Method for recovering scandium

Patent metadata

Field	Value
Publication number	US-11214849-B2
Application number	US-201716077821-A
Country	US
Kind code	B2
Filing date	Feb 21, 2017
Priority date	Feb 23, 2016
Publication date	Jan 4, 2022
Grant date	Jan 4, 2022

Abstract

A method for recovering scandium, by which scandium is able to be recovered from nickel oxide ore. The present invention comprises: a leaching step S 1 for obtaining a leachate by leaching a nickel oxide ore containing scandium with use of sulfuric acid; a neutralization step by adding a neutralizing agent thereto; a sulfurization step by adding a sulfurizing agent to the post-neutralization solution; an ion exchange step by bringing the post-sulfurization solution into contact with a chelating resin; a dissolution step by obtaining a precipitate of scandium hydroxide by adding an alkali into the scandium eluent, and subsequently adding an acid solution to the scandium hydroxide; a solvent extraction step by bringing the scandium acid dissolution liquid into contact with a neutral extractant; and a scandium recovery step by adding oxalic acid to the extraction residue and subsequently roasting the salt of scandium oxalate.

First claim

The invention claimed is:

1. A method for recovering scandium comprising:
a leaching step of leaching nickel oxide ore containing scandium and an actinoid element with sulfuric acid at high temperature and high pressure to obtain a leachate and a leach residue;
a neutralization step of adding a neutralizing agent to the leachate to obtain a neutralized precipitate and a post-neutralization liquid;
a sulfuration step of adding a sulfurizing agent to the post-neutralization liquid to obtain nickel sulfide and a post-sulfuration liquid;
an ion exchange step of bringing the post-sulfuration liquid into contact with a chelating resin to adsorb scandium in the post-sulfuration liquid to the chelating resin and thus to obtain a scandium eluate;
a dissolution step of adding an alkali to the scandium eluate to obtain a precipitate of scandium hydroxide, then adding an acid solution to the scandium hydroxide, and performing acid dissolution to obtain a scandium-dissolved acid liquid;
a solvent extraction step of maintaining a pH of the scandium-dissolved acid liquid in a range of between 1.0 or more and 2.5 or less and bringing the scandium-dissolved acid liquid into contact with a neutral extractant containing phosphorus to extract and separate impurity elements other than scandium and to obtain a raffinate liquid containing scandium; and
a scandium recovering step of adding oxalic acid to the raffinate liquid to generate a salt of scandium oxalate and roasting the salt of scandium oxalate to obtain scandium oxide.

2. The method for recovering scandium according to claim 1 , wherein the chelating resin is a resin containing iminodiacetic acid as a functional group, and the ion exchange step includes:
an adsorption step of bringing the post-sulfuration liquid into contact with the chelating resin to adsorb the scandium to the chelating resin;
an aluminum removing step of bringing a sulfuric acid solution at 0.1 N or less into contact with the scandium-adsorbed chelating resin in the adsorption step to remove aluminum adsorbed to the chelating resin in the adsorption step;
a scandium elution step of bringing a sulfuric acid solution at 0.3 N or more and less than 3 N into contact with the chelating resin subjected to the aluminum removing step to obtain the scandium eluate; and
a chromium removing step of bringing a sulfuric acid solution at 3 N or more into contact with the chelating resin subjected to the scandium elution step to remove chromium adsorbed to the chelating resin in the adsorption step.

3. The method for recovering scandium according to claim 1 , wherein
the solvent extraction step includes:
an extraction step of mixing the scandium-dissolved acid liquid with an organic solvent containing the neutral extractant and separating the mixture into a post-extraction organic solvent extracted impurity elements other than scandium and a raffinate liquid;
a scrubbing step of mixing the post-extraction organic solvent with an acid solution having a concentration of 1.0 mol/1 or more and 5.0 mol/1 or less and recovering scandium from the post-extraction organic solvent to obtain a post-washing organic solvent; and
a backward extraction step of adding a backward extractant to the post-washing organic solvent and backward extracting impurity elements from the post-washing organic solvent to obtain a backward extraction liquid.

4. The method for recovering scandium according claim 1 , wherein a scandium-dissolved nitric acid liquid of a scandium-dissolved acid liquid is obtained by adding a nitric acid solution to the scandium hydroxide and performing acid dissolution in the dissolution step.

