Magnetite production from bauxite residue

Patent metadata

Field	Value
Publication number	US-10836649-B2
Application number	US-201816213243-A
Country	US
Kind code	B2
Filing date	Dec 7, 2018
Priority date	Dec 8, 2017
Publication date	Nov 17, 2020
Grant date	Nov 17, 2020

Abstract

A low-temperature leaching operation employs a raw, red mud slurry directly from aluminum production for an oxalic acid leaching of ferric oxalate. Residual calcium, titanium, aluminum and other rare earths are also recoverable in a secondary stream. Monitoring and control of the pH of the leach solution yields soluble ferric oxalate without high temperatures or specific radiation or light sources. Addition of iron powder results in precipitation of ferrous oxalate, isolated by magnetic separation from the iron powder which recirculates in the solution. Magnetite may then be produced by heating the ferrous oxalate in low pO2 conditions.

First claim

What is claimed is:

1. A method for extracting ferrous oxalate from red mud, comprising:
grinding raw red mud to a particulate size of P 80 of 75 microns;
adding a leach agent consisting of oxalic acid to the ground, raw red mud to form a leach solution;
monitoring and controlling the pH of the leach solution to maintain the pH in a range between 1.5-3.0 to form ferric oxalate in the leach solution;
adding iron powder to the leach solution for combining with the ferric oxalate in the leach solution;
precipitating ferrous oxalate from the leach solution;
extracting a secondary recycling stream including Al and Ti from insoluble oxalates remaining in the leach solution following precipitation of the ferrous oxalate from the leach solution; and
separating the iron powder from the ferrous oxalate via magnetic separation, the iron powder returned to continue precipitation of ferrous oxalate.

2. The method of claim 1 further comprising maintaining the temperature of the leach solution between 80-100° C. during leaching of the ferric oxalate and maintaining the temperature at least at 50° C. during precipitation of the ferrous oxalate.

3. The method of claim 1 wherein the raw red mud is a hydrated slurry resulting from a waste stream in aluminum refinement.

4. The method of claim 1 further comprising monitoring and controlling the pH of the leach solution to a range between 2.0-2.5 for leaching ferric oxalate.

5. The method of claim 1 further comprising maintaining the temperature of the leach solution between 90-95° C. during leaching of the ferric oxalate.

6. The method of claim 1 further comprising heating the precipitated ferrous oxalate in a low pO 2 environment for generating magnetite.

7. The method of claim 6 further comprising heating in the range of 500-1300° C.

8. The method of claim 1 wherein maintaining the pH during oxalic acid leaching until precipitation of the ferrous oxalate results in formation of insoluble ferrous oxalate from soluble ferric oxalate in the leach solution.

9. The method of claim 1 further comprising receiving the raw red mud as a byproduct form aluminum refining.

10. The method of claim 9 further comprising co-locating a containment apparatus for the red mud and precipitated ferrous oxalate with an aluminum refining operation for receiving the raw red mud from the co-located aluminum refinement.

11. The method of claim 1 further comprising performing precipitation in ambient visible light and an absence of UV lighting.

12. The method of claim 1 further comprising heating the precipitated ferrous oxalate in a reduced partial pressure pO 2 environment for generating at least 99% pure magnetite.

13. The method of claim 12 further comprising heating the precipitated ferrous oxalate in an N 2 , low pO 2 atmosphere in a vertical tube furnace.

14. A method for extracting ferrous oxalate from red mud, comprising:
grinding raw red mud to a particulate size of P80 of 75 microns;
adding a leach agent consisting of oxalic acid to a hydrated slurry of the around red mud to form a leach solution, the red mud resulting from a waste stream in aluminum refinement;
monitoring and controlling the pH of the leach solution to maintain the pH of the leach solution in a range between 1.5-3.0 to form ferric oxalate in the leach solution;
maintaining the temperature of the leach solution between 80-100° C. during leaching of the ferric oxalate;
adding iron powder to the leach solution for combining with ferric oxalate in the leach solution;
precipitating and filtering ferrous oxalate from the leach solution;
extracting a secondary recycling stream including Al and Ti from insoluble oxalates remaining in the leach solution following precipitation of the ferrous oxalate from the leach solution; and
separating the iron powder from the ferrous oxalate via magnetic separation, the iron powder returned to continue precipitation of ferrous oxalate.

Assignees

• Worcester Polytech Inst

Inventors

• Gostu Sumedh
• Mishra Brajendra

Classifications

• Y02P10/20

  Recycling · CPC title

• C07F15/025

  without a metal-carbon linkage · CPC title

• C22B3/16

  in organic solutions · CPC title

• C01G49/08 Primary

  Ferroso-ferric oxide [Fe3O4] · CPC title