CN108754163A - A method of the Extraction of rare earth metal from rare earth waste - Google Patents
A method of the Extraction of rare earth metal from rare earth waste Download PDFInfo
- Publication number
- CN108754163A CN108754163A CN201810859269.3A CN201810859269A CN108754163A CN 108754163 A CN108754163 A CN 108754163A CN 201810859269 A CN201810859269 A CN 201810859269A CN 108754163 A CN108754163 A CN 108754163A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- waste
- calcination
- earth metal
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/004—Dry processes separating two or more metals by melting out (liquation), i.e. heating above the temperature of the lower melting metal component(s); by fractional crystallisation (controlled freezing)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/003—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals by induction
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The method of the invention particularly discloses a kind of from rare earth waste Extraction of rare earth metal.Specifically technical characteristic is：Waste material containing praseodymium neodymium iron boron is put into crucible, it is different using the fusing point of praseodymium neodymium element, by under the action of electromagnetic induction, electric current, rare earth is set to start to melt, under the conditions of 1000-1100 DEG C, makes into molten liquid, add slag-cleaning agent at this time, high price ferrous components are made to form the slag charge of solidification and remove at above-mentioned equivalent temperature, and molten liquid, which is poured into mold, makes its solidification obtain praseodymium neodymium metal.
Description
Technical field
The invention belongs to rare earth field of deep, and in particular to a kind of side of the Extraction of rare earth metallic element from rare earth waste
Method.
Background technology
Rare earth has the title of industrial " gold " can be with other materials group since it is with physical characteristics such as excellent photoelectromagnetics
At different properties, new material various in style, most significant function is exactly to increase substantially the quality and property of other products
Can, reach the unrivaled quality of traditional material and performance, have been widely used in rare earth material, new energy materials, luminescent material,
The high-tech sectors such as catalysis material.Metallurgical industry, petrochemical industry, glass ceramics, the various fields such as permanent magnet micromotor, military enterprise
It is widely used.It is generated in rare earth new material prepares process since rare earth material is applied in the extensive of each field
The waste material that waste residue material and product are generated in long-time using failure, these waste material slags are the secondary money of valuable reclaiming
Source, rare earth waste and waste material secondary resource regeneration be also Rare-earth Industry sustainable development there is an urgent need to and inevitable choice,
Be conducive to the utilization of resources and environmental protection.
The recycling of country's rare earth waste at present, majority all concentrate on the discarded fluorescent lamp of processing or utilize rare earth waste
Produce rare earth oxide.But the either constituents extraction of rare earth waste or/and separation, method mostly use sulfuric acid, hydrochloric acid or
The acid solutions such as oxalic acid are precipitated with ammonia solution, are detached and obtained product as dissolving matchmaker again.In rare earth metallurgy technical field,
The molten referred to as wet method of acid that rare earth and other valuable metal element extractions are used.Also there is use in existing disclosed patented technology
Pyrogenic process-wet method combines recycling such as（CN 104388684A）.Chinese patent CN 102643992A are also specifically disclosed that a kind of " rare earth
The recovery method of waste material ", the technical scheme steps are：
(1) precipitation additive and fluxing agent powder are added into rare earth waste, mixture is obtained after mixing, wherein decomposing
The dosage of auxiliary agent is the 20-200wt% of rare earth waste total weight, and the dosage of fluxing agent is the 1- of rare earth waste total weight
20wt%；
(2) mixture for obtaining step (1) was in 600-1400 DEG C of roasting temperature 1-6 hours；
(3) to step (2) obtain in product of roasting be added acid solution carry out acid it is molten, transition it is isolated mainly containing rare earth member
The pickle liquor of element and acid leaching residue；
(4) rare earth element and other metallic elements in pickle liquor are detached.
In the prior art using acid as the double salt precipitation method of solvent, although to high-purity recycle rare earth achieve compared with
Good application effect, but the unpleasant penetrating odor with regard to being generated in production process, and a large amount of waste water for generating（In practical life
One ton of rare earth is often processed in production will produce 50-100m3Waste water）, crops and water resource to periphery cause serious dirt
Dye, it is careful or cause Health cost to resident.It finds more energy conservation and environmental protection and ecological environment is safeguarded to rare earth waste recovery method
There is an urgent need to.
