Method for separating and extracting rare-earth and regenerating rare-earth polishing powder from rare-earth polishing powder waste

Patent metadata

Field	Value
Publication number	US-2023286822-A1
Application number	US-202318139844-A
Country	US
Kind code	A1
Filing date	Apr 26, 2023
Priority date	Dec 2, 2020
Publication date	Sep 14, 2023
Grant date	—

Abstract

The invention relates to a method of separating and extracting rare-earths from rare-earth polishing powder waste and regenerating rare-earth polishing powder, which is characterized by: firstly, process the waste powder with first acid leaching, alkali roasting, and second acid leaching to separate and extract rare-earths from rare-earth polishing powder waste to obtain the leaching solution of rare-earth chloride; secondly, precipitate from the leaching solution with ammonia to remove impurities and hydrochloric acid solution to obtain the purified solution of rare-earth chloride; thirdly, co-precipitate from the solution acquired in the second step with hydrofluoric acid, ammonium bicarbonate, and dispersant to obtain the lanthanum cerium fluoro-carbonate; and finally, after drying, two-stage high-temperature calcination, and ball milling, the regenerated rare-earth polishing powder with decent polishing performance can be obtained. The total leaching efficiency of rare-earths in the rare-earth polishing powder waste of the present invention reaches more than 95%, and the total recovery efficiency of rare-earths reaches more than 93%, which realizes the efficient separation, extraction, and regeneration of rare-earths in the rare-earth polishing powder waste.

First claim

What is claimed is:

1 . A method of separating and extracting rare-earth and regenerating rare-earth polishing powder from rare-earth polishing powder waste, characterized by the following specific steps:
(1) Ball milling pretreatment: the rare-earth polishing powder waste is ball milled to a particle size of less than 200 mesh to obtain ball milled waste; (2) First acid leaching: put the ball milled waste obtained in step (1) into a container and add hydrochloric acid solution to obtain a mixture, heat and stir the mixture to conduct a first acid leaching reaction, and conduct filtration after the first acid leaching reaction is completed to obtain leaching residue and leaching liquor 1 , molar concentration of the hydrochloric acid solution is 5-8 mol/L, a solid-liquid ratio of the ball milled waste and the hydrochloric acid solution is 1:4-1:8 kg/L, leaching temperature is 70-80° C., and leaching time is 1-3 hours at a stirring speed of 500-600 rpm; (3) Alkali roasting: mix the leaching residue obtained in step (2) with alkali to obtain a mixture and roast the mixture to obtain a roasted mixture, a mass ratio of the leaching residue to the alkali is 1:1-1:5, roasting temperature is 800-1000° C., and roasting time is 1-3 hours; (4) Water leaching: put the roasted mixture obtained in step (3) in water and stir, a solid-to-liquid ratio of the roasted mixture and water is 1:4-1:9 kg/L in water leaching process, water leaching temperature is 80-90° C., water leaching time is 2-3 hours, and stirring speed is 500 to 600 rpm, after the water leaching process finishes, separate solid residue from liquid phase and conduct filtration to obtain water leaching residue; (5) Second acid leaching: add hydrochloric acid solution into the water leaching residue obtained in step (4) for a secondary acid leaching reaction, and after the secondary acid leaching reaction is completed, separate solid and liquid phase and conduct filtration to obtain leaching liquor 2 , a molar concentration of the hydrochloric acid solution is 6-10 mol/L, a solid-liquid ratio of the water leaching residue and the hydrochloric acid solution is 1:4-1:10 kg/L, leaching temperature is 80-90° C., leaching time is 2-6 hours, and stirring speed is 500-600 rpm; (6) Preparation of rare-earth hydroxide: mix the leaching liquor 1 obtained in step (2) and the leaching liquor 2 obtained in step (5) to obtain a mixed solution, add an ammonia solution with a mass percentage of 25% to the mixed solution while heating and stirring, until the pH of the solution reaches 8-9, conduct filtration to obtain rare-earth hydroxide, heating temperature is 90-95° C. , and stirring speed is 500-600 rpm; (7) Preparation of rare-earth chloride solution: add a hydrochloric acid solution with a mass percentage of 37% to the rare-earth hydroxide obtained in step (6) for acidolysis, and after white precipitate disappears, continue to add hydrochloric acid with a concentration of 37% by mass until pH reaches 2-4 to obtain a rare-earth chloride solution; (8) Preparation of lanthanum cerium fluoro-carbonate: add hydrofluoric acid with a mass percentage of 40% to the rare-earth chloride solution obtained in step (7), and add an ammonium bicarbonate solution with a mass concentration of 100-120 g/L at a rate of 20-30 ml/min while stirring, then add dispersant to the mixed solution while stirring, age in a constant temperature water bath for 2-4 hours, and conduct filtration to obtain lanthanum cerium fluoro-carbonate; a volume ratio of rare-earth chloride to hydrofluoric acid is 20:1-40:1, and a volume ratio of the ammonium bicarbonate solution to the rare-earth chloride solution is 1:1, a temperature of water bath is 50-60° C., a mass percentage of the dispersant is 1-2%, and stirring speed is 800-1000 rpm; (9) Regenerate rare-earth polishing powder: dry the lanthanum cerium fluoro-carbonate obtained in step (8) at 105° C. for 24 hours, and calcine at high temperature in a muffle furnace, the calcine process is as follows: raise the temperature from room temperature to 600° C. ; keep at 600° C. for 2-3 hours; then raise the temperature from 600° C. to 1000° C. at a heating speed of 1° C./min; keep at 1000° C. for 4-6 hours; ball mill and obtain regenerated rare-earth polishing powder.

2 . The method according to claim 1 , wherein the alkali used in the alkali roasting process in step (3) is NaOH or KOH.

3 . The method according to claim 1 , wherein the dispersant used in step (8) is one of the followings: polyethylene glycol-400, polyethylene glycol-600 or polyethylene glycol-800.

Assignees

• Univ Beijing Technology

Inventors

• Wu Yufeng
• Song Minwei
• Zhang Qijun

Classifications

• C22B7/007 Primary

  by acid leaching · CPC title

• C22B7/006

  Wet processes · CPC title

• C22B1/005

  Preliminary treatment of scrap (C22B1/02 - C22B1/26 take precedence) · CPC title

• C22B59/00

  Obtaining rare earth metals · CPC title

• C09G1/02 Primary

  containing abrasives or grinding agents {(abrasives as such C09K3/14; polishing of semi-conductors H10P52/40)} · CPC title