CN103343234A - Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation - Google Patents
Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation Download PDFInfo
- Publication number
- CN103343234A CN103343234A CN2013103066576A CN201310306657A CN103343234A CN 103343234 A CN103343234 A CN 103343234A CN 2013103066576 A CN2013103066576 A CN 2013103066576A CN 201310306657 A CN201310306657 A CN 201310306657A CN 103343234 A CN103343234 A CN 103343234A
- Authority
- CN
- China
- Prior art keywords
- precipitation
- neodymium
- iron boron
- neodymium iron
- greasy filth
- 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.)
- Granted
Links
Images
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Removal Of Specific Substances (AREA)
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
The present invention relates to the method that a kind of neodymium iron boron greasy filth prepares one step of regeneration neodymium iron boron co-precipitation neodymium-iron alloy and prepares the neodymium ferriferous oxide, belong to the recycling of neodymium iron boron greasy filth.
Background technology
Nowadays, just have in per 6 new technologies one relevant with rare earth, this proves absolutely effect and the status of rare earth in new technology.Rare earth is 21 century important strategic resource, is " monosodium glutamate " of modern industry.Why rare earth element is called as " 21 century strategy element ", is because it has other elements and does not possess specific physical character and chemical property.Based on many rare earth new materials that these characteristics are made, excellent performance, of many uses, be used for fields such as electronic information, mechanics of communication, automobile making, the energy and aerospace in a large number.Rare earth was described as " material VITAMIN " and " 21 century high-tech and the treasure-house of functional materials " etc. once.
Rare earth element is as rare and expensive grand strategy resource, and the valuable element that comprehensively reclaims in the waste material is very valuable work; Rationally reclaim rare earth element, can not only save and protect national resource, reduce cost and increase economic efficiency, be conducive to domestic each field and develop steadily in the long term, also help the cycling and reutilization of rare earth element and the Sustainable development of country.
And as the neodymium iron boron that is rich in the rare earth element didymium, neodymium iron boron reclaiming work is seemed very important naturally.The iron boron magnet magnetic energy product is 240～440kJ/m
3, be known as the present age " king of permanent magnetism ", be the present known the highest permanent magnet material of over-all properties.Compare with traditional magnet, the magnetic energy product of rare earth permanent-magnetic material will exceed 4～10 times, and other magnetic properties also far exceed conventional magnet; And the magnetic energy product of Nd-Fe-Bo permanent magnet material more will exceed 8～10 times of traditional magnetic material.
The technical process of NdFeB waste recovery has multiple, as the molten depositing technology of acid, double salt conversion process, the excellent molten technology of hydrochloric acid etc.Following some traditional recovery methods of listing:
Comprehensive above present rare earth recovery method, though these technologies can regain rare earth, but also there are problems: at first finally, the endless chain of above technology and formation useless circulation truly, the product that these technologies obtain only is rare earth oxide, and does not make the mechanicals that can directly use.And the rare-earth oxidation material desire purify for industrial can direct applied high-purity single rare earth, also need carry out tens grades of extraction process, its extraction agent is very expensive especially, social benefit obviously reduces.Secondly on economic benefit, except above-mentioned when the purification high-purity single rare earth, extraction process will consume beyond the extraction agent of a large amount of acid solutions, time and costliness, the common sour molten precipitator method will be carried out secondary sedimentation to rare earth when reclaiming rare earth, not only flow process is longer for it, invest higherly, and the rate of recovery is lower, and economic benefit is obviously very low; And extract in the technology of rare earth at full extraction process, though the purity of this technology rare earth when reclaiming rare earth is higher, and can obtain the cobalt element of higher degree, but its numerous and diverse chemical technology and high cost make this method can't accepted by industrial production at the very start.Again, from the angle of energy-conserving and environment-protective, no matter be the excellent molten method of hydrochloric acid, full extraction process or the sulfuric acid double salt precipitator method, they all can form a large amount of acid-base waste fluids and toxic and harmful in rare earth reclaims.Only in extraction process, because need higher liquid liquor ratio and better back extraction effect, its sour consumption all is normal stoichiometric more than 10 times, and the acid-base waste fluid that these processes form is in technology end intractable all; Moreover, the sulfuric acid double salt precipitator method will produce the SO very big to the human injury in the process that reclaims iron
2And H
2S gas.