Invention content
For deficiency in the prior art, a kind of method of the Extraction of rare earth metal from rare earth waste is provided, the present invention is not
With with use acid solution wet underwater welding in the prior art, also it is different with use ammonia solution as soaking the processing methods such as mine agent.This hair
Bright is the fusing point difference using each element in rare earth in temperature, excess material is added at a certain temperature, by different element extractions
Out, the pollution problem in rare earth waste removal process to environment is fundamentally solved.
In order to realize the present invention, the following technical solutions are specifically adopted：
A method of the Extraction of rare earth metal from rare earth waste, steps are as follows：
（1）Rare earth waste is placed in crucible, induction furnace is sent into；
（2）Induction furnace is opened and is heated, temperature is made to rise to 1000-1100 DEG C of calcination 10-15min；
（3）Crucible after above-mentioned heating calcination is taken out, Transition Materials are added, continue to be heated to 1000-1100 DEG C of calcination 10-
15min makes material all melt；
（4）Slag-cleaning agent is added into the material after above-mentioned dissolve, continues under the conditions of 1000-1100 DEG C after calcination 10-15min,
Stop heating；
（5）Material after above-mentioned heated calcination is taken out, the slag charge of solidification is removed；
（6）The molten liquid after solidifying slag charge will be removed to pour into after mold solidification up to rare earth metal.
Above-mentioned steps（1）The rare earth waste be neodymium iron boron leftover bits and pieces, neodymium iron boron polished material, one kind in grinding wheel material or
It is a variety of.
Above-mentioned steps（3）Described in transition material be content 95.5%（W/W）Rare earth metal.
Further, the addition of the transition material is 4 by rare earth waste and the weight ratio of transition material:1 ratio is matched
Than.
Above-mentioned steps（4）The slag-cleaning agent is the arbitrary proportioning of one or both of sodium metasilicate, potassium silicate.
Further, the addition of the slag-cleaning agent is the 0.25%-0.5% of rare earth waste weight.
The present invention program be using rare earth metal fusing point and boron therein, iron temperature melting point difference, in a constant temperature
Under the conditions of degree, transition material is added, using different fusing points, can step by step extract different element sepatations, it is of the invention
Main purpose is based on Extraction of rare earth metal praseodymium neodymium, and therefore, the transition material used is praseodymium neodymium metal, technical process
It is then that the waste material containing praseodymium neodymium iron boron is put into crucible, it is different using the fusing point of praseodymium neodymium element, by electromagnetic induction, electric current
Under the action of, make rare earth start to melt, under the conditions of 1000-1100 DEG C, makes into molten liquid, add slag-cleaning agent at this time, upper
It states the slag charge for making high price ferrous components form solidification at equivalent temperature and removes, and molten liquid, which is poured into mold, makes its solidification obtain
Obtain praseodymium neodymium metal.
Beneficial effects of the present invention
（1）The method of the present invention is fundamentally solved does not use acid solution leach extraction method to the processing and utilization of the rare earth waste of recycling,
Process does not generate waste liquid and exhaust gas, avoids environmental pollution caused by conventional method.Present invention process flow is short, saving of labor saves
When, cost effective consumes energy low.
（2）The method of the present invention is the different melting points using thulium, makes dystectic iron and the praseodymium neodymium of low melting point
It can be efficiently separated, and gained praseodymium neodymium metal element content is high, by product using icp analysis instrument according to conventional point
Analysis method is analyzed, and praseodymium neodymium tenor reaches 99%, meets the requirement of production rare-earth metal material.
（3）Mainly the praseodymium neodymium metallic element in rare earth waste is extracted in present invention process, the melting temperature of rare earth
At 900-1000 DEG C, degree starts to melt degree, and when reaching 1100 degree of temperature, melting terminates, however, iron rule is in 1200 DEG C of temperature
Start to melt, and melting terminates in 1500 DEG C of temperature, for further to the recycling of ferro element then not the present invention's
Range is only handled as the slag charge in present invention process.Therefore, the substantive distinguishing features in present invention process are then to rare earth waste
The temperature of processing control effectively, and temperature control is made to reach whole meltings of praseodymium neodymium element at 1000-1100 DEG C, and obtains dilute
Native praseodymium neodymium metal material, and ferro element then remains in its slag charge, this method is higher to gained praseodymium neodymium tenor, miscellaneous
Matter is less.The present invention realizes the utilization of the high efficiente callback to rare earth waste.
（4）The method of the present invention can realize the low consumption to rare earth secondary resource, pollution-free recycling, and can form scale
Recycling, process conditions are simple and practicable, and processing cost is low, have considerable economic and social benefit, while more having apparent environment
Protect benefit.
