A method of recovering NdFeB oil sludge using reduction diffusion technology

A technology for recycling NdFeB and NdFeB, applied in the direction of recycling technology, etc., can solve the problems of inability to be applied, magnetic powder has no magnetic properties, etc., and achieve the effect of convenient subsequent processing, avoiding secondary waste, and efficient environmental protection process.

Active Publication Date: 2016-11-02
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can be used to obtain sintered NdFeB magnetic powder from NdFeB oil sludge, the obtained magnetic powder has no magnetic properties and cannot be used in practice.

Method used

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  • A method of recovering NdFeB oil sludge using reduction diffusion technology
  • A method of recovering NdFeB oil sludge using reduction diffusion technology
  • A method of recovering NdFeB oil sludge using reduction diffusion technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 40g of NdFeB sludge waste into a beaker, add 400mL of water, heat and distill in a water bath, and dry to obtain 35.2g of sludge powder; add 469mL to the sludge powder to a concentration of 3mol L -1 Hydrochloric acid solution, heated in a water bath at 60°C to dissolve the acid, kept warm for 20 minutes, filtered, and retained the supernatant; use 7mol L -1 Ammonia solution is adjusted to pH=2.0, and 77g of oxalic acid crystals (H 2 C 2 o 4 2H 2 O), added to the above solution, heated in a water bath at a temperature of 70°C, kept warm for 20min, centrifuged in a centrifuge, and the centrifugal speed was 7500r min -1 , time 10min, washed the precipitate 3 times, and dried to obtain the co-precipitation product; put the co-precipitation product into the muffle furnace for roasting, the roasting temperature was 850°C, and the time was 120min to obtain the mixed oxide; test XRD (such as figure 1 Shown) and XRF (as shown in Table 1). Depend on figure 1It can be...

Embodiment 2

[0026] Weigh 40g of NdFeB sludge waste into a beaker, add 400mL of water, heat and distill in a water bath, and dry to obtain 36.2g of sludge powder; add 483mL to the sludge powder to a concentration of 3mol L -1 hydrochloric acid solution, heated in a water bath at 80°C to dissolve the acid, kept warm for 30 minutes, filtered, and retained the supernatant; use 7mol L -1 Ammonia solution is adjusted to pH=2.0, and 80g of oxalic acid crystals (H 2 C 2 o 4 2H 2 O), added to the above solution, heated in a water bath at a temperature of 90°C, kept warm for 30min, centrifuged in a centrifuge, and the centrifugal speed was 7500r min -1 , for 10 minutes, washed the precipitate with water three times, and dried to obtain the co-precipitated product; put the co-precipitated product into a muffle furnace for roasting at a temperature of 900°C for 180 min to obtain a mixed oxide; test XRF, and the results are shown in Table 2.

[0027] According to the mass ratio of rare earth eleme...

Embodiment 3

[0029] Weigh 40g of NdFeB sludge waste into a beaker, add 400mL of water, heat and distill in a water bath, and dry to obtain 33.8g of sludge powder; add 451mL to the sludge powder to a concentration of 3mol L -1 Hydrochloric acid solution, heated in a water bath at 70°C to dissolve the acid, kept warm for 25 minutes, filtered, and retained the supernatant; use 7mol L -1 Ammonia solution is adjusted to pH=2.0, and 74g oxalic acid crystals (H 2 C 2 o 4 2H 2 O), added to the above solution, heated in a water bath at a temperature of 80°C, kept warm for 25min, centrifuged in a centrifuge, and the centrifugal speed was 7500r min -1 , for 10 minutes, washed the precipitate with water three times, and dried to obtain the co-precipitated product; put the co-precipitated product into a muffle furnace for roasting at a temperature of 870°C for 150 min to obtain a mixed oxide; test XRF, and the results are shown in Table 3.

[0030] According to the mass ratio of rare earth elements...

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Abstract

The invention discloses a method for recycling NdFeB oil sludge according to a reduction-diffusion technology, and belongs to the technical field of recycling of NdFeB oil sludge. The method comprises the following steps: (1) oil sludge pretreatment and acid dissolution, (2) co-precipitation and roasting, (3) calcium reduction and diffusion, (4) rinsing and drying, (5) powder mixing and sintering, and the like. The method is efficient and environmentally friendly, and has the advantages that when an NdFeB oil sludge waste material is taken as a raw material, a regenerative NdFeB magnet can be directly obtained; magnetic field ultrasonic treatment is adopted in a rinsing process, so that calcium oxide and other nonmagnetic substances can be effectively removed; through an addition of nanometer powder, the maximum magnetic energy product of the obtained regenerative NdFeB sintered magnet can reach 32 MGOe.

Description

technical field [0001] The invention relates to recycling NdFeB oil sludge to prepare a regenerated sintered NdFeB magnet, and belongs to the technical field of NdFeB oil sludge recovery and utilization. Background technique [0002] Compared with other magnetic materials, NdFeB magnetic materials have excellent magnetic and mechanical properties. Therefore, it is widely used in many fields such as electronic information, household appliances, medical treatment, aerospace, etc., especially plays an important role in the fields of new green energy such as energy-saving vehicles and wind power generation. The wide range of applications brings about a rapid increase in annual output, but in the production process of sintered NdFeB magnets, about 30% of the total weight of raw materials will produce NdFeB waste, including turning blocks and sludge waste. Take China as an example: China is a major producer of NdFeB materials. In 2013, the output was 94,000 tons, accounting for 9...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F8/00B22F9/20
CPCY02W30/50
Inventor 岳明李现涛刘卫强李萌张东涛
Owner BEIJING UNIV OF TECH
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