Summary of the invention
The present invention is directed to above-mentioned these problems, adopt the coprecipitation of single stage method neodymium iron to replace valuable element in the molten back of the method recovered acid solution of selective precipitation neodymium only.This method reclaims neodymium iron simultaneously, and technical process is short, not the wasting of valuable element, and follow-uply can be used to synthetic NdFeB magnetic powder, realizes real recycle, so this method has the economic and practical of getting well.
A kind of method of neodymium iron boron greasy filth regeneration prepared by co-precipitation neodymium ferriferous oxide, it is characterized in that may further comprise the steps: after hydrogen peroxide oxidation is added in the pickling liquor of neodymium iron boron greasy filth, after regulating pH value, once add proper amount of sodium hydroxide, ammoniacal liquor or sodium oxalate precipitation agent, after insulation for some time under 60～100 ℃ of temperature, to precipitate centrifugal oven dry, and roasting at high temperature, the mixture of acquisition neodymium ferriferous oxide.
The technical scheme that the present invention formulates further preferably includes following steps:
When (1) being the precipitation agent of a step co-precipitation with sodium hydroxide, the top condition of its co-precipitation is: after the molten filtration of neodymium iron boron greasy filth acid, filtrate is added excessive mass concentration 30% hydrogen peroxide oxidation and is not stopped to stir; For preventing that ferric hydroxide colloid from generating, selecting to regulate pH value earlier is incubated again, therefore, regulate the preferred PH=7 of PH=4～9(～9 earlier), controlling temperature of reaction then is 60～100 ℃, and the sodium hydroxide solution that adds 1mol/L reacts 60mins under agitation condition, last, to precipitate centrifugal oven dry and be placed in the box-type furnace, ℃ following roasting 90mins in T=400～600; The consumption of preferred sodium hydroxide solution is the corresponding 30ml sodium hydroxide solution of every 5g neodymium iron boron greasy filth.
When (2) being the precipitation agent of a step co-precipitation with ammoniacal liquor, the top condition of its co-precipitation is: after the molten filtration of neodymium iron boron greasy filth acid, filtrate is added excessive mass concentration 30% hydrogen peroxide oxidation and is not stopped to stir, add 30% ammoniacal liquor until regulating the post precipitation solution PH=preferred PH=5.5 of 8～10(～7.5), controlling temperature of reaction then is 60～100 ℃, and standing and reacting 60mins is last, to precipitate centrifugal and dry and be placed in the box-type furnace ℃ following roasting 90mins in T=400～600.
When (3) being the precipitation agent of a step co-precipitation with sodium oxalate, the top condition of its co-precipitation is: after the molten filtration of neodymium iron boron greasy filth acid, filtrate is added excessive mass concentration 30% hydrogen peroxide oxidation and is not stopped to stir, and generates for preventing ferric hydroxide colloid, selects to regulate pH value earlier and is incubated.Therefore, regulate earlier PH=1～3, controlling temperature of reaction again is 60～100 ℃, and add temperature be 35-50 ℃ heat the 0.1mol/L sodium oxalate solution and be allowed to condition at and stir reaction 60mins down.At last, will precipitate centrifugal oven dry and be placed in the box-type furnace, ℃ following roasting 90mins in T=600～800, the corresponding 300ml sodium oxalate solution of preferred every 5g neodymium iron boron greasy filth.
Solid-to-liquid ratio is (1g) in the molten process of neodymium iron boron greasy filth described above acid: (10-15ml).
The mass content of iron neodymium is respectively in the products therefrom of the present invention: 47.89%～63.44%, 18.10%～34.51%, and basic consistent with the mass ratio of iron neodymium in the starting material.
