Magnetic lithium extraction adsorbent, and preparation method therefor and use thereof

The preparation of microspherical magnetic lithium-extracting adsorbents through electrostatic spraying technology has solved the problems of large particles and small surface area of ​​traditional adsorbents, and achieved efficient solid-liquid separation and high-capacity lithium-extracting effects.

WO2025118100A1PCT designated stage expired Publication Date: 2025-06-12GUANGDONG BRUNP RECYCLING TECH CO LTD +1
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Patent Information

Application Number
PCT/CN2023/136096
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Filing Date
2023-12-04
Publication Date
2025-06-12

AI Technical Summary

Technical Problem

During the granulation process, traditional lithium adsorbents have large particles and small surface area, making it difficult to fully exert the lithium extraction capacity. At the same time, the structural stability of magnetic adsorbents is poor, making it difficult to achieve solid-liquid separation through magnetic separation.

Method used

Electrostatic spraying technology is used to drop the mixed solution of iron salt, ferrous salt, aluminum salt and hydrophilic organic polymer into the mixed solution of alkali-lithium salt-ammonium carbonate-ethanol to form a microsphere-shaped magnetic lithium extract adsorbent, and a magnetic adsorbent is obtained through post-treatment.

Benefits of technology

The prepared magnetic lithium extract adsorbent particles have small particle size, large specific surface area, and good magnetic properties. Solid-liquid separation can be achieved through magnets. The lithium extraction process is simpler. The adsorption capacity can reach more than 9.54 mg/g, and the capacity retention rate can reach more than 96.84% after 100 cycles.

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Abstract

Provided are a magnetic lithium extraction adsorbent, and a preparation method therefor and the use thereof. The preparation method comprises the following steps: (1) mixing an iron salt, a ferrous salt, an aluminum salt and a hydrophilic organic polymer with a solvent to obtain a mixed solution; (2) adding the mixed solution into an alkali-lithium salt-ammonium carbonate-ethanol mixed solution dropwise via an electrostatic spraying device by using an injection pump to obtain microspheres; and (3) carrying out a post-treatment on the microspheres to obtain a magnetic lithium extraction adsorbent. The adsorbent prepared by means of the method is magnetic and can realize solid-liquid separation by means of a magnet, without filtering brine and other operations, such that a lithium extraction process is simpler and more convenient.
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Description

A magnetic lithium extraction adsorbent and its preparation method and application Technical Field

[0001] The present invention belongs to the technical field of lithium extraction from salt lakes and relates to a magnetic lithium extraction adsorbent and a preparation method and application thereof. Background Art

[0002] With the continuous advancement of science and technology and the rapid development of the new energy, metallurgy, and aerospace industries, the demand for lithium in various fields has continued to rise. The content of lithium in the Earth's crust is very low, with a small amount found in rock deposits and the majority contained in salt lake brines. China is a major producer of lithium from salt lake brines, accounting for over 80% of the country's lithium resources and approximately one-third of the world's. Preliminary estimates suggest that lithium salt reserves reach tens of millions of tons.

[0003] Currently, the main lithium extraction technologies in China include electrodialysis, extraction, precipitation, calcination, and adsorption. Different salt lakes require different processes and preparation methods. The first four processes are more suitable for extracting high-concentration lithium resources from salt lake brine. However, significant lithium losses occur during the conversion of raw brine into raw brine. Therefore, direct lithium extraction from raw brine reduces resource waste, making adsorption a more competitive method.

[0004] Traditional lithium adsorbents need to be granulated, but the adsorbent particles after granulation are large and have a small specific surface area, making it difficult to fully utilize the adsorbent's lithium extraction capacity.

[0005] CN111644145A discloses a method for preparing a magnetic adsorbent, in which an aluminum-based adsorbent is grown on the surface of a magnetic material. However, this bonding method relies solely on molecular bonds. During the adsorption process, the aluminum-based adsorbent expands and contracts in volume due to the insertion and removal of lithium ions, making it easy for the outer layer to separate from the inner core.

