CN109161934B - Method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals - Google Patents
Method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals Download PDFInfo
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- CN109161934B CN109161934B CN201811347884.2A CN201811347884A CN109161934B CN 109161934 B CN109161934 B CN 109161934B CN 201811347884 A CN201811347884 A CN 201811347884A CN 109161934 B CN109161934 B CN 109161934B
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Abstract
The invention relates to a method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals, which comprises the following steps: directly taking the cut neodymium iron boron alloy waste as an anode, selectively dissolving rare earth elements in the alloy by controlling the anode potential, and forming a perforated microstructure by controlling the anode current density so as to promote the rare earth elements in the alloy to be quickly dissolved into electrolyte; since only rare earth ions and lithium ions are present in the electrolyte, rare earth metals can be directly prepared by electrolysis. The method provided by the invention not only can effectively separate the rare earth elements from the neodymium iron boron alloy waste, but also can directly prepare the rare earth metals, and meanwhile, the anode reaction does not generate gas, thereby avoiding the pollution of the anode gas generated in the traditional process for producing the rare earth metals to the environment, and having good environmental benefit, social benefit and economic benefit.
Description
Technical Field
The invention relates to the technical field of neodymium iron boron waste recovery, in particular to a method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals.
Background
Since the invention of Nd-Fe-B magnetic material by Sagawa et al in 1983, Nd-Fe-B is still the magnetic material with the largest magnetic energy product, and thus has been widely used in many fields. At present, more than 150 million tons of neodymium iron boron magnetic materials are produced globally, wherein the yield of China exceeds 100 million tons, and the yield is still increased by about 10 percent every year. The service life of the common neodymium iron boron magnetic material is 6-8 years, and the service life of the high-performance neodymium iron boron is about 20 years. The scrap neodymium-iron-boron alloy waste contains about 30% of rare earth elements, mainly rare earth neodymium and praseodymium, and the high-performance neodymium-iron-boron material also contains a small amount of rare earth terbium and dysprosium. The recovery of the rare earth elements in the neodymium iron boron alloy waste can effectively reduce the dependence on rare earth primary resources, reduce urban mines formed by solid waste, and can generate remarkable social benefits and considerable economic benefits.
At present, the recovery process of rare earth elements in neodymium iron boron alloy waste materials mostly adopts the following production procedures: oxidizing roasting → acid dissolution → impurity removal → extraction separation → precipitation → ignition, and the rare earth products obtained are mostly rare earth oxides. The method has high rare earth recovery rate, but the flow is complex, and waste liquid containing acid or alkali can be generated, so that certain environmental problems exist. Meanwhile, the recovered product is rare earth oxide, while the rare earth product with the largest demand in the rare earth market at present is rare earth metal, so that secondary processing is needed to be carried out on the rare earth product.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for separating rare earth elements from neodymium iron boron alloy waste and directly preparing rare earth metals, the method not only can effectively separate the rare earth elements from the neodymium iron boron alloy waste, but also can directly prepare the rare earth metals, meanwhile, the anode reaction does not produce gas, the pollution of the anode gas generated in the traditional process for producing the rare earth metals to the environment is avoided, and the method has good environmental benefit, social benefit and economic benefit.
In order to achieve the purpose, the invention provides a method for separating rare earth elements from neodymium iron boron alloy waste and directly preparing rare earth metals, which directly uses the neodymium iron boron alloy waste as an anode, selectively oxidizes the rare earth elements in the neodymium iron boron alloy waste by controlling the anode potential, forms a perforated microstructure by controlling the anode current density, promotes the rare earth elements in the neodymium iron boron alloy waste to be quickly dissolved into electrolyte, and directly prepares the rare earth metals by electrolysis.
The method for separating the rare earth elements in the neodymium iron boron alloy waste and directly preparing the rare earth metals specifically comprises the following steps: placing the cut neodymium iron boron alloy waste into an anode basket, wherein the anode basket is connected with an anode of a direct current power supply through a molybdenum wire; dried LiF and NdF using tungsten wire as cathode and platinum wire as reference electrode3Electrolysis is performed as an electrolyte.
