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Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation

A neodymium-iron-boron and co-precipitation technology, applied in the direction of improving process efficiency, can solve the problems of human injury, acid-base waste liquid is difficult to handle, not made into industrial products, etc., and achieves short operation process and avoids large-scale reagents. Use, the effect of low impurity content

Active Publication Date: 2013-10-09
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Based on the above current rare earth recovery methods, although these processes can regain rare earths, there are still many problems: first of all, from the results, the circular chain of the above processes does not form a real cycle, and the products obtained by these processes are only Rare earth oxides, but not made into industrial products that can be used directly
Only in the extraction process, because of the need for a higher liquid-to-liquid ratio and better stripping effect, the acid consumption is more than 10 times the normal stoichiometric amount, and the acid-base waste liquid formed in these processes is very high at the end of the process. Difficult to handle; not only that, the sulfuric acid double salt precipitation method will produce SO which is very harmful to the human body in the process of iron recovery 2 and H 2 S gas

Method used

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  • Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation
  • Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation
  • Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] First, take 5g of NdFeB oil sludge, add 60ml of 4mol / L hydrochloric acid to the waste, and after fully dissolving, add excess hydrogen peroxide to the filtrate and stir for 10min. Then, adjust the pH values ​​to 4, 7, and 9 by adding ammonia water at a volume ratio of 1:1, and place the filtrate in a collector heating stirrer, control the reaction temperature at 70°C, and slowly add 1 mol / L of hydrogen Sodium oxide 30ml and let it react in the mixer for 60mins. Finally, after centrifuging and drying the precipitate, put it in a box furnace, and bake it at T=400°C for 90mins to obtain the mixed oxide of neodymium iron. Through XRD, XRF and other testing methods, we obtained the following results:

[0025] Compare the phase and element content of the Nd-Fe mixed oxide obtained by adding sodium hydroxide and roasting at the pH value of 4, 7, and 9, and analyze and discuss:

[0026]

[0027]

[0028] Table 1-1 XRF results of oxides obtained by roasting at different ...

Embodiment 2

[0031] First, take 5g of NdFeB oil sludge, add 60ml of 4mol / L hydrochloric acid to the waste, and after fully dissolving, add excess hydrogen peroxide to the filtrate and stir for 10min. Then, the filtrate was placed in a collector heating agitator, the reaction temperature was controlled at 70°C, 30% ammonia water was slowly added to adjust the pH value to 5.5, 7.5, and it was allowed to react in the agitator for 60mins. Finally, after centrifuging and drying the precipitate, put it in a box furnace, and bake it at T=400°C for 90mins to obtain the mixed oxide of neodymium iron. Through XRD, XRF and other testing methods, the following results were obtained:

[0032] Compare the phase and element content of the product obtained by adding ammonia water for precipitation and roasting when the pH value is 5.5 and 7.5, and analyze and discuss:

[0033]

[0034]

[0035] Table 1-2 XRF results of products roasted at different pH values ​​when ammonia water is used as precipit...

Embodiment 3

[0038]First, take 5g of NdFeB oil sludge, add 60ml of 4mol / L hydrochloric acid to the waste, and after fully dissolving, add excess hydrogen peroxide to the filtrate and stir for 10min. Then, the pH value was adjusted to be 2 by adding 1:1 ammonia water, and the filtrate was placed in a collector heating stirrer, and the reaction temperature was controlled to be 70°C, and 300ml of hot 0.1mol / L sodium oxalate solution was slowly added and allowed to It was reacted in the mixer for 60mins. Finally, after centrifuging and drying the precipitate, put it in a box furnace, and bake it at T=800°C for 90mins to obtain the mixed oxide of neodymium and iron. Through XRD, XRF and other testing methods, we obtained the following results:

[0039] Table 1-3 XRF results of Nd-Fe mixed oxide calcined with sodium oxalate as precipitant (%)

[0040]

[0041] Depend on image 3 It can be seen that the peak half-maximum width of the precipitate obtained by burning at 800°C is the smallest,...

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Abstract

The invention relates to a method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation, belonging to the field of recycling of neodymium iron boron oil sludge. The method comprises the following steps of: adding hydrogen peroxide to oxidize a pickling liquid of the neodymium iron boron oil sludge, adjusting the PH value, adding a proper amount of sodium hydroxide, ammonium hydroxide or sodium oxalate precipitating agent at one step, preserving the heat of 60-100 DEG C for a period of time, centrifuging a sediment, drying, and roasting at high temperature to obtain a mixture of the neodymium and iron oxides. The method is short in operation process, simple in operation and capable of avoiding using a great deal of reagents.

Description

technical field [0001] The invention relates to a method for preparing regenerated NdFeB sludge by one-step co-precipitation of NdFe alloy and NdFe oxide, which belongs to the recycling and utilization of NdFeB sludge. Background technique [0002] Today, one out of every six new technologies is related to rare earths, which fully demonstrates the role and status of rare earths in new technologies. Rare earth is an important strategic resource in the 21st century and the "monosodium glutamate" of modern industry. The reason why rare earth elements are called "strategic elements in the 21st century" is because they have special physical and chemical properties that other elements do not have. Many new rare earth materials made based on these characteristics have excellent performance and are widely used, and are widely used in electronic information, communication technology, automobile manufacturing, energy, aerospace and other fields. Rare earths have been hailed as "mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B3/06C22B3/44C22B59/00
CPCY02P10/20
Inventor 刘敏赖伟鸿索红莉李萌尹小文金琼花岳明刘卫强张东涛马麟王毅
Owner BEIJING UNIV OF TECH
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