Lithium-ion adsorption material, and preparation method and use thereof

Patent metadata

Field	Value
Publication number	US-2025352986-A1
Application number	US-202519008037-A
Country	US
Kind code	A1
Filing date	Jan 2, 2025
Priority date	May 15, 2024
Publication date	Nov 20, 2025
Grant date	—

Abstract

Disclosed are a lithium-ion adsorption material, a preparation method and use thereof. The preparation method includes: mixing sodium alginate, calcium carbonate, gluconolactone and water to obtain a sodium alginate hydrogel; The soaking the sodium alginate hydrogel into an oxidizing solution, and subjecting a resulting solution to oxidative ring-opening reaction to obtain an oxidized sodium alginate hydrogel; mixing the oxidized sodium alginate hydrogel, a dispersant, a solvent and a lithium-based compound, and subjecting an obtained mixture to aldol condensation reaction to obtain a lithium-based sodium alginate hydrogel; and subjecting the lithium-based sodium alginate hydrogel to acid-washing and freeze-drying in sequence to obtain the lithium ion adsorption material.

First claim

What is claimed is:

1 . A method for preparing a lithium-ion adsorption material, comprising:
1) mixing sodium alginate, calcium carbonate, gluconolactone and water to obtain a sodium alginate hydrogel; 2) soaking the sodium alginate hydrogel into an oxidizing solution, and subjecting a resulting solution to oxidative ring-opening reaction to obtain an oxidized sodium alginate hydrogel; 3) mixing the oxidized sodium alginate hydrogel, a dispersant, a solvent and a lithium-based compound, and subjecting an obtained mixture to aldol condensation reaction to obtain a lithium-based sodium alginate hydrogel; and 4) subjecting the lithium-based sodium alginate hydrogel to acid-washing and freeze-drying in sequence to obtain the lithium-ion adsorption material.

2 . The method of claim 1 , wherein in step 1), a mass to volume ratio of the sodium alginate, the calcium carbonate, and the gluconolactone to water is in a range of 0.5-1.25 g:0.045-0.12 g:0.16-0.41 g:25 mL.

3 . The method of claim 1 , wherein in step 2),
the oxidizing solution is selected from the group consisting of a potassium permanganate solution and a sodium periodate solution, a mass to volume ratio of the potassium permanganate to water in the potassium permanganate solution is in a range of 0.6-1.2 g:80 mL, and a mass to volume ratio of sodium periodate to water in the sodium periodate solution is in a range of 0.6-1.2 g:80 mL; and a mass to volume ratio of the sodium alginate hydrogel to the oxidizing solution is in a range of 25-30 g:80 mL.

4 . The method of claim 2 , wherein in step 2),
the oxidizing solution is selected from the group consisting of a potassium permanganate solution and a sodium periodate solution, a mass to volume ratio of the potassium permanganate to water in the potassium permanganate solution is in a range of 0.6-1.2 g:80 mL, and a mass to volume ratio of sodium periodate to water in the sodium periodate solution is in a range of 0.6-1.2 g:80 mL; and a mass to volume ratio of the sodium alginate hydrogel to the oxidizing solution is in a range of 25-30 g:80 mL.

5 . The method of claim 3 , wherein in step 2), the oxidative ring-opening reaction is conducted under a dark condition at a temperature of 40° C. to 60° C. for 8 h to 12 h.

6 . The method of claim 5 , wherein in step 3),
the dispersant is selected from the group consisting of dimethyl sulfoxide, anhydrous ethanol, methanol and acetonitrile; the solvent is selected from the group consisting of diethylene glycol, triethylene glycol and dihydroxydibutyl ether; the lithium-based compound is selected from the group consisting of n-butyl lithium, lithium carbonate, propyl lithium and benzyl lithium; a mass to volume ratio of the oxidized sodium alginate hydrogel to the dispersant is in a range of 20-30 g:50-100 mL; under the condition that the lithium-based compound is selected from the group consisting of the n-butyl lithium, the propyl lithium and the benzyl lithium, a volume ratio of the solvent to the lithium-based compound is in a range of 0.5-1.5:0.3-1.5, and a mass to volume ratio of the oxidized sodium alginate hydrogel to the lithium-based compound is in a range of 20-30 g:0.3-1.5 mL; and under the condition that the lithium-based compound is the lithium carbonate, a volume to mass ratio of the solvent to the lithium-based compound is in a range of 0.5-1.5 mL: 0.2-1 g, and a mass ratio of the oxidized sodium alginate hydrogel to the lithium-based compound is in a range of 20-30:0.2-1.