Preferably, the neodymium iron boron alloy scrap is a neodymium iron boron alloy scrap with a main metal phase.
Preferably, the neodymium iron boron alloy scrap after cutting is a block of 10mm x 10 mm.
Preferably, the anode basket is made of molybdenum wire.
Preferably, NdF3Are LiF and NdF30 to 80% of the mass sum.
Preferably, the temperature of electrolysis is 850-1100 ℃.
Preferably, the potential of the anode is between-2.00V and-0.29V relative to a platinum wire reference electrode.
Preferably, the current density of the anode is 0.22-0.61A/cm2。
Preferably, the distance between the electrodes is 27-33 mm.
Compared with the prior art, the method for treating the neodymium iron boron alloy waste has the following advantages:
(1) the method provided by the invention has short process flow, does not introduce impurity elements, and converts the rare earth elements in the neodymium iron boron alloy waste into rare earth metals in one step in the electrolytic furnace;
(2) the method provided by the invention does not introduce consumed chemical reagents and avoids generating new pollution. Meanwhile, the anode reaction does not generate gas, so that the environmental problem is avoided, and the method has good environmental benefit, social benefit and economic benefit;
(3) the product obtained by the method provided by the invention is rare earth metal, and can be directly applied without secondary processing of the product.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a graph of cyclic voltammetry for praseodymium and neodymium ions detected in LiF electrolyte in example 1 of the present invention;
FIG. 2 is an XRD spectrum of neodymium iron boron alloy waste before and after separation of rare earth elements in example 1 of the present invention;
FIG. 3 is an SEM photograph of the cross section of the neodymium-iron-boron alloy waste material after rare earth element separation in example 1 of the invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
The experimental procedures in the following examples are conventional unless otherwise specified. The test materials used in the following examples were purchased from a conventional store unless otherwise specified. In the quantitative tests in the following examples, three replicates were set, and the data are the mean or the mean ± standard deviation of the three replicates.
The invention provides a method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals, which comprises the following steps:
cutting the neodymium iron boron alloy waste into blocks of 10mm multiplied by 10mm, and placing the blocks into an anode basket made of molybdenum wires, wherein the anode basket is connected with the anode of a direct current power supply by the molybdenum wires;
a tungsten wire is used as a cathode and is connected with a cathode of a direct current power supply, and a platinum wire is used as a reference electrode;
mixing LiF and NdF3Vacuum drying at 400 deg.C for 24 hr, and mixing to obtain NdF powder3The mass fraction of (A) is 0-80%; placing the uniformly mixed fluoride in a boron nitride crucible, and then placing the boron nitride crucible in a vacuum electrolytic furnace; controlling the temperature to be 850-1100 ℃, and after the materials in the crucible are melted, electrifying direct current to carry out electrolysis; wherein the current density of the anode is controlled to be 0.22-0.61A/cm2And controlling the anode potential to be between-2.00V and-0.29V (relative to a Pt reference electrode), wherein the electrode distance is 27-33 mm.
As a result: after electrolysis for 1-4 hours, the separation efficiency of rare earth neodymium in the neodymium-iron-boron alloy waste is 91.6% -93.9%, and the separation efficiency of rare earth praseodymium is 98.3% -98.4%. Rare earth metals are collected near the cathode, wherein the mass fraction of neodymium is 44.8-89.1%, and the mass fraction of praseodymium is 10.1-10.9%.
The method for separating rare earth elements from neodymium iron boron alloy waste and directly preparing rare earth metals provided by the invention is further explained by combining specific embodiments.
