IP Library Granted Patent US 10,280,483
Granted Patent B2
US 10,280,483 · App. 14/826,334 · Granted May 7, 2019

Solvent extraction of transition metals

Inventors: Peter Tkac (Naperville, IL); George F. Vandegrift, III (Crest Hill, IL); David A. Rotsch (Montgomery, IL)
Assignee: UCHICAGO ARGONNE, LLC
C22B34/34C22B3/0005C22B7/007Y02P10/234
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Quick Facts
Patent No.
US 10,280,483
App. No.
14/826,334
Granted
May 7, 2019
Kind
B2
Abstract

The invention provides a continuous method for extracting transition metal, the method comprising: supplying a spent generator liquor comprising transition metal in highly alkaline solution; mixing the liquor with acid thereby generating a solution, wherein the transition metal resides within the solution; combining the solution with an organic liquid comprising tributyl phosphate or other neutral extractant to extract the transition metal within the organic liquid; washing the extracted transition metal in the organic liquid with acid so as to remove non-transition-metal salts from the organic liquid phase; and stripping the washed transition metal loadedorganic liquid phase with hydroxide, water or complexing agent to remove the transition metal from the organic phase.

Claims (22)

1. A continuous method for extracting transition metals, the method comprising:

a. supplying a spent generator liquor comprising transition metal in alkaline liquid;

b. mixing the spent generator liquor with acid to form an acidic solution of the transition metal;

c. contacting the acidic solution with an organic liquid comprising a neutral extractant to extract the transition metal into the organic liquid;

d. washing the extracted transition metal in the organic liquid with hydrochloric acid so as to remove potassium from the organic liquid; and

e. removing more than 97 percent of the transition metal from the organic liquid from the organic liquid washed in step d.

2. The method as recited in claim 1 wherein the step of mixing the spent generator liquor with acid results in anions of the acid combining with cations of the alkaline liquid to form a salt and precipitate out of the solution.

3. The method as recited in claim 1 wherein the organic liquid is an extractant selected from the group consisting of tributyl phosphate, trioctylphosphine oxide, octyl(phenyl)-N, N-di-isobutylcarbamoylmethylphosphine oxide, and combinations thereof.

4. The method as recited in claim 1 wherein step c further results in potassium salt being confined to an aqueous phase.

5. The method as recited in claim 1 wherein an acid concentration in the washing step is less than or equal to the concentration used in the mixing step.

6. The method as recited in claim 1 wherein the removing step yields organic solution which is recycled to the mixing step.

7. The method as recited in claim 1 wherein the transition metal is an element selected from the group consisting of Mo, Tc, Ti, Ga, Sb, Zn, Sn, Nb, and combinations thereof.

8. The method as recited in claim 1 further comprising subjecting the removed transition metal to sublimation or differential solubility to form a solid phase containing the transition metal.

9. The method as recited in claim 8 wherein the solid phase is a salt of the transition metal.

10. The method as recited in claim 9 wherein the salt is heated to create solid phase oxides of transition metals.

11. The method as recited in claim 1 wherein the step of removing the transition metal from the organic liquid comprises contacting the organic liquid with hydroxide, or water, or a complexant.

12. The method as recited in claim 11 wherein the hydroxide is potassium hydroxide, or sodium hydroxide or ammonium hydroxide, or combinations thereof.

13. The method as recited in claim 12 wherein the lowest molarity of the hydroxide is approximately 0.1M.

14. The method as recited in claim 1 wherein the step of removing the transition metal from the organic liquid comprises contacting the organic liquid with a complexant selected from the group consisting of acetohydroxamic acid, trialkylammonium salts of ethylenediaminetetraacetic acid, triethylenetetraminehexaacetic acid, oxalic acid, and combinations thereof.

15. The method as recited in claim 1 wherein the metal is Mo and the concentration of extracted Mo is up to 0.5M.

16. The method as recited in claim 1 wherein the neutral extractant is a phosphorous based extractant having the general formula PO x R 3 , where x is 1-4, and R is an aqueous insoluble oxygen containing organic compounds that contain ether, ketone, ester, amides, or combinations thereof.

17. The method as recited in claim 1 wherein the hydrochloric acid has a concentration of between 1M to 10M.

Assignments (2)
CONFIRMATORY LICENSE Recorded Oct 26, 2015
From: UCHICAGO ARGONNE, LLC
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 036985/0596 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 7, 2015
From: TKAC, PETER; VANDEGRIFT III, GEORGE F.; ROTSCH, DAVID A.
To: UCHICAGO ARGONNE, LLC
Reel/Frame 036746/0155 →
Continuity (2)
Provisional Application 62160024 · May 12, 2015
Related Publication 20160333442A1 · Nov 17, 2016