Continuous solvent extraction process for generation of high grade rare earth oxides from leachates generated from coal sources

Patent metadata

Field	Value
Publication number	US-11186895-B2
Application number	US-201916534738-A
Country	US
Kind code	B2
Filing date	Aug 7, 2019
Priority date	Aug 7, 2018
Publication date	Nov 30, 2021
Grant date	Nov 30, 2021

Abstract

A continuous solvent extract process is provided for concentrating rare earth elements from leachates generated from coal sources. The process involves solvent extraction which utilizes an organic extractant mixed into an organic solvent.

First claim

What is claimed:

1. A method of recovering rare earth elements from an aqueous coal source leachate, comprising:
contacting, in a roughing circuit, rare earth elements in the aqueous coal source leachate with the organic phase to extract the rare earth elements into an organic phase and leave contaminants in an aqueous phase;
scrubbing, in the roughing circuit, additional contaminants from the organic phase;
stripping, in the roughing circuit, the rare earth elements from the organic phase; and
recovering the rare earth elements in a rare earth element containing solution.

2. The method of claim 1 , including using an organic extractant in the organic phase to provide preferential extraction of the rare earth elements from the aqueous coal source leachate.

3. The method of claim 2 , including completing the contacting at an operating pH of between 0.5 and 3.5.

4. The method of claim 1 , including using a first acid to selectively scrub the additional contaminants from the organic phase at a first pH.

5. The method of claim 4 , including using a second acid to strip the rare earth elements from the organic phase at a second pH wherein said second pH<said first pH.

6. The method of claim 1 , including cleaning the rare earth elements in the rare earth element containing solution to upgrade purity of the rare earth elements.

7. The method of claim 6 , wherein said cleaning includes subjecting the rare earth elements in the rare earth element containing solution to additional contacting, scrubbing and stripping steps with an organic phase in a cleaning circuit separate from the roughing circuit.

8. The method of claim 7 , including maximizing contaminant rejection and recycling unextracted rare earth elements back to a leaching circuit upstream of the roughing circuit or a feed of the roughing circuit.

9. The method of claim 8 , including subjecting a stripped solution from the cleaning circuit to oxalate precipitation after pH adjustment to a predetermined pH.

10. The method of claim 6 , wherein said cleaning includes incrementally raising the pH of an aqueous solution in which the rare earth elements are held whereby different groups of contaminants are precipitated in different pH ranges.

11. The method of claim 10 , wherein said cleaning is performed in a selective precipitation circuit separate from the roughing circuit.

12. The method of claim 11 , including re-dissolving rare earth element hydroxides and precipitating as oxalates by adding calculated amounts of oxalic acid at a predetermined pH.

13. The method of claim 6 , including subjecting recovered rare earth elements to oxalic precipitation by first bringing the pH of the rare earth element containing solution to a predetermined pH and then adding a calculated amount of oxalic acid to precipitate the rare earth elements preferentially.

14. The method of claim 1 , including, following stripping, recovering scandium from the organic phase by saponification in a saponification circuit separate from the roughing circuit.

15. The method of claim 14 , including treating the organic phase with an alkali solution causing the scandium to precipitate as scandium hydroxide and then filtering the scandium hydroxide from an aqueous solution.

16. The method of claim 15 , including recycling the organic phase from the saponification circuit back to the roughing circuit.

17. The method of claim 16 , further including treating the organic phase with a third acid to remove additional contaminants prior to treating the organic phase with an alkali solution.

18. The method of claim 17 , further including treating the aqueous solution with a fourth acid to exchange a saponification ion with H + prior to recycling back to the roughing circuit.

19. The method of claim 1 , including maintaining an aqueous to organic ratio in the roughing circuit of 1:1 to 1:100 at a pH of 0.5 to 3.5 and a concentration of organic extractant of between 0.5% and 10%.

20. The method of claim 14 , including adding a phase modifier to the organic phase to assist in saponification and improve selective recovery of said rare earth elements.

21. The method of claim 1 including pretreating an aqueous feed with a reducing agent to the roughing circuit for reduction of ferric iron to ferrous iron to decrease contamination.

22. The method of claim 21 , including using the reducing agent selected from a group consisting of sulfur gasses, pyrite, copper, ascorbic acid, metallic iron and combinations thereof.

Assignees

• Univ Kentucky Res Found

Inventors

• Werner Joshua Michael
• Chandra Alind
• Honaker Rick Q

Classifications

• C22B59/00 Primary

  Obtaining rare earth metals · CPC title

• C22B3/382

  Phosphine chalcogenides, e.g. compounds of the formula R3P=X with X = O, S, Se or Te · CPC title

• C22B3/44 Primary

  by chemical processes (treatment or purification of solutions by liquid-liquid extraction C22B3/26, by ion-exchange extraction C22B3/42) · CPC title

• C22B3/3842

  Phosphinic acid, e.g. H2P(O)(OH) · CPC title

• C22B3/383

  Tervalent phosphorus oxyacids, esters thereof · CPC title