[0006] CN108607503A discloses a magnetic adsorbent for extracting lithium from brine with a high magnesium-to-lithium ratio in salt lakes and an application method thereof. Zeolite powder with a particle size of 100-300 μm is screened, a manganese salt solution is added thereto, and then lithium hydroxide is added. The zeolite powder is used as a template to form a lithium ion adsorbent LiMn2O4 in the zeolite micropores. The surface of the lithium ion adsorbent LiMn2O4 particles is coated with a nano-silicon dioxide dispersion, and Fe3O4 or γ-Fe2O3 magnetic powder and calcium chloride are further adhered thereto. Calcium silicate is formed by the nano-silicon dioxide and calcium chloride to firmly fix the magnetic powder on the surface. The powder is dried to obtain a spherical magnetic powder with a porous outer layer.

[0007] The magnetic adsorbent material prepared by the above scheme has poor structural stability, and the prepared adsorbent particles are small, and are difficult to be separated by magnetism when dissolved or dispersed in a solution, resulting in adsorbent loss.

[0008] Summary of the Invention

[0009] The following is a summary of the subject matter described in detail herein. This summary is not intended to limit the scope of the claims.

[0010] The purpose of the present disclosure is to provide a magnetic lithium extraction adsorbent and its preparation method and application. The adsorbent prepared by the method described in the present disclosure has magnetism, and solid-liquid separation can be achieved by magnets. There is no need to filter the brine, etc., and the lithium extraction process is simpler.

[0011] To achieve this purpose, the present disclosure adopts the following technical solutions:

[0012] In a first aspect, the present disclosure provides a method for preparing a magnetic lithium extraction adsorbent, the preparation method comprising the following steps:

[0013] (1) mixing a ferric salt, a ferrous salt, an aluminum salt, and a hydrophilic organic polymer with a solvent to obtain a mixed solution;

[0014] (2) using a syringe pump, dripping the mixed solution into the alkali-lithium salt-ammonium carbonate salt-ethanol mixed solution through an electrostatic spray device to obtain microspheres;

[0015] (3) Post-processing the microspheres to obtain the magnetic lithium extraction adsorbent.

[0016] This invention encapsulates magnetic material and adsorbent into spheres using a hydrophilic organic polymer. The microspheres have a narrow particle size distribution, ensuring uniformity of material composition. They maintain excellent sphericity even after prolonged adsorption and are less susceptible to breakage and dissolution. The granulation process for the aluminum-based adsorbent is simplified through electrostatic spraying, combining the granulation step with the synthesis step, allowing the adsorbent to be synthesized during the granulation process, eliminating the need for subsequent powder granulation.

[0017] In one embodiment, the iron salt in step (1) includes any one of ferric chloride, ferric sulfate or ferric nitrate, or a combination of at least two thereof.

[0018] In one embodiment, the ferrous salt includes any one of ferrous chloride, ferrous sulfate, or ferrous nitrate, or a combination of at least two thereof.

[0019] In one embodiment, the aluminum salt includes any one of aluminum chloride, aluminum sulfate, or aluminum nitrate, or a combination of at least two thereof.

[0020] In one embodiment, the hydrophilic organic polymer includes any one or a combination of at least two of polystyrene, epoxy resin, polymethyl methacrylate, polyvinyl chloride, chitosan or chlorinated polyvinyl chloride.

[0021] In one embodiment, the solvent includes any one of N-methylpyrrolidone, acetone, or ethyl acetate, or a combination of at least two thereof.

[0022] In one embodiment, the molar ratio of ferrous ions in the ferrous salt to ferric ions in the ferric salt in step (1) is (1-1.5):(2-3), for example: 1:2, 1.2:2.5, 1.5:2.2, 1.8:2.5 or 1.5:3, etc.

[0023] In one embodiment, the molar ratio of the total molar amount of the iron element in the iron salt and the ferrous salt to the aluminum element in the aluminum salt is (0.05-0.1):1, for example: 0.05:1, 0.06:1, 0.08:1, 0.09:1 or 0.1:1, etc.

