Solvent extraction of transition metals

Patent metadata

Field	Value
Publication number	US-10280483-B2
Application number	US-201514826334-A
Country	US
Kind code	B2
Filing date	Aug 14, 2015
Priority date	May 12, 2015
Publication date	May 7, 2019
Grant date	May 7, 2019

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.

First claim

The embodiment of the invention in which an exclusive property or privilege is claimed is defined as follows:

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.

Assignees

• Tkac Peter
• Vandegrift Iii George F
• Rotsch David A
• Uchicago Argonne Llc

Inventors

• Tkac Peter
• Vandegrift Iii George F
• Rotsch David A

Classifications

• C22B7/007

  by acid leaching · CPC title

• C22B34/34 Primary

  Obtaining molybdenum {(treatment or purification of solutions by adsorption on solids C22B3/24, by liquid-liquid extraction C22B3/26, by ion-exchange extraction C22B3/42; preparation of molybdenum involving liquid-liquid extraction, adsorption or ion-exchange C01G39/003)} · CPC title

• Y02P10/234

  Cross-Sectional Technologies · mapped topic

• C22B3/0005

  Chemistry & Metallurgy · mapped topic

• C22B3/26

  by liquid-liquid extraction using organic compounds · CPC title