Method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge

A technology of NdFeB and oil sludge, which is applied in the field of NdFeB oil sludge recovery and reuse, can solve the problem of high cost and achieve the effect of short recovery path, simple operation and low recovery cost

Active Publication Date: 2014-06-25
BEIJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The smelting method uses metal neodymium as raw material, which ha

Method used

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  • Method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge
  • Method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge
  • Method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Weigh 20g of NdFeB sludge and add 50ml of water to dissolve it in a beaker;

[0048] (2) Add the mixed liquid to the rotating bottle and fix it on the right end of the rotating shaft;

[0049] (3) Close the vacuum valve, vacuum, and keep the pressure inside the tube at 0.01MPa;

[0050] (4) Set the temperature to 50°C, the rotation speed to 10rpm, adjust the height of the rotating bottle, turn on the heating button and the rotating button of the rotary evaporator, and start the water bath heating;

[0051] (5) Take out the remainder after the water has evaporated.

[0052] (6) Put the remainder in a beaker, add an appropriate amount of 4mol / L hydrochloric acid, add excess hydrogen peroxide to stir after dissolution, and remove non-metal elements such as B after filtration;

[0053] (7) Adjust the pH of the solution to 8 by adding ammonia with a volume ratio of 1:1, and let it stand for 1 hour;

[0054] (8) After centrifugation, dry the precipitate and place it in a box furnace ...

Embodiment 2

[0063] (1) Weigh 20g of NdFeB sludge and add 50ml of water to dissolve it in a beaker;

[0064] (2) Add the mixed liquid to the rotating bottle and fix it on the right end of the rotating shaft;

[0065] (3) Close the vacuum valve, vacuumize, and keep the pressure in the tube at 0.08MPa;

[0066] (4) Set the temperature to 70°C, the rotation speed to 100rpm, adjust the height of the rotating bottle, turn on the heating button and the rotating button of the rotary evaporator, and start the water bath heating;

[0067] (5) Take out the remainder after the water has evaporated.

[0068] (6) Put the remainder in a beaker, add an appropriate amount of 4mol / L hydrochloric acid, add excess hydrogen peroxide to stir after dissolution, and remove non-metal elements such as B after filtration;

[0069] (7) Adjust the pH of the solution to 9 by adding ammonia with a volume ratio of 1:1, and let it stand for 1.5;

[0070] (8) After centrifugation, the precipitate is dried and placed in a box furnace ...

Embodiment 3

[0080] (1) Weigh 20g of NdFeB sludge and add 50ml of water to dissolve it in a beaker;

[0081] (2) Add the mixed liquid to the rotating bottle and fix it on the right end of the rotating shaft;

[0082] (3) Close the vacuum valve, vacuum, and maintain the pressure inside the tube at 0.1MPa;

[0083] (4) Set the temperature to 100°C, the rotation speed to 300rpm, adjust the height of the rotating bottle, turn on the heating button and the rotating button of the rotary evaporator, and start the water bath heating;

[0084] (5) Take out the remainder after the water has evaporated.

[0085] (6) Put the remainder in a beaker, add an appropriate amount of 4mol / L hydrochloric acid, add excess hydrogen peroxide to stir after dissolution, and remove non-metal elements such as B after filtration;

[0086] (7) Adjust the pH of the solution to 9 by adding ammonia with a volume ratio of 1:1, and let it stand for 2 hours;

[0087] (8) After centrifugation, dry the precipitate and place it in a box fu...

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Abstract

The invention discloses a method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge, and belongs to the technical field of recovering and recycling of the neodymium iron boron oily sludge. The method comprises the following technological processes: distilling and separating neodymium iron boron oily sludge; coprecipitating and recovering all valuable elements; mixing oxides; adding the substances such as calcium metal and the like according to the ratio; mixing reactants; carrying out thermal reduction and diffusion at high temperature; removing a calcium oxide in the product; drying in vacuum; forming the regenerated neodymium iron boron magnetic powder, wherein the step of 'coprecipitating and recovering all valuable elements' can be accepted or rejected according to existence of metal elements harmful to the magnetic property in the neodymium iron boron oily sludge; a part of impurities are removed from the neodymium iron boron oily sludge by distillation and separation; the mixed oxides are obtained by coprecipitation of the valuable elements; calcium metal particles are added, and subjected to reduction diffusion reaction at 850-1150 DEG C; the regenerated neodymium iron boron magnetic powder can be directly obtained from the product after chemical separation and drying. The method has the advantages that environmental protection is facilitated, the technological process is shortened, the recovery cost is reduced, and a part of technical problems are solved.

Description

Technical field [0001] The invention relates to a method for preparing regenerated NdFeB magnetic powder from NdFeB sludge, and belongs to the technical field of NdFeB sludge recovery and reuse. technical background [0002] Since the conversion of NdFeB to industrial production, the world's sintered NdFeB output has increased day by day. The development of sintered NdFeB magnets in China has grown by leaps and bounds, with an annual growth rate of about 30% to 50%. However, with the rapid development of sintered NdFeB in China, the production of sintered NdFeB The utilization of rare earths, the raw material used by NdFeB, is also increasing at an alarming rate. Although China’s industrial reserves of rare earth resources account for about 80% of the world’s total, it is a veritable large country of rare earth resources. If the recycling of raw materials is not considered, it is still Will soon face the grim reality of lack of resources. [0003] In the production and processing ...

Claims

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Application Information

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IPC IPC(8): C22B7/00B22F9/16H01F1/057
CPCY02P10/20
Inventor 刘敏尹小文李春燕赖伟鸿朱伟华索红莉岳明
Owner BEIJING UNIV OF TECH
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