[0024] In one embodiment, the solid-to-liquid ratio of the hydrophilic organic polymer to the solvent in step (1) is 5 to 20 mg / mL, for example, 5 mg / mL, 8 mg / mL, 10 mg / mL, 15 mg / mL or 20 mg / mL.

[0025] In one embodiment, the mixing stirring temperature in step (1) is 60-80°C, for example, 60°C, 65°C, 70°C, 75°C or 80°C.

[0026] In one embodiment, the mixing stirring time is 5 to 10 hours, for example, 5 hours, 6 hours, 8 hours, 9 hours or 10 hours.

[0027] In one embodiment, the flow rate of the mixed solution in the injection pump in step (2) is 1 to 8 mL / h, for example, 1 mL / h, 2 mL / h, 4 mL / h, 6 mL / h or 8 mL / h.

[0028] In one embodiment, the voltage of the electrostatic spray device is 16 to 22 kV, for example, 16 kV, 18 kV, 20 kV, 21 kV or 22 kV.

[0029] In one embodiment, the concentration of ammonium carbonate in the alkali-lithium salt-ammonium carbonate-ethanol mixed solution in step (2) is 0.1 to 0.5 mol / L, for example, 0.1 mol / L, 0.2 mol / L, 0.3 mol / L, 0.4 mol / L or 0.5 mol / L.

[0030] In one embodiment, the concentration of the alkali in the alkali-lithium salt-ammonium carbonate-ethanol mixed solution is 1 to 3 mol / L, for example, 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L or 3 mol / L.

[0031] In one embodiment, the concentration of the lithium salt in the alkali-lithium salt-ammonium carbonate-ethanol mixed solution is 0.1-1 mol / L, for example, 0.1 mol / L, 0.2 mol / L, 0.5 mol / L, 0.8 mol / L or 1 mol / L.

[0032] In one embodiment, the alkali-lithium salt-ammonium carbonate salt-ethanol mixed solution in step (2) includes water.

[0033] In one embodiment, the volume ratio of ethanol to water is (2-5):1, for example: 2:1, 2.5:1, 3:1, 4:1 or 5:1, etc.

[0034] In one embodiment, the post-treatment in step (3) includes washing and drying.

[0035] In one embodiment, the washing detergent comprises ultrapure water.

[0036] In one embodiment, the washing is performed until the pH of the microspheres is neutral.

[0037] In one embodiment, the median particle size D50 of the magnetic lithium extraction adsorbent is 100-1000 μm, for example, 100 μm, 200 μm, 500 μm, 800 μm or 1000 μm.

[0038] In a second aspect, the present disclosure provides a magnetic adsorbent for lithium extraction, which is prepared by the method described in the first aspect.

[0039] The adsorbent prepared by the method disclosed in the present invention is magnetic and can achieve solid-liquid separation by a magnet, eliminating the need for filtering the brine and other operations, making the lithium extraction process simpler.

[0040] In a third aspect, the present disclosure provides an application of the magnetic lithium extraction adsorbent as described in the second aspect, wherein the magnetic lithium extraction adsorbent is used for extracting lithium from salt lakes.

[0041] Compared with the prior art, the present disclosure has the following beneficial effects:

[0042] (1) Compared to traditional granulation methods, the adsorbent particles prepared by the method disclosed herein have a smaller particle size and a larger specific surface area, which is more conducive to contact between the adsorbent and brine. The hydrophilic organic polymer also facilitates brine wetting of the adsorbent. In addition, the ammonium carbonate decomposes during the drying process to produce gas, which creates certain pores in the microspheres and further increases the specific surface area of ​​the adsorbent. All of these can increase the lithium extraction capacity of the adsorbent.

[0043] (2) The adsorption capacity disclosed in the present invention can reach above 9.54 mg / g, and the capacity retention rate of the lithium extraction adsorbent can reach above 96.84% after 100 cycles.

