Recovery and purification of transition elements

Patent metadata

Field	Value
Publication number	US-2016333442-A1
Application number	US-201514826334-A
Country	US
Kind code	A1
Filing date	Aug 14, 2015
Priority date	May 12, 2015
Publication date	Nov 17, 2016
Grant date	—

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 liquor; b. mixing the liquor with acid thereby generating a solution, wherein the transition metal resides within the solution; c. combining the solution with an organic liquid to transfer the transition metal within the organic liquid; d. washing the extracted transition metal in the organic liquid with acid so as to remove potassium and other contaminants from the organic liquid phase; and e. removing the transition metal from the organic phase.

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

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

4 . The method as recited in claim 1 wherein the combining step further results in potassium salt and nontargeted metals being confined to an aqueous phase in the extraction process.

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 contacting step yields organic solution which is recycled to the mixing step.

7 . The method as recited in claim 1 wherein the transition metal is Mo, or Tc, or Ti, or Ga, or Sb, or Zn, or Sn, or Nb, and combinations thereof.

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

9 . The method as recited in claim 8 wherein the solid phase comprises the transition metals.

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

11 . The method as recited in claim 10 wherein the salt is heated to create solid phase molybdenum oxide, or, lower oxide or molybdenum metal, or other oxides of transition metals.

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

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

14 . The method as recited in claim 11 wherein the minimal molarity of the hydroxide is approximately 0.1M.

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

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

• C22B3/26

  by liquid-liquid extraction using organic compounds · CPC title

• Y02P10/20

  Recycling · CPC title