5. The method for recovering scandium according to claim 1 , wherein a scandium-dissolved hydrochloric acid liquid of a scandium-dissolved acid liquid is obtained by adding a hydrochloric acid solution to the scandium hydroxide and performing acid dissolution in the dissolution step.

6. The method for recovering scandium according to claim 5 , wherein in the solvent extraction step,
a chloride concentration in the scandium-dissolved hydrochloric acid liquid obtained in the dissolution step is adjusted to 2.0 mol/1 or more and 6.0 mol/1 or less and the scandium-dissolved hydrochloric acid liquid is brought into contact with the neutral extractant.

7. The method for recovering scandium according to claim 1 , wherein the scandium recovering step includes:
a step of adding sodium hydroxide having a concentration of 5.0 mol/1 or more and 8.0 mol/1 or less to the raffinate liquid obtained in the solvent extraction step to obtain a precipitate of scandium hydroxide;
a step of dissolving the precipitate of scandium hydroxide obtained with sulfuric acid or hydrochloric acid and adding oxalic acid to the dissolved liquid obtained through the dissolution to obtain a crystal of scandium oxalate; and
a step of calcining the crystal of scandium oxalate.

8. The method for recovering scandium according to claim 2 , wherein
the solvent extraction step includes:
an extraction step of mixing the scandium-dissolved acid liquid with an organic solvent containing the neutral extractant and separating the mixture into a post-extraction organic solvent extracted impurity elements other than scandium and a raffinate liquid;
a scrubbing step of mixing the post-extraction organic solvent with an acid solution having a concentration of 1.0 mol/1 or more and 5.0 mol/1 or less and recovering scandium from the post-extraction organic solvent to obtain a post-washing organic solvent; and
a backward extraction step of adding a backward extractant to the post-washing organic solvent and backward extracting impurity elements from the post-washing organic solvent to obtain a backward extraction liquid.

9. The method for recovering scandium according claim 2 , wherein a scandium-dissolved nitric acid liquid of a scandium-dissolved acid liquid is obtained by adding a nitric acid solution to the scandium hydroxide and performing acid dissolution in the dissolution step.

10. The method for recovering scandium according claim 3 , wherein a scandium-dissolved nitric acid liquid of a scandium-dissolved acid liquid is obtained by adding a nitric acid solution to the scandium hydroxide and performing acid dissolution in the dissolution step.

11. The method for recovering scandium according to claim 2 , wherein a scandium-dissolved hydrochloric acid liquid of a scandium-dissolved acid liquid is obtained by adding a hydrochloric acid solution to the scandium hydroxide and performing acid dissolution in the dissolution step.

12. The method for recovering scandium according to claim 3 , wherein a scandium-dissolved hydrochloric acid liquid of a scandium-dissolved acid liquid is obtained by adding a hydrochloric acid solution to the scandium hydroxide and performing acid dissolution in the dissolution step.

13. The method for recovering scandium according to claim 2 , wherein the scandium recovering step includes:
a step of adding sodium hydroxide having a concentration of 5.0 mol/1 or more and 8.0 mol/1 or less to the raffinate liquid obtained in the solvent extraction step to obtain a precipitate of scandium hydroxide;
a step of dissolving the precipitate of scandium hydroxide obtained with sulfuric acid or hydrochloric acid and adding oxalic acid to the dissolved liquid obtained through the dissolution to obtain a crystal of scandium oxalate; and
a step of calcining the crystal of scandium oxalate.

14. The method for recovering scandium according to claim 3 , wherein the scandium recovering step includes:
a step of adding sodium hydroxide having a concentration of 5.0 mol/1

Assignees

• Sumitomo Metal Mining Co

Inventors

• Nagai Hidemasa
• Kudo Keiji
• Matsuoka Itsumi
• Ozaki Yoshitomo
• Shoji Hirofumi
• Matsumoto Shin-Ya
• Higaki Tatsuya

Classifications

• C22B3/26

  by liquid-liquid extraction using organic compounds · CPC title

• C22B3/44

  by chemical processes (treatment or purification of solutions by liquid-liquid extraction C22B3/26, by ion-exchange extraction C22B3/42) · CPC title

• C01G53/11

  Sulfides; Oxysulfides · CPC title

• C01F17/13

  by using ion exchange resins, e.g. chelate resins · CPC title

• C22B3/08

  Sulfuric acid {, other sulfurated acids or salts thereof} · CPC title