[0044] Still other aspects will become apparent upon reading and understanding the accompanying drawings and detailed description. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] The accompanying drawings are used to provide a further understanding of the technical solution of this article and constitute a part of the specification. Together with the embodiments of this application, they are used to explain the technical solution of this article and do not constitute a limitation on the technical solution of this article.

[0046] FIG1 is a SEM image of the magnetic lithium extraction adsorbent prepared in Example 1 of the present disclosure.

[0047] FIG2 is a hysteresis curve diagram of the magnetic lithium extraction adsorbent prepared in Example 1 of the present disclosure. DETAILED DESCRIPTION

[0048] The technical solution of the present disclosure is further described below through specific implementation methods. Those skilled in the art should understand that the embodiments are only used to help understand the present disclosure and should not be regarded as specific limitations of the present disclosure.

[0049] Example 1

[0050] This embodiment provides a magnetic lithium extraction adsorbent, and the preparation method of the magnetic lithium extraction adsorbent is as follows:

[0051] (1) 0.02 mol ferrous sulfate, 0.0175 mol ferric sulfate (Fe 2+ :Fe 3+ =1.5:2.65) with 10 g of epoxy resin and 1 mol of aluminum sulfate were added to 1 L of acetone and stirred at 60° C. for 10 h to prepare a homogeneous solution;

[0052] (2) Using a syringe pump (5 mL / h) and an electrostatic spray device, the homogeneous solution was dripped into an alkali-lithium salt-ammonium carbonate salt-ethanol mixed solution to obtain microspheres, wherein the concentration of ammonium bicarbonate was 0.2 mol / L, the concentration of sodium hydroxide was 2 mol / L, the concentration of lithium chloride was 0.2 mol / L, the volume ratio of ethanol to water was 2.5:1, and the voltage of the electrostatic spray device was 20 kV;

[0053] (3) After filtering the microspheres, wash them with ultrapure water to a pH of about 7, and dry them at 80°C for 10 h to obtain a magnetic lithium extraction adsorbent with a D50 of 300 μm.

[0054] The SEM image of the magnetic lithium extraction adsorbent is shown in FIG1 . As can be seen from FIG1 , the magnetic lithium extraction adsorbent is spherical, and the particle size distribution of the microspheres is narrow, which can ensure the uniformity of the material composition.

[0055] The hysteresis curve of the magnetic lithium extraction adsorbent is shown in Figure 2. As can be seen from Figure 2, the specific saturation magnetization intensity of the magnetic lithium extraction adsorbent is 10.89emμ / g. The magnetic lithium extraction adsorbent has good magnetic properties, and the hysteresis loop changes in a trend that first rises rapidly with the increase of magnetic field intensity and then tends to be flat, which is consistent with the characteristics of strong magnetic materials. The specific saturation magnetization intensity of the magnetic lithium extraction adsorbent is slightly lower than that of the magnetic titanium adsorbent, which may be because the magnetic lithium extraction adsorbent is an amorphous crystal and the magnetization phenomenon of this component is not obvious.

[0056] Example 2

[0057] This embodiment provides a magnetic lithium extraction adsorbent, and the preparation method of the magnetic lithium extraction adsorbent is as follows:

[0058] (1) 0.015 mol of ferrous sulfate and 0.019 mol of ferric sulfate (Fe 2+ :Fe 3+ =1:2.5) with 5 g of polystyrene and 1 mol of aluminum sulfate, added to 1 L of acetone and stirred at 60°C for 10 h to prepare a homogeneous solution;

[0059] (2) Using a syringe pump (1 mL / h) and an electrostatic spray device, the homogeneous solution was dripped into an alkali-lithium salt-ammonium carbonate-ethanol mixed solution to obtain microspheres, wherein the concentration of ammonium bicarbonate was 0.1 mol / L, the concentration of sodium hydroxide was 1 mol / L, the concentration of lithium chloride was 0.1 mol / L, the volume ratio of ethanol to water was 2:1, and the voltage of the electrostatic spray device was 16 kV;

[0060] (3) After filtering the microspheres, wash them with ultrapure water to a pH of about 7, and dry them at 80°C for 10 h to obtain a magnetic lithium extraction adsorbent with a D50 of 100 μm.

