Separation of rare earth elements

Patent metadata

Field	Value
Publication number	US-12247268-B2
Application number	US-202418930515-A
Country	US
Kind code	B2
Filing date	Oct 29, 2024
Priority date	Nov 20, 2019
Publication date	Mar 11, 2025
Grant date	Mar 11, 2025

Abstract

A sublimation/distillation apparatus including a crucible with an open end, a heating device thermally coupled to the crucible, an actively cooled collection substrate disposed above the open end of the crucible, and a vacuum chamber housing the crucible, the heating device, and the actively cooled collection substrate.

First claim

What is claimed is:

1. A method for purifying lutetium, the method comprising:
reducing ytterbium oxide to ytterbium metal;
irradiating the ytterbium metal to generate lutetium, thereby forming a solid composition comprising ytterbium and lutetium;
subliming or distilling ytterbium from the solid composition in an inert or reduced pressure environment and at a temperature of about 400° C. to about 1500° C. to leave a lutetium composition comprising a higher weight percentage of lutetium than was present in the solid composition; and
collecting the ytterbium for reuse.

2. The method of claim 1 , wherein the temperature is about 400° C. to about 1200° C.

3. The method of claim 1 , wherein the temperature is about 400° C. to about 650° C.

4. The method of claim 1 , wherein the temperature is about 470° C. to about 630° C.

5. The method of claim 1 , wherein the temperature is greater than 800° C. to about 1500° C.

6. The method of claim 1 , wherein the reduced pressure is about 1×10 −8 torr to about 1×10 −1 torr.

7. The method of claim 1 , wherein the reduced pressure is about 1×10 −6 torr to about 1×10 −1 torr.

8. The method of claim 1 , wherein the reduced pressure is about 1×10 −6 torr to about 1×10 −3 torr.

9. The method of claim 1 , wherein the temperature is about 400° C. to less than 700° C.

10. The method of claim 9 , wherein the reduced pressure is 1×10 −3 torr or less.

11. The method of claim 1 , wherein the inert or reduced pressure environment comprises an inert environment.

12. The method of claim 1 , wherein the subliming or distilling is conducted at a rate of about 20 min/g to about 60 min/g of solid composition.

13. The method of claim 1 , wherein the process yields a ytterbium mass reduction of the solid composition from 1000:1 to 40,000:1.

14. The method of claim 1 , wherein the process yields a ytterbium mass reduction of the solid composition of greater than 3000:1.

15. The method of claim 1 , wherein the process yields a ytterbium mass reduction of the solid composition of greater than 10,000:1.

16. The method of claim 1 , wherein the lutetium composition comprises about 1 wt % to 90 wt % of ytterbium.

17. The method of claim 1 , wherein the ytterbium is collected in an amount that is about 90 wt % to about 99.999 wt % of the ytterbium present in the solid composition.

18. The method of claim 1 , wherein the ytterbium comprises Yb-176 and the lutetium comprises Lu-177.

19. A method comprising:
heating a solid composition of ytterbium and lutetium to a first temperature in an inert or reduced pressure environment;
retaining the solid composition at the first temperature in the inert or reduced pressure environment; and
heating the solid composition to a second temperature that is greater than the first temperature in the inert or reduced pressure environment such that ytterbium sublimes, distills, or both sublimes and distills from the solid composition to leave a lutetium composition comprising a higher weight percentage of lutetium than was present in the solid composition, wherein the second temperature is about 400° C. to about 1500° C.

20. The method of claim 19 , wherein the reduced pressure is 1×10 −3 torr or less and the second temperature is about 400° C. to less than 700° C.

21. The method of claim 19 , wherein the reduced pressure is 1×10 −4 torr or less.

22. The method of claim 19 , wherein the second temperature is about 400° C. to about 650° C.

23. The method of claim 19 , further comprising prior to heating the solid composition of ytterbium and lutetium to the first temperature:
reducing ytterbium oxide to ytterbium metal; and
irradiating the ytterbium metal to generate lutetium, thereby forming the solid composition comprising ytterbium and lutetium; and
after heating the solid composition to the second temperature, collecting the ytterbium for reuse.

24. A method for purifying lutetium, the method comprising:
subliming or distilling ytterbium from a solid composition in an environment comprising a pressure of 1×10 −3 torr or less and at a temperature of about 400° C. to less than 700° C. to leave a lutetium composition comprising a higher weight percentage of lutetium than was present in the solid composition.

25. The method of claim 24 , further comprising prior to subliming or distilling the ytterbium from the solid composition:
reducing ytterbium oxide to ytterbium metal; and
irradiating the ytterbium metal to generate lutetium, thereby forming the solid composition comprising ytterbium and lutetium; and
after subliming or distilling the ytterbium from the solid composition, collecting the ytterbium for reuse.

26. The method of claim 24 , wherein the process yields a ytterbium mass reduction of the solid composition of greater than 3000:1.

27. The method of claim 24 , wherein the ytterbium is collected in an amount that is about 90 wt % to about 99.999 wt % of the ytterbium present in the solid composition.

28. A method for purifying lutetium, the method comprising:
subliming or distilling ytterbium from a solid composition in an environment comprising a pressure of about 1×10 −6 torr to about 1×10 −1 torr and at a temperature of about 470° C. to 630° C. to leave a lutetium composition comprising a higher weight percentage of lutetium than was present in the solid composition.

29. The method of claim 28 , further comprising prior to subliming or distilling the ytterbium from the solid composition:
reducing ytterbium oxide to ytterbium metal; and
irradiating the ytterbium metal to generate lutetium, thereby forming the solid composition comprising ytterbium and lutetium; and
after subliming or distilling the ytterbium from the solid composition, collecting the ytterbium for reuse.

30. The method of claim 28 , wherein the process yields a ytterbium mass reduction of the solid composition of greater than 3000:1.

Assignees

• Shine Technologies Llc

Inventors

• Piefer Gregory
• Van Abel Eric
• Sisson Richard

Classifications

• Y02P10/20

  Recycling · CPC title

• C22B9/04

  Refining by applying a vacuum · CPC title

• C22B9/02

  Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action {including acoustic waves; (C22B9/003, C22B9/006, C22B9/05, C22B9/22 take precedence)} · CPC title

• G21G2001/0094

  Other isotopes not provided for in the groups listed above · CPC title

• C22B3/205

  using adducts or inclusion complexes · CPC title