The invention has the beneficial effects as follows:
(1) can one the step with the co-precipitation of neodymium iron, operating process is short, and is simple to operate, avoided the use of extensive reagent;
(2) inquired into sodium hydroxide, ammoniacal liquor, sodium oxalate three kinds of precipitation agents in the effect of single stage method co-precipitation iron neodymium, wherein the co-precipitation effect of sodium oxalate is better, and at the bottom of the foreign matter content, powder particle is even;
(3) for subsequent preparation neodymium iron boron regeneration magnetic provides favourable condition, realize the industry endless chain, for " mine, city " lays a good foundation.
Description of drawings
The XRD figure of the neodymium ferriferous oxide that Fig. 1 obtains under different pH values when being precipitation agent for embodiment 1 with NaOH is composed;
The XRD figure of the neodymium ferriferous oxide that Fig. 2 obtains under different pH values when being precipitation agent for embodiment 2 with ammoniacal liquor is composed;
Fig. 3 is the XRD figure spectrum of the neodymium ferriferous oxide that obtains of precipitation agent with the sodium oxalate for embodiment 3.
Embodiment
Below in conjunction with example the present invention is further specified, but the present invention is not limited to following examples.Following hydrogen peroxide is mass concentration 30% hydrogen peroxide.
Embodiment 1:
At first, get 5g neodymium iron boron greasy filth, add 4mol/L hydrochloric acid 60ml in the waste material, fully the dissolving back is added excessive hydrogen peroxide in the filtrate and is stirred 10min.Then, be that the ammoniacal liquor of 1:1 is regulated pH value and is respectively 4,7,9 by adding volume ratio, and filtrate placed the heat collecting type heating stirrer that the control temperature of reaction is 70 ℃, slowly adds the sodium hydroxide 30ml of 1mol/L and is allowed to condition at and react 60mins in the agitator.At last, will precipitate centrifugal oven dry and be placed in the box-type furnace, at T=400 ℃ of following roasting 90mins, namely get the neodymium Iron mixed oxide.By means of testing such as XRD, XRF, we obtain following result:
Relatively thing phase, the constituent content of the neodymium Iron mixed oxide that roasting obtains after pH value is to add sodium hydroxide at 4,7,9 o'clock, and analyze discussion:
The XRF result (%) of the oxide compound that the roasting that table 1-1 obtains under different pH values when being precipitation agent with NaOH obtains
By above result contrast, think in PH7～9 o'clock, be that the pH value of more satisfactory step precipitator method is chosen scope, its foreign matter content and kind are all lower, and the conversion by yield, and its rate of recovery is also higher.
Embodiment 2
At first, get 5g neodymium iron boron greasy filth, add 4mol/L hydrochloric acid 60ml in the waste material, fully the dissolving back is added excessive hydrogen peroxide in the filtrate and is stirred 10min.Then, and filtrate placed the heat collecting type heating stirrer, the control temperature of reaction is 70 ℃, and slowly adding the pH value that 30% ammoniacal liquor regulates is 5.5,7.5, and is allowed to condition at and reacts 60mins in the agitator.At last, will precipitate centrifugal oven dry and be placed in the box-type furnace, at T=400 ℃ of following roasting 90mins, namely get the neodymium Iron mixed oxide.By means of testing such as XRD, XRF, obtain following result:
Be that roasting obtains thing phase, the constituent content of product after adding ammonia precipitation process at 5.5,7.5 o'clock in pH value relatively, and analyze discussion:
Table 1-2 when being precipitation agent with ammoniacal liquor under different pH values roasting obtain the XRF result (%) of product
As seen from Figure 2, when using ammoniacal liquor as precipitation agent, have only ferric oxide not have the Neodymium trioxide phase mutually in the XRD figure spectrum; And the peak of ferric oxide is very low by force.But XRF result shows (table 1-2), have neodymium element to precipitate in the precipitation, and proportion is not low in precipitation, has reached 20.13% and 18.10% in pH=5.5 and pH=7.5 respectively.The content of impurity elements such as Al, Si, Zn, Ca and P is also very low.With the method for one step of ammoniacal liquor precipitated iron ion and neodymium ion, the elemental composition that obtains is better.