[0061] Example 3

[0062] This embodiment provides a magnetic lithium extraction adsorbent, and the preparation method of the magnetic lithium extraction adsorbent is as follows:

[0063] (1) 0.02 mol of ferrous sulfate and 0.03 mol of ferric sulfate (Fe 2+ :Fe 3+ =1:3) with 20 g of polymethyl methacrylate and 1 mol of aluminum sulfate, added to 1 L of ethyl acetate and stirred at 70°C for 8 h to prepare a homogeneous solution;

[0064] (2) Using a syringe pump (8 mL / h) and an electrostatic spray device, the homogeneous solution was dripped into an alkali-lithium salt-ammonium carbonate-ethanol mixed solution to obtain microspheres, wherein the concentration of ammonium bicarbonate was 0.5 mol / L, the concentration of sodium hydroxide was 3 mol / L, the concentration of lithium chloride was 1 mol / L, the volume ratio of ethanol to water was 5:1, and the voltage of the electrostatic spray device was 22 kV;

[0065] (3) After filtering the microspheres, wash them with ultrapure water to a pH of about 7, and dry them at 80°C for 10 h to obtain a magnetic lithium extraction adsorbent with a D50 of 1000 μm.

[0066] Example 4

[0067] The only difference between this embodiment and embodiment 1 is that Fe 2+ :Fe 3+ =1:1, and other conditions and parameters are exactly the same as those in Example 1.

[0068] Example 5

[0069] The only difference between this embodiment and embodiment 1 is that Fe 2+ :Fe 3+ =1:4, and other conditions and parameters are exactly the same as those in Example 1.

[0070] Example 6

[0071] The only difference between this embodiment and embodiment 1 is that the mass of the epoxy resin is 3 g, and the other conditions and parameters are exactly the same as those in embodiment 1.

[0072] Example 7

[0073] The only difference between this embodiment and embodiment 1 is that the mass of the epoxy resin is 30 g, and the other conditions and parameters are exactly the same as those in embodiment 1.

[0074] Example 8

[0075] The only difference between this embodiment and embodiment 1 is that the volume ratio of ethanol to water is 1:2, and other conditions and parameters are exactly the same as those in embodiment 1.

[0076] Example 9

[0077] The only difference between this embodiment and embodiment 1 is that the electrostatic spray voltage is 10 kV, and other conditions and parameters are exactly the same as those in embodiment 1.

[0078] Example 10

[0079] The only difference between this embodiment and embodiment 1 is that the flow rate of the syringe pump is 20 mL / h, and the other conditions and parameters are exactly the same as those in embodiment 1.

[0080] Comparative Example 1

[0081] This comparative example provides a magnetic lithium extraction adsorbent, and the preparation method of the magnetic lithium extraction adsorbent is as follows:

[0082] Ferroferric oxide with a D50 of 150 nm was used as the inner core and dispersed in a 1 mol / L aluminum chloride solution with a solid-liquid ratio of 1 mg / mL. A 2 mol / L sodium hydroxide solution was then added, with the molar amount of sodium hydroxide being three times that of aluminum chloride. Subsequently, lithium chloride, which was half the molar amount of aluminum chloride, was added. After the dispersion reaction, the mixture was stirred for 1 hour to obtain an aluminum adsorbent with an inner magnetic core.

[0083] Comparative Example 2

[0084] The only difference between this comparative example and Example 1 is that no hydrophilic organic polymer is added, and other conditions and parameters are exactly the same as those in Example 1.