Example 1
The embodiment provides a method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals, which comprises the following steps:
cutting the neodymium iron boron alloy waste into blocks of 10mm multiplied by 10mm, and placing the blocks into an anode basket made of molybdenum wires, wherein the anode basket is connected with the anode of a direct current power supply by the molybdenum wires; analyzing the mass fractions of the components in the neodymium iron boron alloy waste material by using an inductively coupled plasma emission spectrometer (ICP-AES) to obtain Nd27.1%, Pr8.1%, Fe63.7% and B1.1%;
a tungsten wire is used as a cathode and is connected with a cathode of a direct current power supply, and a platinum wire is used as a reference electrode;
drying LiF in vacuum at 400 ℃ for 24 hours, then placing the LiF in a boron nitride crucible, and then placing the LiF in a vacuum electrolytic furnace; controlling the temperature at 850 ℃, and electrifying direct current for electrolysis after materials in the crucible are melted; wherein the anode current density is controlled to be 0.22A/cm2The anode potential was controlled between-2.00V and-0.29V (relative to the Pt reference electrode) and the electrode distance was 27 mm.
As a result: after 1 hour of electrolysis, neodymium ions and praseodymium ions were detected in the electrolyte by an electrochemical workstation; fig. 1 is a graph of cyclic voltammograms of praseodymium and neodymium ions detected in a LiF electrolyte.
Carrying out X-ray diffraction (XRD) analysis on the neodymium iron boron alloy waste before and after the separation of the rare earth ions, and analyzing to obtain that the neodymium iron boron alloy waste cannot detect a rare earth phase after the separation of the rare earth elements; FIG. 2 is an XRD spectrum of neodymium iron boron alloy waste before and after rare earth element separation.
ICP-AES analysis is carried out on the separated anode product, the mass fractions of the components in the anode product are Nd3.4%, Pr0.2%, Fe94.8% and B1.6%, and the separation efficiency of neodymium is 91.6% and the separation efficiency of praseodymium is 98.3% through calculation.
The microstructure of the separated neodymium iron boron alloy waste is characterized by adopting a Scanning Electron Microscope (SEM), and the microstructure of the open pores formed by the neodymium iron boron alloy waste is proved; FIG. 3 is an SEM photograph of the cross section of the neodymium iron boron alloy waste material after rare earth element separation. No precipitate was collected at the cathode.
Example 2
The embodiment provides a method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals, which comprises the following steps:
cutting the neodymium iron boron alloy waste into blocks of 10mm multiplied by 10mm, and placing the blocks into an anode basket made of molybdenum wires, wherein the anode basket is connected with the anode of a direct current power supply by the molybdenum wires; analyzing the mass fractions of the components in the neodymium iron boron alloy waste material by using an inductively coupled plasma emission spectrometer (ICP-AES) to obtain Nd27.1%, Pr8.1%, Fe63.7% and B1.1%;
a tungsten wire is used as a cathode and is connected with a cathode of a direct current power supply, and a platinum wire is used as a reference electrode;
drying LiF in vacuum at 400 ℃ for 24 hours, then placing the LiF in a boron nitride crucible, and then placing the LiF in a vacuum electrolytic furnace; controlling the temperature at 1100 ℃, and after the materials in the crucible are melted, electrifying direct current to carry out electrolysis; wherein the anode current density is controlled to be 0.40A/cm2The anode potential was controlled between-2.00V and-0.29V (relative to the Pt reference electrode) and the electrode distance was 33 mm.
As a result: after 4 hours of electrolysis, neodymium ions and praseodymium ions were detected in the electrolyte by the electrochemical workstation.
XRD analysis is carried out on the neodymium iron boron waste materials before and after rare earth ion separation, and the analysis shows that the neodymium iron boron waste materials can not detect rare earth phase after rare earth element separation.
The separated anode product was subjected to ICP-AES analysis to obtain anode products in which the mass fractions of the components were nd2.7%, pr0.2%, fe95.4%, and B1.7%, and the separation efficiency of neodymium was 93.3% and the separation efficiency of praseodymium was 98.4% were calculated.
The microstructure of the separated neodymium iron boron alloy waste is characterized by adopting SEM, and the microstructure of open pores formed by the neodymium iron boron alloy waste is proved.
ICP-AES analysis was performed on the precipitates collected at the cathode, and the mass fractions of the respective elements in the cathode product were Li45.1%, Nd44.8%, and Pr10.1%.