Embodiment 3
At first, get 5g neodymium iron boron greasy filth, add 4mol/L hydrochloric acid 60ml in the waste material, fully the dissolving back is added excessive hydrogen peroxide in the filtrate and is stirred 10min.Then, regulate pH value by the ammoniacal liquor that adds 1:1 and be respectively 2, and filtrate is placed the heat collecting type heating stirrer, the control temperature of reaction is 70 ℃, slowly adds the 0.1mol/L sodium oxalate solution 300ml of heat and is allowed to condition at and react 60mins in the agitator.At last, will precipitate centrifugal oven dry and be placed in the box-type furnace, at T=800 ℃ of following roasting 90mins, namely get the neodymium Iron mixed oxide.By means of testing such as XRD, XRF, we obtain following result:
The XRF result (%) of the neodymium Iron mixed oxide that table 1-3 obtains for the precipitation agent roasting with the sodium oxalate
As seen from Figure 3, in the spike halfwidth minimum of the 800 ℃ of resulting throw out thing of calcination phase spectral lines, intensity is the highest, and the influence of the impurity back of the body end is minimum, thus we at this moment precipitated crystal degree is best as can be seen.The XRF result of table 1-3 shows that the yield of rare earth element is also very high, and neodymium element has reached 34.51%, and the praseodymium element has reached 10.87%.
By adding a step precipitation of sodium oxalate, can obtain uniform particles, the precipitation of better crystallinity degree.And foreign matter content is less; The cleaning in the process and removing by experiment of sodium ion and chlorion.With sodium oxalate as coprecipitator primary sedimentation Nd preferably
3+And Fe
3+, and proportioning is more near the material ratio of neodymium iron boron; Can be the subsequent ball milling condition that facilitates.
Claims (8)
1. the method for neodymium iron boron greasy filth regeneration prepared by co-precipitation neodymium ferriferous oxide, it is characterized in that, may further comprise the steps: after hydrogen peroxide oxidation is added in the pickling liquor of neodymium iron boron greasy filth, regulate pH value, once the sodium hydroxide of Tian Jiaing, ammoniacal liquor or sodium oxalate precipitation agent after insulation for some time under 60～100 ℃ of temperature, will precipitate centrifugal oven dry, and roasting at high temperature, obtain the neodymium ferriferous oxide.
2. according to the method for claim 1, it is characterized in that when being the precipitation agent of a step co-precipitation with sodium hydroxide, the top condition of its co-precipitation is: after the molten filtration of neodymium iron boron greasy filth acid, filtrate is added excessive mass concentration 30% hydrogen peroxide oxidation and is not stopped to stir; For preventing that ferric hydroxide colloid from generating, selecting to regulate pH value earlier is incubated again, therefore, regulate PH=4～9 earlier, controlling temperature of reaction then is 60～100 ℃, and the sodium hydroxide solution that adds 1mol/L reacts 60mins under agitation condition, last, to precipitate centrifugal oven dry and be placed in the box-type furnace, ℃ following roasting 90mins in T=400～600; The consumption of preferred sodium hydroxide solution is the corresponding 30ml sodium hydroxide solution of every 5g neodymium iron boron greasy filth.
3. according to the method for claim 2, it is characterized in that, regulate PH=7～9.
4. according to the method for claim 1, it is characterized in that, when being the precipitation agent of a step co-precipitation with ammoniacal liquor, the top condition of its co-precipitation is: after the molten filtration of neodymium iron boron greasy filth acid, filtrate is added excessive mass concentration 30% hydrogen peroxide oxidation and is not stopped to stir, add 30% ammoniacal liquor until regulating post precipitation solution PH=8～10, controlling temperature of reaction then is 60～100 ℃, and standing and reacting 60mins is last, to precipitate centrifugal and dry and be placed in the box-type furnace ℃ following roasting 90mins in T=400～600.
5. according to the method for claim 4, it is characterized in that, add 30% ammoniacal liquor until regulating post precipitation solution PH=5.5～7.5.
