# US 11,028,461 B2 · Bauxite residue recycling > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,028,461 B2 - Document ID: US11028461B2 - Status: Granted - Kind: B2 - Application number: 16/030,041 - Filed: 2018-07-09 - Published: 2019-02-07 - Granted: 2021-06-08 - Earliest claimed: 2017-05-11 - Assignees: Worcester Polytechnic Institute - Applicants: Worcester Polytechnic Institute - Inventors: Marion H. Emmert; Remya P. Narayanan - Web page: https://patentgrep.com/patent/US11028461B2 ## CPC - C22B 59/00: Obtaining rare earth metals - C22B 3/44: by chemical processes (treatment or purification of solutions by liquid-liquid extraction C22B3/26, by ion-exchange extraction C22B3/42) - C22B 7/002: {by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)} - C22B 7/007: {by acid leaching} - Y02P 10/20: Recycling - C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS - Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS ## Abstract Recovery of scandium from mined red mud includes adding an acid to a quantity of red mud for converting oxides in the red mud, and roasting the quantity of red mud for decomposing compounds having low thermal stability, typically iron and titanium. Water is added to the roasted red mud for leaching the converted oxides into a leach liquor mixture including scandium and other dissolved rare earths, and the leach liquor mixture is agitated by sonication or ball milling to increase an exposed surface area of red mud particles in the leach liquor. PH of the leach liquor is adjusted to precipitate the rare earths while leaving the scandium in solution in the leach liquor, followed by precipitating the separated scandium oxalate remaining in the leach liquor by reducing the pH and adding oxalic acid. Precipitated scandium oxalate may then be filtered from the leach liquor. ## Claims ### Claim 1 A method for recovering scandium from mined red mud, comprising: adding an acid to a quantity of red mud for converting oxides in the red mud; roasting the quantity of red mud; adding water to the roasted red mud for leaching the converted oxides into a leach liquor mixture including scandium and rare earths; agitating the leach liquor mixture to increase an exposed surface area of red mud particles in the leach liquor; adjusting the pH of the leach liquor to precipitate the rare earths while leaving the scandium in solution in the leach liquor; precipitating scandium oxalate from the leach liquor by reducing the pH and adding oxalic acid; and filtering the precipitated scandium oxalate from the leach liquor. ### Claim 2 (depends on 1) The method of claim 1 wherein the red mud includes scandium, iron and titanium, further comprising extracting iron oxide and titanium oxide from the roasted red mud. ### Claim 3 (depends on 1) The method of claim 1 further comprising adding sulfuric acid to the red mud for converting oxides in the red mud to sulfates, the sulfates including iron, titanium and scandium. ### Claim 4 (depends on 3) The method of claim 3 wherein the roasting includes heating at least until iron sulfate and titanium sulfate form iron oxide and titanium oxide, respectively, and scandium sulfate and rare earth sulfates remain in solution. ### Claim 5 (depends on 4) The method of claim 4 wherein roasting occurs in a tube furnace, the tube furnace extracting sulfur trioxide and water vapors, the extracted sulfur trioxide unavailable for combination with the iron and titanium. ### Claim 6 (depends on 1) The method of claim 1 wherein the added acid performs sulphation, the sulphation and roasting results in undetectable levels of iron and titanium upon forming the leach liquor mixture, the levels being less than 5 ppm. ### Claim 7 (depends on 1) The method of claim 1 wherein the roasting occurs at temperatures in the range of 650° C. to 750° C. ### Claim 8 (depends on 1) The method of claim 1 wherein the roasting occurs at temperatures in the range of 700° C. to 715° C. ### Claim 9 (depends on 1) The method of claim 1 wherein adjusting the pH includes bringing the pH to around 8.0 for precipitating rare earths other than scandium. ### Claim 10 (depends on 9) The method of claim 9 further comprising adding sodium hydroxide to bring the pH to 8.0. ### Claim 11 (depends on 1) The method of claim 1 further comprising precipitating oxides including Y, La, Ce, Pr, Nd, Gd, Dy, Er, and Yb. ### Claim 12 (depends on 11) The method of claim 11 further comprising reducing the pH to 0.0 by adding H2SO4, and adding oxalic acid to bring the pH to 1.0. ### Claim 13 (depends on 1) The method of claim 1 wherein sulphating includes heating to between 100° C.-120° C. using a ratio of red mud to sulfuric acid to water of 1:0.8:0.4 for 18 hours to form metal sulfates, followed by roasting at a temperature >600° C. to decompose titanium and iron to oxide form. ### Claim 14 A method for recovering scandium from red mud waste resulting from bauxite mining, comprising: sulphating the red mud by adding sulfuric acid for converting oxides to sulfates; roasting the sulphated red mud until less than 5 ppm iron sulfate and titanium sulfate remain; agitating a leach mixture including the roasted red mud by sonication or ball milling to leach scandium from the red mud into a leach liquor; and precipitating rare earths other than scandium from the leach liquor to generate a solution including scandium sulfate. ### Claim 15 (depends on 14) The method of claim 14 further comprising precipitating scandium oxalate from the scandium sulfate solution by adding oxalic acid. ### Claim 16 In an aluminum/bauxite mining operation having a stream of red mud as a discarded byproduct, a method of processing and recovering scandium from the discarded red mud, comprising: gathering a quantity of red mud from a waste stream of byproducts resulting from bauxite mining; sulphating the quantity of red mud by adding sulfuric acid to convert oxides in the red mud to sulfates, the oxides including iron oxide and titanium oxide; roasting the sulphated red mud 700° C. for 1 hour in a tube furnace, the tube furnace providing ventilation for evacuating sulfates; leaching scandium by adding water to the roasted red mud to form a leach mixture; agitating the leach mixture by ball milling to expose crystalline structures of scandium to the water for leaching and resulting in a leach liquor including dissolved scandium and rare earths; adjusting the pH of the leach liquor to 8.0 from addition of sodium hydroxide to precipitate rare earths and leave scandium in solution in the leach liquor; filtering the precipitated rare earths to a filtrate including the dissolved scandium; reducing the pH to 1.0 by addition of sulfuric acid; and adding oxalic acid to precipitate scandium oxalate. ### Claim 17 (depends on 1) The method of claim 1 wherein precipitating the scandium oxalate includes bringing the pH to between 0.0 and 1.0. ### Claim 18 (depends on 17) The method of claim 17 further comprising adding H2SO4 to reduce the pH, and adding oxalic acid to combine with the scandium in solution to precipitate the scandium oxalate.