[0085] Performance testing:

[0086] The adsorption performance test method is the static adsorption method. This adsorbent is used for Li + To extract lithium from brine with a concentration of 500 ppm, take 20 g of deionized water and mix it with 2 g of lithium adsorbent. Extract lithium at room temperature for 10 hours. Measure the brine concentration before and after adsorption, and calculate the adsorption capacity according to the following formula.

[0087] The adsorption capacity of the adsorbent is: Q = V (C0-C) / m;

[0088] Q is the adsorption capacity, mg / g; V is the volume of the adsorption liquid, L; m is the mass of the adsorbent, g; C0 and C are the lithium ion concentrations in the brine before and after adsorption, respectively, mg / L.

[0089] The ratio of the adsorption capacity after 100 cycles to the initial adsorption capacity was used to obtain the capacity retention rate after 100 cycles.

[0090] The test results are shown in Table 1:

[0091] Table 1

[0092] As can be seen from Table 1, from Examples 1-3, the adsorption capacity of the present disclosure can reach above 9.54 mg / g, and the capacity retention rate of the lithium extraction adsorbent can reach above 96.84% after 100 cycles.

[0093] By comparing Example 1 with Examples 4-5, it can be seen that in the preparation process of the magnetic lithium extraction adsorbent described in the present disclosure, the molar ratio of ferrous salt to ferric salt affects its performance. The molar ratio of ferrous salt to ferric salt is controlled within (1-1.5): (2-3), and the performance of the obtained adsorbent is better. If the ratio of ferrous salt to trivalent iron salt is not within this range, it is difficult to form ferrosoferric oxide in the alcohol solution, which reduces the magnetic properties of the lithium extraction adsorbent and increases the difficulty of solid-liquid separation of the adsorbent after lithium extraction.

[0094] By comparing Example 1 with Examples 6-7, it can be seen that during the preparation process of the magnetic lithium extraction adsorbent described in the present disclosure, the solid-liquid ratio of the hydrophilic organic polymer to the solvent will affect its performance. When the solid-liquid ratio of the hydrophilic organic polymer to the solvent is controlled at 5-20 mg / mL, the performance of the adsorbent obtained is better. If the amount of hydrophilic organic polymer added is too large, the adsorption capacity of the adsorbent will be reduced. If the amount of hydrophilic organic polymer added is too small, the brine cannot fully infiltrate the adsorbent, which is not conducive to the realization of its adsorption capacity.

[0095] By comparing Example 1 and Example 8, it can be seen that in the preparation process of the magnetic lithium extraction adsorbent described in the present disclosure, when the ethanol content in the alkali-lithium salt-ammonium carbonate salt-ethanol mixed solution in step (2) is low, the divalent iron ions and the trivalent iron ions in the mixed solution are difficult to undergo the above-mentioned reaction, which affects the magnetic properties of the adsorbent.

[0096] A comparison of Examples 1 and 9 shows that during the preparation of the magnetic lithium extraction adsorbent described in this disclosure, a low electrostatic spray voltage results in a larger spherical particle size, which reduces the material's specific surface area and affects adsorption capacity. Increasing the voltage does not further affect the spherical particle size, so there is no need to increase the voltage and increase energy consumption.

[0097] By comparing Example 1 and Example 10, it can be seen that during the preparation of the magnetic lithium extraction adsorbent disclosed in the present invention, the flow rate of the injection pump is too high, which destroys the balance of fluid surface tension, gravity, and electric field force, resulting in an irregular spherical structure and easy dissolution during adsorption.

[0098] By comparing Example 1 and Comparative Example 1, it can be seen that the adsorbent particle size directly using ferrosoferric oxide as the magnetic core is relatively small. During the magnetic adsorption process, some particles may be dispersed in the solution and cannot be attracted by the magnet. Compared with this, the particle size of the present invention is more appropriate, which can not only ensure the specific surface area of ​​the adsorbent, but also ensure the efficiency of the adsorbent during solid-liquid separation.