6. according to the method for claim 1, it is characterized in that, when being the precipitation agent of a step co-precipitation with sodium oxalate, the top condition of its co-precipitation is: after the molten filtration of neodymium iron boron greasy filth acid, filtrate is added excessive mass concentration 30% hydrogen peroxide oxidation and is not stopped to stir, for preventing that ferric hydroxide colloid from generating, selecting to regulate pH value earlier is incubated again, therefore, regulate PH=1～3 earlier, controlling temperature of reaction again is 60～100 ℃, and add temperature be 35-50 ℃ heat the 0.1mol/L sodium oxalate solution and be allowed to condition at and stir reaction 60mins down.At last, will precipitate centrifugal oven dry and be placed in the box-type furnace, ℃ following roasting 90mins in T=600～800, the corresponding 300ml sodium oxalate solution of preferred every 5g neodymium iron boron greasy filth.
7. according to the method for claim 1, it is characterized in that solid-to-liquid ratio is (1g) in the molten process of neodymium iron boron greasy filth acid: (10-15ml).
8. the neodymium ferriferous oxide for preparing according to the described method of claim 1-7, the mass content of its iron neodymium is respectively: 47.89%～63.44%, 18.10%～34.51%, all the other are the content of other elements.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310306657.6A CN103343234B (en) | 2013-07-19 | 2013-07-19 | Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310306657.6A CN103343234B (en) | 2013-07-19 | 2013-07-19 | Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103343234A true CN103343234A (en) | 2013-10-09 |
| CN103343234B CN103343234B (en) | 2015-01-14 |
Family
ID=49278059
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310306657.6A Active CN103343234B (en) | 2013-07-19 | 2013-07-19 | Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103343234B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103667715A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under C2H2O4-OH system |
| CN103667716A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under C2H2O4-NH3 system |
| CN103667719A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under OH-OH system |
| CN103667717A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under CO3-OH system |
| CN103789549A (en) * | 2013-12-17 | 2014-05-14 | 北京工业大学 | Method for synchronously recycling neodymium, praseodymium, dysprosium, cobalt and iron from neodymium-iron-boron oil sludge in NH3-OH system |
| CN103882234A (en) * | 2014-03-18 | 2014-06-25 | 北京工业大学 | Method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge |
| CN104498717A (en) * | 2014-12-02 | 2015-04-08 | 上海应用技术学院 | Recovery method for metal powder in rolling oil sludge |
| CN105238929A (en) * | 2014-10-06 | 2016-01-13 | 董亚伦 | Recovery and reuse of rare earth in waste Nd-Fe-B permanent magnet material |
| CN107794373A (en) * | 2017-11-06 | 2018-03-13 | 王志勇 | The integrated conduct method of the useless magnetic material of neodymium iron boron |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058232A (en) * | 1990-07-19 | 1992-01-29 | 中南工业大学 | From neodymium iron boron waste material, extract the method for neodymium |
| CN1119216A (en) * | 1994-09-22 | 1996-03-27 | 泰兴市君泰稀土实业有限公司 | Process for preparing neodymium and neodymium-dysprosium compounds by recovering waste neodymium-iron-boron |
| CN1237643A (en) * | 1998-05-12 | 1999-12-08 | 住友金属矿山株式会社 | Recovering method of valuable composition from rare earth element-containing material and alloy powder obtained therefrom |
| CN1605638A (en) * | 2004-06-28 | 2005-04-13 | 辽宁美宝稀土材料有限公司 | Process for recovering rare earth from neodymium-ion-boron waste materials |
| CN101200304A (en) * | 2007-09-19 | 2008-06-18 | 王洪志 | Technique for producing 99% praseodymium-neodymium oxides by using Nd-Fe-B smelting slag |
