RO115996B1 - PROCESS FOR RECOVERING WASTE NdFeB MAGNETIC ALLOY - Google Patents

PROCESS FOR RECOVERING WASTE NdFeB MAGNETIC ALLOY Download PDF

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Publication number
RO115996B1
RO115996B1 RO9800578A RO9800578A RO115996B1 RO 115996 B1 RO115996 B1 RO 115996B1 RO 9800578 A RO9800578 A RO 9800578A RO 9800578 A RO9800578 A RO 9800578A RO 115996 B1 RO115996 B1 RO 115996B1
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RO
Romania
Prior art keywords
solution
magnetic alloy
ndfeb magnetic
recovering waste
magnetic
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RO9800578A
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Romanian (ro)
Inventor
Wilhelm Kappel
Stefania Alexandru
Mirela Maria Codescu
Ion Ivan
Nicolae Stancu
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S C Icpe Sa
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Priority to RO9800578A priority Critical patent/RO115996B1/en
Publication of RO115996B1 publication Critical patent/RO115996B1/en

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  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention relates to a process for recovering waste NdFeB magnetic alloy accomplished by means of the following succession of phases: selection according to the criterion of the chemical composition; etching with a solution of 10% acetic acid or a mixture of 10% citric and oxalic acid solutions in a ratio of 1:1 and afterwards with a solution of 10% NaOH or Na2CO3, flushing with warm water jet after each operation; tight hydrogenation at 1...5 bars and 100...150 °C for brittleness; crushing up to a granulation of 3...6 micrometers. The process allows a complete recovery of the magnetic waste resulting from cutting operations.

Description

Invenția se referă la un procedeu de recuperare de aliaje magnetice NdFeB.The invention relates to a process for recovering NdFeB magnetic alloys.

Este cunoscut un procedeu chimic de recuperare a neodymului din deșeuri magnetice tip NdFeB, prin tratare cu acid acetic și acid fluorhidric și electroliză cu acid sulfuric și uscarea cu microunde a fluorurii de Nd obținută [ US 5362459],A chemical process for the recovery of neodymium from NdFeB type magnetic waste is known, by treatment with acetic acid and hydrofluoric acid and electrolysis with sulfuric acid and microwave drying of the obtained Nd fluoride [US 5362459],

Procedeul prezintă dezavantajul că nu permite o recuperare completă a componentelor materialului magnetic.The process has the disadvantage that it does not allow a complete recovery of the magnetic material components.

Problema care apare este de a realiza o recuperare avansată a componenților materialului magnetic NdFeB, printr-un procedeu economic și nepoluant.The problem that arises is to realize an advanced recovery of the components of the magnetic material NdFeB, through an economic and non-polluting process.

Procedeul de recuperare a deșeurilor de aliaje magnetice NdFeB, conform invenției, rezolvă această problemă, prin aceea că, în scopul recuperării deșeurilor de aliaje magnetice NdFeB, acestea sunt sortate după criteriul compoziției chimice, după care se decapează, în scopul îndepărtării oxizilor prin tratare cu soluție 10% de acid acetic sau amestec 1:1 soluții 10% de acid citric și oxalic și apoi soluție de 10% de NaOH sau Na2C03, după fiecare operație făcându-se spălare în jet de apă caldă, materialul astfel pregătit supunându-se hidrogenării, într-o incintă etanșă, la o presiune de 1...5 bar și la o temperatură de 1OO...15O°C, pentru a deveni friabil, în scopul ușurării operației de măcinare în moara cu bile, până la obținerea unei granulații de 3 ...6pm, care să permită procesarea pulberii după metode cunoscute.The process of recovering NdFeB magnetic alloy waste, according to the invention, solves this problem, in that, for the purpose of recovering NdFeB magnetic alloy waste, they are sorted according to the chemical composition criterion, after which they are pickled, in order to remove the oxides by treatment with 10% acetic acid solution or 1: 1 solution 10% citric and oxalic acid solution and then 10% NaOH or Na 2 C0 3 solution , after each operation being washed in hot water jet, the material thus prepared submitting -is hydrogenated, in a sealed enclosure, at a pressure of 1 ... 5 bar and at a temperature of 1OO ... 15 ° C, to become friable, in order to facilitate the milling operation in the ball mill, up to when obtaining a granulation of 3 ... 6pm, which allows the processing of the powder according to known methods.

Procedeul, conform invenției, oferă următoarele avantaje:The process according to the invention offers the following advantages:

- permite recuperarea integrală a deșeurilor de aliaje magnetice NdFeB, rezultate din operații de debitare;- allows full recovery of NdFeB magnetic alloy waste, resulting from cutting operations;

- permite obținerea unei granulații de 3...6pm, optimă pentru procesarea ulterioară a pulberii;- allows to obtain a granulation of 3 ... 6pm, optimal for the subsequent processing of the powder;

- carcteristicile magnetice obținute sunt reproductibile și conforme cu compoziția chimică;- the magnetic characteristics obtained are reproducible and conform to the chemical composition;

- nu necesită dotări tehnice costisitoare.- does not require expensive technical equipment.