Claims

1. A preparation method of a magnetic lithium extraction adsorbent, comprising the following steps: (1) Mix an iron salt, a ferrous salt, an aluminum salt, and a hydrophilic organic polymer with a solvent to obtain a mixed solution; (2) Using a syringe pump, drop the mixed solution into an alkali-lithium salt-ammonium carbonate-ethanol mixed solution through an electrostatic spraying device to obtain microspheres; (3) Post-treat the microspheres to obtain the magnetic lithium extraction adsorbent.

2. The preparation method according to claim 1, wherein the iron salt in step (1) includes any one or a combination of at least two of ferric chloride, ferric sulfate, or ferric nitrate.

3. The preparation method according to claim 1 or 2, wherein the ferrous salt includes any one or a combination of at least two of ferrous chloride, ferrous sulfate, or ferrous nitrate.

4. The preparation method according to any one of claims 1-3, wherein the aluminum salt includes any one or a combination of at least two of aluminum chloride, aluminum sulfate, or aluminum nitrate.

5. The preparation method according to any one of claims 1-4, wherein the hydrophilic organic polymer includes any one or a combination of at least two of polystyrene, epoxy resin, polymethyl methacrylate, polyvinyl chloride, chitosan, or chlorinated polyvinyl chloride.

6. The preparation method according to any one of claims 1-5, wherein the solvent includes any one or a combination of at least two of N-methylpyrrolidone, acetone, or ethyl acetate.

7. The preparation method according to any one of claims 1-6, wherein the molar ratio of ferrous ions in the ferrous salt to ferric ions in the iron salt in step (1) is (1-1.5):(2-3).

8. The preparation method according to any one of claims 1-7, wherein the total molar amount of iron elements in the iron salt and the ferrous salt to the molar amount of aluminum element in the aluminum salt is (0.05-0.1):

1.

9. The preparation method according to any one of claims 1-8, wherein the solid-liquid ratio of the hydrophilic organic polymer to the solvent is 5-20 mg / mL.

10. The preparation method according to any one of claims 1-9, wherein the stirring temperature of the mixing in step (1) is 60-80 °C; Optionally, the stirring time of the mixing is 5-10 h.

11. The preparation method according to any one of claims 1-10, wherein the flow rate of the mixed solution in the syringe pump in step (2) is 1-8 mL / h; Optionally, the voltage of the electrostatic spraying device is 16-22 kV.

12. The preparation method according to any one of claims 1-11, wherein the concentration of ammonium carbonate in the alkali-lithium salt-ammonium carbonate-ethanol mixed solution in step (2) is 0.1-0.5 mol / L; Optionally, the concentration of the alkali in the alkali-lithium salt-ammonium carbonate-ethanol mixed solution is 1-3 mol / L; Optionally, the concentration of the lithium salt in the alkali-lithium salt-ammonium carbonate-ethanol mixed solution is 0.1-1 mol / L.

13. The preparation method according to any one of claims 1-12, wherein the alkali-lithium salt-ammonium carbonate-ethanol mixed solution in step (2) includes water; Optionally, the volume ratio of ethanol to water is (2-5):

1.

14. The preparation method according to any one of claims 1-13, wherein, the post-treatment in step (3) includes washing and drying; optionally, the detergent for washing includes ultrapure water; optionally, the washing is carried out until the pH of the microspheres is neutral; optionally, the median particle size D50 of the magnetic lithium extraction adsorbent is 100-1000 μm.

15. A magnetic lithium extraction adsorbent prepared by the method according to any one of claims 1-14.

16. Use of a magnetic lithium extraction adsorbent according to claim 15 for extracting lithium from salt lakes.

Citation Information

Patent Citations

  • Preparation process of lithium adsorbent

    CN106507704B

  • Preparation method of magnetic aluminum salt lithium adsorbent

    CN110639467A

  • Preparation method of magnetic iron-doped aluminum lithium adsorbent

    CN116272837A

  • Lithium adsorbent and method for extracting lithium from salt lake

    CN116351384A

  • Aluminum-based lithium ion-sieve (LIS), and preparation method and use thereof

    US20230330622A1