-170 ℃ at a second rate of 5-15 ℃/min, and carrying out heat preservation treatment for 1-3 h to obtain an aluminum-based layered lithium adsorbent;
wherein the first rate is less than the second rate.
2. The method of claim 1, wherein the lithium source is selected from one or more of lithium chloride, lithium hydroxide, or lithium nitrate;
the aluminum source is selected from aluminum chloride.
3. The method according to claim 1, wherein the pH is adjusted to 5.6 to 7.5.
4. The method according to claim 1, wherein the microwave has a frequency of 500 to 800W.
5. The preparation method according to claim 1, wherein the molar ratio of the lithium source to the aluminum source is 1 to 3: 1.
6. the production method according to claim 5, wherein the molar ratio of the lithium source to the aluminum source is 1.4: 1.
7. the method according to claim 1, wherein the temperature is raised to 100 ℃ at a first rate of 6.7 ℃/min for 3min, and then raised to 160 ℃ at a second rate of 10 ℃/min for 2 h.
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CN117358196A (en) * | 2023-09-20 | 2024-01-09 | 中国地质科学院矿产资源研究所 | Preparation method of bauxite-based aluminum lithium ion adsorbent and brine lithium extraction method |
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CN117358196B (en) * | 2023-09-20 | 2024-03-15 | 中国地质科学院矿产资源研究所 | Preparation method of bauxite-based aluminum lithium ion adsorbent and brine lithium extraction method |
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