Invenția este prezentată, în continuare, prin două exemple de aplicare, în legătură și cu fig. 1 și 2, care reprezintă caracteristicile magnetice ale magneților realizați cu materialul recuperat conform celor două exemple.The invention is further illustrated by two embodiments, in connection with FIG. 1 and 2, which represent the magnetic characteristics of the magnets made with the recovered material according to the two examples.

Exemplul 1. Conform invenției, deșeurile de aliaje magnetice NdFeB, cu sau fără adaosuri de Dy, Al, V, se supun operației de decapare prin tratare cu soluție 10% de acid acetic sau cu amestec 1:1 soluții 10% de acid citric și oxalic și apoi cu o soluție de 10% de NaOH sau Na2C03, după fiecare operație făcându-se spălare în jet de apă caldă, care are ca scop atât îndepărtarea produșilor de reacție, cât și a soluțiilor de decapare.Example 1. According to the invention, waste NdFeB magnetic alloys, with or without additions of Dy, Al, V, are subjected to pickling by treatment with 10% acetic acid solution or with 1: 1 10% citric acid solution and oxalic and then with a solution of 10% NaOH or Na 2 C0 3 , after each operation washing in hot water, which aims at both the removal of the reaction products and the pickling solutions.

Deșeurile decapate sunt apoi încărcate într-o incintă etanșă, în care se introduce hidrogen, la o presiune de 1...5 bar, după ce anterior s-a efectuat o vidare la o presiune de 2-1D2 1O2 bar.The pickled waste is then loaded into a sealed enclosure, in which hydrogen is introduced, at a pressure of 1 ... 5 bar, after previously a vacuum was carried out at a pressure of 2-1D 2 1O 2 bar.

Prin adsorbție de hidrogen, deșeurile de aliaje magnetice sinterizate devin friabile și pot fi foarte ușor măcinate într-o moară cu bile, pentru a se ajunge la o granulație de 3...6pm, care să permită recuperarea materialului, prin procesarea ulterioară a pulberii obținute.By hydrogen adsorption, the sintered magnetic alloy waste becomes brittle and can be easily ground in a ball mill, to reach a granulation of 3 ... 6pm, which will allow the material to be recovered, by further processing the powder. obtained.

Caracteristicile magnetice obținute pe un magnet realizat pe această cale sunt cele date în fig. 1.The magnetic characteristics obtained on a magnet made in this way are those given in fig. 1.

Exemplul 2. Pentru recuperarea deșeurilor de aliaje magnetice NdFeB, cu adaosuri de Co, acestea, după decapare și încărcare în incinta etanșă de hidrogenare, se încălzesc în atmosferă de hidrogen, la o presiune de 1...2 bar, la temperaturi cuprinse în intervalul 1OO...15O°C, pentru amorsarea reacției de adsorbție a hidrogenului.Example 2. For the recovery of waste NdFeB magnetic alloys, with Co additions, these, after pickling and loading in the hydrogenation enclosure, are heated in a hydrogen atmosphere, at a pressure of 1 ... 2 bar, at temperatures in in the range 1OO ... 15 ° C, for initiating the hydrogen adsorption reaction.

RO 115996 BlRO 115996 Bl

Materialul hidrogenat urmează etapele tehnologice obișnuite pentru procesarea 5 o aliajelor magnetice NdFeB.The hydrogenated material follows the usual technological steps for processing 5 NdFeB magnetic alloys.

Caracteristicile magnetice obținute sunt date în fig. 2.The magnetic characteristics obtained are given in fig. 2.

Claims (1)

RevendicareClaim Procedeu de recuperare a deșeurilor de aliaje magnetice Nd FeB, caracterizat prin aceea că este realizat prin succesiunea fazică: sortare după criteriul compoziției chimice; decapare cu soluție 10% acid acetic sau amestec 1:1 de soluții 10% acid citric și oxialic și apoi cu soluție 10% de NaOH sau NaaC03, cu spălare cu jet de apă caldă după fiecare operație; hidrogenare etanșă la 1 ...5 bar și 1OO...15O°C, pentru 60 friabilizare; măcinare până la 3...6pm granulație.Nd FeB magnetic alloy waste recovery process, characterized by the fact that it is achieved by phase succession: sorting according to the chemical composition criterion; pickling with 10% acetic acid solution or 1: 1 solution of 10% citric and oxialic acid solutions and then with 10% NaOH or Na solution of C0 3 , with hot water wash after each operation; sealed hydrogenation at 1 ... 5 bar and 1OO ... 15 ° C, for 60 friability; grinding until 3 ... 6pm granulation.
RO9800578A 1998-02-27 1998-02-27 PROCESS FOR RECOVERING WASTE NdFeB MAGNETIC ALLOY RO115996B1 (en)

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RO9800578A RO115996B1 (en) 1998-02-27 1998-02-27 PROCESS FOR RECOVERING WASTE NdFeB MAGNETIC ALLOY

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RO115996B1 true RO115996B1 (en) 2000-08-30

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103934450A (en) * 2014-03-26 2014-07-23 辽宁五寰科技发展有限公司 Method for reusing sintered reclaimed NdFeB material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103934450A (en) * 2014-03-26 2014-07-23 辽宁五寰科技发展有限公司 Method for reusing sintered reclaimed NdFeB material

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