Method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide

Patent metadata

Field	Value
Publication number	US-11414324-B2
Application number	US-201916648660-A
Country	US
Kind code	B2
Filing date	Apr 19, 2019
Priority date	Dec 26, 2018
Publication date	Aug 16, 2022
Grant date	Aug 16, 2022

Abstract

Described is a method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide. This method includes a. adding an aluminum salt to the brine, adding an alkali solution, then subjecting to crystallization reaction and solid-liquid separation to obtain lithium-containing brine; b. evaporating and concentrating the lithium-containing brine, adding an aluminum salt, adding an alkali solution dropwise to perform a co-precipitation reaction and solid-liquid separation to obtain a lithium-containing layered material filter cake, wherein in steps a and b, the alkali solution is an alkali solution free of carbonate ion; c. dispersing the lithium-containing layered material filter cake in deionized water to form a suspension slurry, then adjusting the pH value of the suspension slurry so as to carry out a lithium deintercalation reaction; d. filtering to obtain aluminum hydroxide filter cake; e. washing the aluminum hydroxide filter cake with deionized water and drying.

First claim

The invention claimed is:

1. A method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide, the method comprising:
a. adding an aluminum salt to a salt lake brine to obtain a mixed salt solution A, adding an alkali solution to the mixed salt solution A for co-precipitation reaction, then subjecting to crystallization reaction and solid-liquid separation at the end of the crystallization reaction to obtain magnesium-aluminum hydrotalcite solid product and lithium-containing brine, wherein in step a, the alkali solution is an alkali solution free of carbonate ion;
b. evaporating and concentrating the lithium-containing brine to obtain a lithium-rich brine, adding an aluminum salt to the lithium-rich brine to obtain a mixed salt solution B, adding an alkali solution dropwise to the mixed salt solution B to perform a co-precipitation reaction and solid-liquid separation after the end of the reaction to obtain a lithium-containing liquid and a lithium-containing layered material filter cake, wherein in step b, the alkali solution is an alkali solution free of carbonate ion and wherein in step b, the lithium-containing layered material has a chemical formula LiAlx(OH)3xCl mH2O, where x=1-10, and m=1-10;
c. dispersing the lithium-containing layered material filter cake in deionized water to form a suspension slurry, then adjusting the pH value of the suspension slurry so as to carry out a lithium deintercalation reaction;
d. filtering the slurry obtained after the lithium deintercalation reaction to obtain a lithium-containing solution and aluminum hydroxide filter cake; and
e. washing the aluminum hydroxide filter cake with deionized water and drying to obtain aluminum hydroxide solid.

2. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein the brine in step a is sulfate type or chloride type salt lake brine, which is rich in Li+, Mg2+, K+, and Na+, and in which the concentration of Li+ is 1-3 g/L, the concentration of Mg2+ is 10-30 g/L, the concentration of K+ is 5-7 g/L, and the concentration of Na+ is 70-90 g/L, with respect to the total volume of the brine.

3. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the lithium ion concentration in the lithium-rich brine is 0.1-0.5 g/L with respect to the total volume of the lithium-rich brine.

4. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the molar concentration of lithium ion is 1-6 times that of aluminum ion in the mixed salt solution B.

5. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the aluminum salt is aluminum nitrate and/or aluminum chloride.

6. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the alkali solution has a molar concentration of 2-4 mol/L with respect to its total volume; and the alkali solution is added dropwise at a rate of 1-2 mL/min.

7. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the alkali solution is aqueous sodium hydroxide solution and/or aqueous potassium hydroxide solution.

8. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the co-precipitation reaction is carried out at a temperature of 40° C.-100° C. for a period of 6-24 hours, with the pH controlled at 7-8 during the reaction.

9. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the lithium-containing layered material filter cake has a solid content of 60-95%.

10. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step b, the concentration of Li+ is 0.01-0.05 g/L, the concentration of K+ is 0.5-1 g/L, the concentration of Na+ is 40-60 g/L, the concentration of Cl− is 50-70 g/L, and the concentration of SO 4 2− is 1-5 g/L in the lithium-containing liquid, with respect to the total volume of the lithium-containing liquid.

11. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , further comprising an operation of evaporating and concentrating the lithium-containing liquid from step b to a lithium ion concentration of 0.1-0.5 g/L and then recycling it as the lithium-containing brine.

12. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step c, the suspension slurry has a solid content of 5-50 g/L with respect to the total volume of the suspension slurry.

13. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step c, the adjusting the pH value of the suspension slurry is to adjust the pH value of the suspension slurry to 5-8.

14. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step c, the pH value of the suspension slurry is adjusted to 5-8 by using hydrochloric acid or aqueous sodium hydroxide solution with a molar concentration of 2-4 mol/L.

15. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step c, the lithium deintercalation reaction is carried out at a temperature of 60° C.-100° C. for a period of 30 to 180 minutes.

16. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step c, the lithium deintercalation reaction is carried out at a stirring rate of 30-200 rpm.

17. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , further comprising an operation of evaporating and concentrating the lithium-containing solution from step d to a lithium ion concentration of 20-25 g/L and then using it as a lithium solution for preparing battery grade lithium carbonate.

18. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step e, the washing with deionized water is repeated 3 to 5 times.

19. The method for extracting lithium from salt lake brine and simultaneously preparing aluminum hydroxide according to claim 1 , wherein in step e, the drying is carried out at 60° C.-80° C. for 3-12 hours.

Assignees

• Univ Beijing Chem Tech

Inventors

• Xiang Xu
• Duan Xue

Classifications

• C01D15/08 Primary

  Carbonates; Bicarbonates · CPC title

• B01D9/0054 Primary

  Use of anti-solvent · CPC title

• C01F7/784

  Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions · CPC title

• C01P2006/82

  water content · CPC title

• B01D9/0018

  Evaporation of components of the mixture to be separated · CPC title