Example 3
The embodiment provides a method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals, which comprises the following steps:
cutting the neodymium iron boron alloy waste into blocks of 10mm multiplied by 10mm, and placing the blocks into an anode basket made of molybdenum wires, wherein the anode basket is connected with the anode of a direct current power supply by the molybdenum wires; analyzing the mass fractions of the components in the neodymium iron boron alloy waste material by using an inductively coupled plasma emission spectrometer (ICP-AES) to obtain Nd27.1%, Pr8.1%, Fe63.7% and B1.1%;
a tungsten wire is used as a cathode and is connected with a cathode of a direct current power supply, and a platinum wire is used as a reference electrode;
mixing LiF and NdF3Vacuum drying at 400 deg.C for 24 hr, and mixing to obtain NdF powder3The mass fraction of (A) is 80%; uniformly mixing fluoride (LiF and NdF)3) Placing the mixture in a boron nitride crucible and then in a vacuum electrolytic furnace; controlling the temperature at 1050 ℃, and after the materials in the crucible are melted, electrifying direct current to carry out electrolysis; wherein the anode current density is controlled to be 0.61A/cm2The anode potential was controlled between-2.00V and-0.29V (relative to the Pt reference electrode) and the electrode distance was 29 mm.
As a result: after 2 hours of electrolysis, XRD analysis is carried out on the neodymium iron boron alloy waste materials before and after the separation of the rare earth ions, and the analysis shows that the neodymium iron boron alloy waste materials can not detect the rare earth phase after the separation of the rare earth elements.
The separated anode product was subjected to ICP-AES analysis to obtain anode products in which the mass fractions of the components were nd2.5%, pr0.2%, fe95.6%, and B1.7%, and the separation efficiency of neodymium was 93.9% and the separation efficiency of praseodymium was 98.4% were calculated.
The microstructure of the separated neodymium iron boron alloy waste is characterized by adopting SEM, and the microstructure of open pores formed by the neodymium iron boron alloy waste is proved.
ICP-AES analysis was performed on the precipitates collected at the cathode, and the mass fractions of the respective elements in the cathode product were Nd89.1% and Pr10.9%.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains. Unless specifically stated otherwise, the relative steps, numerical expressions, and values of the components and steps set forth in these embodiments do not limit the scope of the present invention. In all examples shown and described herein, unless otherwise specified, any particular value should be construed as merely illustrative, and not restrictive, and thus other examples of example embodiments may have different values.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention, and all of the technical solutions are covered in the protective scope of the present invention.
Claims (1)
1. A method for separating rare earth elements in neodymium iron boron alloy waste and directly preparing rare earth metals is characterized in that:
the method comprises the steps of directly taking neodymium iron boron alloy waste as an anode, selectively oxidizing rare earth elements in the neodymium iron boron alloy waste by controlling the anode potential, forming a perforated microstructure by controlling the anode current density, promoting the rare earth elements in the neodymium iron boron alloy waste to be rapidly dissolved into electrolyte, and directly preparing rare earth metals by electrolysis;
placing the cut neodymium iron boron alloy waste into an anode basket, wherein the anode basket is connected with an anode of a direct current power supply through a molybdenum wire; dried LiF and NdF using tungsten wire as cathode and platinum wire as reference electrode3Performing electrolysis as an electrolyte;
the neodymium iron boron alloy waste is a neodymium iron boron alloy waste with a metal phase as a main component;
the cut neodymium iron boron alloy waste is a block of 10mm multiplied by 10 mm;
the anode basket is prepared by molybdenum wires;
the NdF3Are LiF and NdF30-80% of the mass sum;
the temperature of the electrolysis is 850-1100 ℃;
the potential of the anode is between-2.00V and-0.29V relative to a platinum wire reference electrode;
the current density of the anode is 0.22-0.61A/cm2；
The distance between the electrodes is 27 to 33 mm.
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| CN110482563B (en) * | 2019-08-26 | 2020-04-24 | 山东大学 | Method for preparing crystalline boron powder |
| CN111154980B (en) * | 2020-02-04 | 2021-04-16 | 北京科技大学 | Neodymium iron boron waste solution electrolytic regeneration method |
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