Specific implementation mode
Embodiment 1
（1）Neodymium iron boron leftover bits and pieces 400g is taken, is placed in crucible, induction furnace is sent into；
（2）Induction furnace is opened and is heated, temperature is made to rise to 1100 DEG C of calcination 10min；
（3）Crucible after above-mentioned heating calcination is taken out, it is 99.5% that content, which is added,（W/W）Rare earth metal excess material 100g,
It continues to be fed into induction furnace and is heated to 1100 DEG C of calcination 10min, material is made all to melt；
（4）1.6g sodium metasilicate slag-cleaning agents are added into the material after above-mentioned melting, continue under the conditions of 1100 DEG C, calcination 10min
Afterwards, stop heating；
（5）Material after above-mentioned heated calcination is taken out, the slag charge of solidification is removed；
（6）Will remove solidification slag charge after molten liquid pour into mold make its solidification to get rare earth metal.It is analyzed through icp analysis instrument,
Praseodymium neodymium tenor is 99.54%.
Embodiment 2
（1）Neodymium iron boron polished material and grinding wheel material 400g are taken, is placed in crucible, induction furnace is sent into；
（2）Induction furnace is opened and is heated, temperature is made to rise to 1000 DEG C of calcination 15min；
（3）Crucible after above-mentioned heating calcination is taken out, it is 99.5% that content, which is added,（W/W）Rare earth metal excess material 100g,
It continues to be fed into induction furnace and is heated to 1000 DEG C of calcination 15min, material is made all to melt；
（4）1.2g sodium metasilicate slag-cleaning agents are added into the material after above-mentioned melting, continue under the conditions of 1000 DEG C, calcination 15min
Afterwards, stop heating；
（5）Material after above-mentioned heated calcination is taken out, the slag charge of solidification is removed；
（6）Will remove solidification slag charge after molten liquid pour into mold make its solidification to get rare earth metal.It is analyzed through icp analysis instrument,
Praseodymium neodymium tenor is 99.62%.
Embodiment 3
（1）Neodymium iron boron leftover bits and pieces 400g is taken, is placed in crucible, induction furnace is sent into；
（2）Induction furnace is opened and is heated, temperature is made to rise to 1000 DEG C of calcination 15min；
（3）Crucible after above-mentioned heating calcination is taken out, it is 99.5% that content, which is added,（W/W）Rare earth metal excess material 100g,
It continues to be fed into induction furnace and is heated to 1000 DEG C of calcination 15min, material is made all to melt；
（4）2g potassium silicate slag-cleaning agents are added into the material after above-mentioned melting, continue under the conditions of 1050 DEG C, after calcination 13min,
Stop heating；
（5）Material after above-mentioned heated calcination is taken out, solidification slag charge is removed；
（6）Will remove solidification slag charge after molten liquid pour into mold make its solidification to get rare earth metal.It is analyzed through icp analysis instrument,
Praseodymium neodymium tenor is 99.57%.
Claims (3)
1. a kind of method of the Extraction of rare earth metal from rare earth waste, which is characterized in that steps are as follows：
（1）Rare earth waste is placed in crucible, induction furnace is sent into；
（2）Induction furnace is opened and is heated, temperature is made to rise to 1000-1100 DEG C of calcination 10-15min；
（3）Crucible after above-mentioned heating calcination is taken out, Transition Materials are added, continue to be heated to 1000-1100 DEG C of calcination 10-
15min makes material all melt；
（4）Slag-cleaning agent is added into the material after above-mentioned dissolve, continues under the conditions of 1000-1100 DEG C after calcination 10-15min,
Stop heating；
（5）Material after above-mentioned heated calcination is taken out, the slag charge of solidification is removed；
（6）The molten liquid after solidifying slag charge will be removed to pour into after mold solidification up to rare earth metal；The rare earth waste is neodymium
Iron boron leftover bits and pieces, it is one or more in neodymium iron boron polished material, grinding wheel material；The transition material is the dilute of content 95.5%W/W
Earth metal；The slag-cleaning agent is the arbitrary proportioning of one or both of sodium metasilicate, potassium silicate.
2. the method for the Extraction of rare earth metal according to claim 1 from rare earth waste, which is characterized in that the transition
The addition of material is 4 by rare earth waste and the weight ratio of transition material:1 proportions.
