IP Library Granted Patent US 11,959,154
Granted Patent B2
US 11,959,154 · App. 17/520,869 · Granted Apr 16, 2024

Process for making modified DTPA-associated organosilica media for use in solid-liquid extraction of rare earth elements

Inventors: Timothy M. Dittrich (Grosse Pointe Woods, MI); Matthew J. Allen (Plymouth, MI); Mohammed Dardona (Garden City, MI); Jessica L. Hovey (Garden City, MI)
Assignee: Wayne State University
C22B59/00B01J20/22C22B3/24
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Quick Facts
Patent No.
US 11,959,154
App. No.
17/520,869
Granted
Apr 16, 2024
Kind
B2
Abstract

A process for making modified diethylenetriaminepentaacetic acid (DTPA)-associated media for use in solid-liquid extraction of rare earth elements is disclosed. The process includes functionalizing DTPA with hydrophobic groups to form modified DTPA; dissolving the modified DTPA into a methanol solution; loading the modified DTPA solution to a solid support; rotating the modified DTPA-loaded solid support to allow for association; and removing the methanol to obtain the modified-DTPA-associated media.

Claims (28)

1. A modified DTPA-associated media for use in solid-liquid extraction, comprising modified diethylenetriaminepentaacetic acid (DTPA) chemically associated via hydrophobic interactions with a hydrophobic solid support, wherein the modified DTPA includes DTPA functionalized with hydrophobic groups.

2. The modified DTPA-associated media of claim 1 , wherein the hydrophobic solid support is an organosilica platform.

3. The modified DTPA-associated media of claim 1 , wherein the hydrophobic groups includes one or more alkyl groups.

4. The modified DTPA-associated media of claim 1 , wherein the hydrophobic groups includes two hydrophobic ethylhexyl groups.

5. The modified DTPA-associated media of claim 1 , wherein the modified DTPA has the following formula:

wherein R is C 4 H 9 , C 6 H 13 , C 12 H 25 , C 14 H 29 , or C 16 H 33 .

6. A process for making modified diethylenetriaminepentaacetic acid (DTPA)-associated media for use in solid-liquid extraction of rare earth elements, comprising:

functionalizing DTPA with hydrophobic groups to form modified DTPA;

dissolving the modified DTPA into a methanol solution;

loading the modified DTPA solution to a solid support;

rotating the modified DTPA-loaded solid support to allow for association; and

removing the methanol to obtain the modified DTPA-associated media;

wherein the modified DTPA is chemically associated via hydrophobic interactions with the solid support.

7. The process of claim 6 , wherein the hydrophobic groups includes one or more alkyl groups.

8. The process of claim 6 , wherein the hydrophobic groups includes two hydrophobic ethylhexyl groups.

9. The process of claim 6 , wherein the modified DTPA has the following formula:

wherein R is C 4 H 9 , C 6 H 13 , C 12 H 25 , C 14 H 29 , or C 16 H 33 .

10. The process of claim 6 , wherein the solid support comprises an organosilica platform.

11. The process of claim 6 , wherein rotating the modified DTPA-loaded solid support includes centrifuging the modified DTPA-loaded solid support in the methanol solution at 15-50 rpm for approximately 1-5 hours at ambient temperature.

12. The modified DTPA-associated media of claim 1 , wherein the hydrophobic groups anchor the modified DTPA to the solid support through hydrophobic interactions.

13. The modified DTPA-associated media of claim 1 , wherein the modified DTPA remains chemically associated via said hydrophobic interactions with the solid support for at least five (5) cycles of re-use.

14. A solid-liquid extraction sorbent, comprising:

a modified DTPA-associated media including modified diethylenetriaminepentaacetic acid (DTPA) chemically associated with an organosilica solid support, wherein the modified DTPA includes DTPA functionalized with two hydrophobic groups; and

wherein the two hydrophobic groups anchor the modified DTPA to the organosilica solid support through hydrophobic interactions.

15. The solid-liquid extraction sorbent of claim 14 , wherein the two hydrophobic groups includes one or more alkyl groups.

16. The solid-liquid extraction sorbent of claim 14 , wherein the hydrophobic groups includes two hydrophobic ethylhexyl groups.

17. The solid-liquid extraction sorbent of claim 14 , wherein the modified DTPA has the following formula:

wherein R is C 4 H 9 , C 6 H 13 , C 12 H 25 , C 14 H 29 , or C 16 H 33 .

Assignments (2)
CONFIRMATORY LICENSE Recorded Feb 10, 2025
From: WAYNE STATE UNIVERSITY
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 070159/0448 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 8, 2021
From: DITTRICH, TIMOTHY M.; ALLEN, MATTHEW J.; DARDONA, MOHAMMED; HOVEY, JESSICA L.
To: WAYNE STATE UNIVERSITY
Reel/Frame 058043/0792 →
Continuity (2)
Provisional Application 63111479 · Nov 9, 2020
Related Publication 20220145422A1 · May 12, 2022