7 . The method of claim 6 , wherein in step 3), the aldol condensation reaction is conducted at a pH value of 10 to 12 for 6 h to 18 h.

8 . The method of claim 6 , wherein in step 4), the acid-washing is conducted using an acid solution at a concentration of 0.05 mol/L to 0.2 mol/L, the acid solution is selected from the group consisting of hydrochloric acid and nitric acid; the acid-washing is conducted for 1 h to 2 h; and a mass to volume ratio of the lithium-based sodium alginate hydrogel to the acid solution is in a range of 22-32 g:50-80 mL.

9 . The method of claim 7 , wherein in step 4), the acid-washing is conducted using an acid solution at a concentration of 0.05 mol/L to 0.2 mol/L, the acid solution is selected from the group consisting of hydrochloric acid and nitric acid; the acid-washing is conducted for 1 h to 2 h; and a mass to volume ratio of the lithium-based sodium alginate hydrogel to the acid solution is in a range of 22-32 g:50-80 mL.

10 . The method of claim 8 , wherein in step 4), the freeze-drying is conducted at a temperature of −70° C. to −50° C. for 40 h to 60 h.

11 . A lithium-ion adsorption material prepared by the method of claim 1 .

12 . The lithium-ion adsorption material of claim 11 , wherein in step 1), a mass to volume ratio of the sodium alginate, the calcium carbonate, and the gluconolactone to water is in a range of 0.5-1.25 g:0.045-0.12 g:0.16-0.41 g:25 mL.

13 . The lithium-ion adsorption material of claim 11 , wherein in step 2),
the oxidizing solution is selected from the group consisting of a potassium permanganate solution and a sodium periodate solution, a mass to volume ratio of the potassium permanganate to water in the potassium permanganate solution is in a range of 0.6-1.2 g:80 mL, and a mass to volume ratio of sodium periodate to water in the sodium periodate solution is in a range of 0.6-1.2 g:80 mL; and a mass to volume ratio of the sodium alginate hydrogel to the oxidizing solution is in a range of 25-30 g:80 mL.

14 . The lithium-ion adsorption material of claim 11 , wherein in step 2), the oxidative ring-opening reaction is conducted under dark condition at a temperature of 40° C. to 60° C. for 8 h to 12 h.

15 . The lithium-ion adsorption material of claim 11 , wherein in step 3),
the dispersant is selected from the group consisting of dimethyl sulfoxide, anhydrous ethanol, methanol and acetonitrile; the solvent is selected from the group consisting of diethylene glycol, triethylene glycol and dihydroxydibutyl ether; the lithium-based compound is selected from the group consisting of n-butyl lithium, lithium carbonate, propyl lithium and benzyl lithium; a mass to volume ratio of the oxidized sodium alginate hydrogel to the dispersant is in a range of 20-30 g:50-100 mL; under the condition that the lithium-based compound is selected from the group consisting of the n-butyl lithium, the propyl lithium and the benzyl lithium, a volume ratio of the solvent to the lithium-based compound is in a range of 0.5-1.5:0.3-1.5, and a mass to volume ratio of the oxidized sodium alginate hydrogel to the lithium-based compound is in a range of 20-30 g:0.3-1.5 mL; and under the condition that the lithium-based compound is the lithium carbonate, a volume to mass ratio of the solvent to the lithium-based compound is in a range of 0.5-1.5 mL: 0.2-1 g, and a mass ratio of the oxidized sodium alginate hydrogel to the lithium-based compound is in a range of 20-30:0.2-1.

16 . The lithium-ion adsorption material of claim 11 , wherein in step 3), the aldol condensation reaction is conducted at a pH value of 10 to 12 for 6 h to 18 h.

17 . The lithium-ion adsorption material of claim 11 , wherein in step 4), the acid-washing is conducted using an acid solution at a concentration of 0.05 mol/L to 0.2 mol/L, the acid solution is selected from the group consisting of hydrochloric acid and nitric acid; the acid-washing is conducted for 1 h to 2 h; and a mass to volume ratio of the lithium-based sodium alginate hydrogel to the acid solution is in a range of 22-32 g:50-80 mL.

Assignees

• Univ Hainan

Inventors

• Lu Lingbin
• Xu Yutao

Classifications

• B01J20/3078

  Thermal treatment, e.g. calcining or pyrolizing · CPC title

• B01J20/24

  Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives · CPC title

• B01J20/3085

  Chemical treatments not covered by groups B01J20/3007 - B01J20/3078 · CPC title

• B01J20/3071 Primary

  Washing or leaching · CPC title

• B01J20/226 Primary

  Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF] (preparation of metal complexes containing carboxylic acid moieties C07C51/418; MOF's per se C07F) · CPC title