3. the method for the Extraction of rare earth metal according to claim 1 from rare earth waste, which is characterized in that the scarfing cinder
The addition of agent is the 0.25%~0.5% of rare earth waste weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810859269.3A CN108754163A (en) | 2018-07-31 | 2018-07-31 | A method of the Extraction of rare earth metal from rare earth waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810859269.3A CN108754163A (en) | 2018-07-31 | 2018-07-31 | A method of the Extraction of rare earth metal from rare earth waste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108754163A true CN108754163A (en) | 2018-11-06 |
Family
ID=63968449
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810859269.3A Pending CN108754163A (en) | 2018-07-31 | 2018-07-31 | A method of the Extraction of rare earth metal from rare earth waste |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108754163A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111876795A (en) * | 2020-07-28 | 2020-11-03 | 江苏金石稀土有限公司 | Method for recovering electrolyte in rare earth molten salt slag |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335925A (en) * | 1998-12-25 | 2002-02-13 | 昭和电工株式会社 | Method and device for melting rare earth magnet scrap and primary molten alloy of rare earth magnet |
| CN102534236A (en) * | 2012-02-20 | 2012-07-04 | 武汉科技大学 | Method for recovering valuable metal from metallurgical slag materials |
-
2018
- 2018-07-31 CN CN201810859269.3A patent/CN108754163A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335925A (en) * | 1998-12-25 | 2002-02-13 | 昭和电工株式会社 | Method and device for melting rare earth magnet scrap and primary molten alloy of rare earth magnet |
| CN102534236A (en) * | 2012-02-20 | 2012-07-04 | 武汉科技大学 | Method for recovering valuable metal from metallurgical slag materials |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111876795A (en) * | 2020-07-28 | 2020-11-03 | 江苏金石稀土有限公司 | Method for recovering electrolyte in rare earth molten salt slag |
| CN111876795B (en) * | 2020-07-28 | 2022-12-06 | 江苏金石稀土有限公司 | Method for recovering electrolyte in rare earth molten salt slag |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108658483B (en) | Method for preparing auxiliary cementing material by reducing and recycling iron and secondary slag through steel slag | |
| CN103540756A (en) | Method for dissolving out rare-earth by treating waste neodymium-iron-boron materials | |
| CN104190943A (en) | Method for recycling sintered neodymium-iron-boron waste materials | |
| CN106498169B (en) | A kind of neodymium iron boron waste material recovery process | |
| CN103924088A (en) | Method for recovering and treating waste batteries or materials containing Co and/or Ni | |
| CN105567985A (en) | Recovery method of rare earth metal electrolysis fused salt slag | |
| WO2020151478A1 (en) | Method for recovering rare earth element from neodymium-iron-boron scrap by means of extraction with liquid metal bismuth | |
| CN102534271A (en) | Production method of vanadium-aluminum alloy | |
| CN103993182B (en) | The comprehensive recovering process of secondary resource in a kind of iron vitriol slag | |
| CN103849775A (en) | Method for recycling nickel and cobalt from high temperature alloyed scrap | |
| CN103146925B (en) | Method of recycling rear earth from neodymium iron boron waste | |
| CN105568007A (en) | Method for recovering rare earth from waste rare earth phosphor | |
| CN104388711A (en) | Method for recovering rare earth by leaching rare earth oxide molten slag | |
| CN103484683A (en) | Comprehensive utilization method of molten titanium-bearing blast furnace slag | |
| CN105132698A (en) | Technology for extracting aluminum and zinc from high-aluminum zinciferous aluminum-zinc residues | |
| CN108754163A (en) | A method of the Extraction of rare earth metal from rare earth waste | |
| CN103123840B (en) | A kind of permanent magnetic material with high compressive strength and preparation method thereof | |
| CN111440953B (en) | Method for synergistically recycling tungsten slag and multi-element iron-rich slag | |
| CN101875494B (en) | Preparation method of low-titanium and high-purity polycrystalline silicon | |
| CN103667751B (en) | Ndfeb magnet waste material is adopted to prepare the method for magnesium neodymium master alloy | |
| CN109136996B (en) | Method for preparing Mg-Nd base intermediate alloy by using neodymium iron boron waste | |
| CN108977674A (en) | A method of the Extraction of rare earth oxide from Rare Earth Electrolysis waste material | |
| CN104046787A (en) | Comprehensive utilization method of cyanidation tailings | |
| CN109517996B (en) | Process for extracting iron in sulfuric acid cinder by aid of enhanced acid leaching method | |
| CN105671311A (en) | Processing method of iron ore |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181106 |
|
| WD01 | Invention patent application deemed withdrawn after publication |