| CN102011020A (en) * | 2009-12-14 | 2011-04-13 | 包头市玺骏稀土有限责任公司 | Method for recovering rare earth elements from neodymium-iron-boron wastes |
| CN102154558A (en) * | 2011-03-23 | 2011-08-17 | 连云港市兆昱新材料实业有限公司 | Method for recovering rare earth by segments from neodymium iron boron waste |
| CN102154557A (en) * | 2011-03-23 | 2011-08-17 | 连云港市兆昱新材料实业有限公司 | Method for recovering rare earth elements from waste neodymium iron boron leftover material |
| CN102206755A (en) * | 2011-03-06 | 2011-10-05 | 林剑 | Method for separating and recovering valuable elements from neodymium-iron-boron wastes |
| KR101147643B1 (en) * | 2012-02-17 | 2012-05-23 | 한국지질자원연구원 | Neodymium leaching method using immersion method |
| CN102912134A (en) * | 2012-09-27 | 2013-02-06 | 信丰县包钢新利稀土有限责任公司 | Neodymium, iron and boron waste recycling process with approximately zero wastewater discharge |
| CN102912112A (en) * | 2012-10-20 | 2013-02-06 | 北京工业大学 | Method for pre-processing neodymium iron boron wire cutting waste oil sludge |
| CN103146925A (en) * | 2013-03-25 | 2013-06-12 | 安徽天泽矿业科技发展有限公司 | Method of recycling rear earth from neodymium iron boron waste |
-
2013
- 2013-07-19 CN CN201310306657.6A patent/CN103343234B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058232A (en) * | 1990-07-19 | 1992-01-29 | 中南工业大学 | From neodymium iron boron waste material, extract the method for neodymium |
| CN1119216A (en) * | 1994-09-22 | 1996-03-27 | 泰兴市君泰稀土实业有限公司 | Process for preparing neodymium and neodymium-dysprosium compounds by recovering waste neodymium-iron-boron |
| CN1237643A (en) * | 1998-05-12 | 1999-12-08 | 住友金属矿山株式会社 | Recovering method of valuable composition from rare earth element-containing material and alloy powder obtained therefrom |
| CN1605638A (en) * | 2004-06-28 | 2005-04-13 | 辽宁美宝稀土材料有限公司 | Process for recovering rare earth from neodymium-ion-boron waste materials |
| CN101200304A (en) * | 2007-09-19 | 2008-06-18 | 王洪志 | Technique for producing 99% praseodymium-neodymium oxides by using Nd-Fe-B smelting slag |
| CN102011020A (en) * | 2009-12-14 | 2011-04-13 | 包头市玺骏稀土有限责任公司 | Method for recovering rare earth elements from neodymium-iron-boron wastes |
| CN102206755A (en) * | 2011-03-06 | 2011-10-05 | 林剑 | Method for separating and recovering valuable elements from neodymium-iron-boron wastes |
| CN102154558A (en) * | 2011-03-23 | 2011-08-17 | 连云港市兆昱新材料实业有限公司 | Method for recovering rare earth by segments from neodymium iron boron waste |
| CN102154557A (en) * | 2011-03-23 | 2011-08-17 | 连云港市兆昱新材料实业有限公司 | Method for recovering rare earth elements from waste neodymium iron boron leftover material |
| KR101147643B1 (en) * | 2012-02-17 | 2012-05-23 | 한국지질자원연구원 | Neodymium leaching method using immersion method |
| CN102912134A (en) * | 2012-09-27 | 2013-02-06 | 信丰县包钢新利稀土有限责任公司 | Neodymium, iron and boron waste recycling process with approximately zero wastewater discharge |
| CN102912112A (en) * | 2012-10-20 | 2013-02-06 | 北京工业大学 | Method for pre-processing neodymium iron boron wire cutting waste oil sludge |
| CN103146925A (en) * | 2013-03-25 | 2013-06-12 | 安徽天泽矿业科技发展有限公司 | Method of recycling rear earth from neodymium iron boron waste |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103667717B (en) * | 2013-12-17 | 2016-06-29 | 北京工业大学 | A kind of at CO3The method simultaneously reclaiming neodymium, praseodymium, dysprosium, cobalt, ferrum under-OH system from neodymium iron boron greasy filth |
| CN103667719B (en) * | 2013-12-17 | 2016-07-06 | 北京工业大学 | A kind of method simultaneously reclaiming neodymium, praseodymium, dysprosium, cobalt, ferrum under OH-OH system from neodymium iron boron greasy filth |
| CN103667716A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under C2H2O4-NH3 system |
| CN103667717A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under CO3-OH system |
| CN103667715B (en) * | 2013-12-17 | 2016-05-18 | 北京工业大学 | A kind of at C2H2O4Under-OH system, from neodymium iron boron greasy filth, reclaim the method for neodymium, praseodymium, dysprosium, cobalt, iron simultaneously |
