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Method for preparing rare earth oxyfluoride

A technology of oxyfluoride and rare earth, which is applied in the field of preparation of rare earth oxyfluoride, can solve the problems of high acidity, difficult treatment, and high fluoride ion concentration of fluorine-containing waste liquid, and achieve effective utilization, high recovery rate, and simple process flow Effect

Active Publication Date: 2021-08-03
内蒙古科技大学包头师范学院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, such fluorine-containing waste liquid has high acidity, high fluoride ion concentration, and is difficult to treat. It needs to undergo neutralization acid, defluorination and other processes before it can be discharged.

Method used

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  • Method for preparing rare earth oxyfluoride
  • Method for preparing rare earth oxyfluoride
  • Method for preparing rare earth oxyfluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0044] This embodiment provides a method for preparing rare earth oxyfluoride, comprising the following steps:

[0045] (1) Mix NdFeB superfine powder waste with a solution containing fluoride ions, stir and react at room temperature for 12 hours to completely dissolve iron oxide, and Nd(OH) 3 React with fluoride ions to form Nd(OH) 2 F precipitation;

[0046] (2) precipitation in the centrifugal separation reaction system;

[0047] (3) Dry the separated precipitate at 650° C. for 4 hours to obtain NdOF powder.

[0048] Among them, the solution containing fluoride ion has a fluoride ion concentration of 0.1mol L -1 Ferric fluoride and a concentration of 1mol L -1The nitric acid solution has a pH value of 0.

[0049] After detection and calculation, the fluoride ion concentration in the solution after separation and precipitation is 0.005mol L -1 , the pH value is 0.51; the total recovery rate of rare earth is 99.5%.

[0050] Figure 5 For the SEM images of different ma...

Embodiment 2

[0052] This embodiment provides a method for preparing rare earth oxyfluoride, comprising the following steps:

[0053] (1) Mix the NdFeB ultrafine powder waste with the solution containing fluoride ions, stir and react at room temperature for 8 hours, so that the iron oxide is completely dissolved, and the Nd(OH) 3 React with fluoride ions to form Nd(OH) 2 F precipitation;

[0054] (2) precipitation in the centrifugal separation reaction system;

[0055] (3) Dry the separated precipitate at 110° C. for 24 hours, and then at 600° C. for 2 hours to obtain NdOF powder.

[0056] Among them, the solution containing fluoride ion has a fluoride ion concentration of 15mol L -1 Potassium fluoride and nitric acid solution, the pH of the solution is 1.

[0057] After detection and calculation, the fluoride ion concentration of the solution after separation and precipitation is 14.98mol L -1 , the pH value is 7.2; the total recovery rate of rare earth is 98.8%.

Embodiment 3

[0059] This embodiment provides a method for preparing rare earth oxyfluoride, comprising the following steps:

[0060] (1) Mix NdFeB superfine powder waste with a solution containing fluoride ions, stir and react at room temperature for 12 hours to completely dissolve iron oxide, and Nd(OH) 3 React with fluoride ions to form Nd(OH) 2 F precipitation;

[0061] (2) precipitation in the centrifugal separation reaction system;

[0062] (3) Dry the separated precipitate at 110° C. for 24 hours, and then at 600° C. for 2 hours to obtain NdOF powder.

[0063] Among them, the solution containing fluoride ion has a fluoride ion concentration of 15mol L -1 Potassium fluoride and nitric acid solution, the pH of the solution is 3.

[0064] After detection and calculation, the fluoride ion concentration in the solution after separation and precipitation is 14.98mol L -1 , the pH value is 7.1; the total recovery rate of rare earth is 95.6%.

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Abstract

The invention discloses a method for preparing rare earth oxyfluoride. The method comprises the following steps of: mixing a treatment object at least containing rare earth hydroxide with a solution containing fluorine ions at normal temperature and normal pressure, separating precipitates generated by a reaction, and drying the precipitates to obtain the rare earth oxyfluoride. According to the method, the principle that rare earth hydroxide reacts with fluorine ions is utilized, the neodymium-iron-boron ultrafine powder waste with the main existence form of rare earth being Nd(OH)3 reacts with fluorine-containing waste liquid, so the fluorine content of the fluorine-containing acid liquid is reduced while the rare earth in the neodymium-iron-boron ultrafine powder waste is recycled, and reutilization of fluorine in the fluorine-containing acid liquid is achieved; and when the method is used for recovering the rare earth, a technological process is simple, the rare earth elements in the neodymium-iron-boron ultrafine powder waste can be extracted only through one-step precipitation, large economic benefits are obtained, and the recovery rate of the rare earth is high and can be higher than 99%.

Description

technical field [0001] The invention relates to the technical field of metallurgy, in particular to a method for preparing rare earth oxyfluorides by using waste NdFeB superfine powder. Background technique [0002] NdFeB has excellent magnetic properties and is widely used in electronic products, wind power generation, new energy vehicles and other fields. At present, more than 150,000 tons of NdFeB are produced in the world every year, and about 30% of NdFeB waste will be generated during the processing process. Among them, about 1.5 kg of NdFeB superfine NdFeB will be produced for every 1 ton of NdFeB produced. powder waste. These ultrafine powder wastes contain 30% to 50% of rare earth elements in the form of rare earth hydroxides. How to recover the rare earth elements in these ultrafine powders is an important research direction. Patent application 201910362707.X discloses a method of using hydrofluoric acid as a solvent to convert rare earth compounds in ultrafine p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/265C01F17/10B82Y30/00B82Y40/00
CPCC01F17/265C01F17/10B82Y30/00B82Y40/00C01P2002/72C01P2004/03C01P2002/88C01P2004/64Y02P10/20
Inventor 孙鹤杨育圣
Owner 内蒙古科技大学包头师范学院
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