A method for recovering NdFeB casing sludge waste by ca-chloride reduction diffusion technology

A technology for recycling NdFeB and NdFeB, which is applied to the improvement of process efficiency, transportation and packaging, metal processing equipment, etc., which can solve the problem of increasing the secondary use and waste of resources, reducing the efficiency of waste recycling, and not considering the use of calcium and other issues, to achieve the effect of environmentally friendly resource recycling, resource conservation, and resource recycling

Active Publication Date: 2020-01-24
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although our previous Chinese patent (Application No.: 201510101336.1) discloses a short-process technology for recycling NdFeB sludge, this technology needs to give priority to the pretreatment of NdFeB sludge waste in the recycling process, which increases the resource consumption. use and waste
In addition, a certain amount of raw materials such as neodymium oxide and iron boron need to be added in the recycling process, and the use of calcium is not considered, and the secondary use of resources increases the recycling cost and reduces the recycling efficiency of waste.

Method used

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  • A method for recovering NdFeB casing sludge waste by ca-chloride reduction diffusion technology
  • A method for recovering NdFeB casing sludge waste by ca-chloride reduction diffusion technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 50g of NdFeB casing sludge and dry it in a blast drying oven at 60°C for 10 hours, and then disperse it by grinding after drying; add 15g of metal calcium particles and 27.8g of potassium chloride to the ground sludge powder, and dry it at 950°C , insulated under an argon atmosphere for 2 hours; the product obtained was soaked in water at 2°C for 30 minutes, and the powder was initially selected with a magnet; the obtained magnetic powder was ultrasonically cleaned with 5vol.% dilute acetic acid for 10 minutes, and then the powder was washed with distilled water until The pH value of the solution is about 8, and finally washed once with alcohol; the cleaned powder is dried in a vacuum environment, and the oxygen content of the dried powder is about 3800ppm; after drying, prevent contact with air and place it directly in a glove box with an argon atmosphere Medium; powder doped with 30wt.% Nd 4 Fe 14 The B alloy powder is rotated in a rolling ball mill for 1.5h, or...

Embodiment 2

[0022] Take 50g of NdFeB bushing sludge and dry it in a blast drying oven at 80°C for 15 hours, and then disperse it by grinding after drying; add 18g of metal calcium particles and 35g of potassium chloride to the ground sludge powder, and dry it at 830°C, Insulate for 2 hours under an argon atmosphere; soak the obtained product in water at 5°C for 60 minutes, and use a magnet to initially select the powder; ultrasonically clean the obtained magnetic powder with 10vol.% dilute acetic acid for 15 minutes, and then wash the powder with distilled water to a solution The pH value is about 8, and finally washed once with alcohol; the cleaned powder is dried in a vacuum environment, and the oxygen content of the dried powder is about 3000ppm; after drying, prevent contact with air and place it directly in a glove box with an argon atmosphere ;Powder doped with 35wt.% Nd 3 PrFe 14 The B alloy powder is rotated in a rolling ball mill for 1.5h, oriented and pressed in a nitrogen atmo...

Embodiment 3

[0024] Take 50g of NdFeB casing sludge and dry it in a blast drying oven at 100°C for 20 hours. After drying, it is dispersed by grinding; the grinded sludge powder is added with 20g of metal calcium particles and 50g of potassium chloride, and dried at 1150°C, Insulate for 2 hours under an argon atmosphere; soak the obtained product in water at 5°C for 90 minutes, and use a magnet to initially select the powder; ultrasonically clean the obtained magnetic powder with 15vol.% dilute acetic acid for 15 minutes, and then wash the powder with distilled water to a solution The pH value is about 8, and finally washed once with alcohol; the cleaned powder is dried in a vacuum environment, and the oxygen content of the dried powder is about 2500ppm; after drying, prevent contact with air and place it directly in a glove box with an argon atmosphere ;Powder doped with 40wt.% Nd 2 PR 1 Dy 1 Fe 14 The B alloy powder is rotated in a rolling ball mill for 1.5h, oriented and pressed in a...

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Abstract

The invention discloses a method for recovering NdFeB casing oil sludge waste through Ca-chloride reduction and diffusion technology, which belongs to the technical field of solid waste recovery and reuse in the rare earth permanent magnet industry. The process includes drying of sintered NdFeB oil sludge waste, reduction and diffusion of Ca-chloride, decalcification by immersion at low temperature, doping of rare earth-rich alloy powder, sintering and heat treatment. Using NdFeB casing hole sludge waste as raw material, Ca-KCl direct reduction and diffusion is used to obtain regenerated NdFeB magnetic powder, and the recovered powder can be sintered to produce regenerated sintered magnets. In this invention, potassium chloride is used as a low-melting point auxiliary agent, which can reduce the reaction temperature and shorten the reaction time, improve the recovery rate, and reduce the amount of calcium metal; the use of low-temperature decalcification can prevent powder oxidation and improve decalcification efficiency; The use of rare earth alloys can supplement rare earths, which is beneficial to composition adjustment and industrial production. The invention realizes the purposes of shortening the recycling process, reducing the recycling cost, reducing the environmental burden and increasing the utilization rate of waste materials.

Description

technical field [0001] The invention relates to a technology for manufacturing regenerated sintered magnets from NdFeB oil sludge waste, and belongs to the technical field of solid waste recovery and reuse in the rare earth permanent magnet industry. Background technique [0002] With the demand for new energy in modern society, energy conversion materials have also been vigorously developed, and the development of rare earth permanent magnet materials has made a huge contribution. As the third generation of rare earth permanent magnet materials, NdFeB permanent magnet materials have been widely used in various fields of science and technology because of their excellent magnetic properties, and the output of sintered NdFeB magnets has also increased year by year. In order to meet the needs of various fields, sintered NdFeB magnets are subjected to different machining processes to obtain the required surface accuracy, size, and shape, and 20% to 30% of sludge waste is generat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/00C22B5/04B22F9/20B22F1/00
CPCC22B5/04C22B7/001B22F9/20B22F1/14Y02P10/20
Inventor 岳明尹小文刘敏路清梅刘卫强王峰邱玉冰徐海波
Owner BEIJING UNIV OF TECH
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