| CN103667715A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under C2H2O4-OH system |
| CN103667716B (en) * | 2013-12-17 | 2016-06-29 | 北京工业大学 | A kind of at C2H2O4-NH3The method simultaneously reclaiming neodymium, praseodymium, dysprosium, cobalt, ferrum under system from neodymium iron boron greasy filth |
| CN103789549B (en) * | 2013-12-17 | 2016-06-01 | 北京工业大学 | A kind of at NH3From neodymium iron boron greasy filth, reclaim the method for neodymium, praseodymium, dysprosium, cobalt, iron under-OH system simultaneously |
| CN103667719A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under OH-OH system |
| CN103789549A (en) * | 2013-12-17 | 2014-05-14 | 北京工业大学 | Method for synchronously recycling neodymium, praseodymium, dysprosium, cobalt and iron from neodymium-iron-boron oil sludge in NH3-OH system |
| CN103882234B (en) * | 2014-03-18 | 2015-12-30 | 北京工业大学 | A kind of method neodymium iron boron greasy filth being prepared into regeneration NdFeB magnetic powder |
| CN103882234A (en) * | 2014-03-18 | 2014-06-25 | 北京工业大学 | Method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge |
| CN105238929A (en) * | 2014-10-06 | 2016-01-13 | 董亚伦 | Recovery and reuse of rare earth in waste Nd-Fe-B permanent magnet material |
| CN105238929B (en) * | 2014-10-06 | 2017-07-04 | 永州市零陵远达新材料有限公司 | A kind of recovery of waste and old Nd-Fe-B permanent magnet material middle rare earth and utilization |
| CN104498717A (en) * | 2014-12-02 | 2015-04-08 | 上海应用技术学院 | Recovery method for metal powder in rolling oil sludge |
| CN107794373A (en) * | 2017-11-06 | 2018-03-13 | 王志勇 | The integrated conduct method of the useless magnetic material of neodymium iron boron |
| CN107794373B (en) * | 2017-11-06 | 2019-01-22 | 孙东江 | The integrated conduct method of the useless magnetic material of neodymium iron boron |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103343234B (en) | 2015-01-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103343234B (en) | Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation | |
| CN103343233B (en) | A kind of neodymium iron boron greasy filth reclaims the method for neodymium iron | |
| Peng | A literature review on leaching and recovery of vanadium | |
| CN103343235B (en) | Method for recovering neodymium and iron from neodymium iron boron oil sludge through two-step co-precipitation | |
| CN104152687B (en) | Aluminium, vanadium, molybdenum, the production technology of nickel element three-waste free discharge are extracted from black shale | |
| CN102432071B (en) | Method for integrally utilizing high-iron-content bauxite | |
| CN102094119A (en) | Method for preparing electrolytic manganese metal with low-grade pyrolusite wet leaching | |
| CN106611841B (en) | A method of nickel-cobalt-manganese ternary material precursor is prepared using nickel cobalt slag charge | |
| CN103773961A (en) | Method for extracting cobalt and nickel from manganese, cobalt and nickel waste residue | |
| CN104073634B (en) | A kind of method of nickel minerals leachate or electrolytic anode liquid deironing | |
| CN101717858B (en) | Method for extracting molybdenum, nickel, vanadium and ferrum from polymetallic black-shale paragentic minerals | |
| CN109554549A (en) | The method that high temperature and pressure leaches rare earth in recycling neodymium iron boron waste material | |
| CN102101699A (en) | Method for extracting pyrolusite and producing manganese sulfate by utilizing by-product in production of titanium white | |
| CN113809424A (en) | Method for recycling mixed waste of lithium nickel cobalt manganese oxide and lithium iron phosphate | |
| CN104480316B (en) | A kind of simplified industrial method reclaiming Co element from neodymium iron boron magnetic materials waste material | |
| CN104388711A (en) | Method for recovering rare earth by leaching rare earth oxide molten slag | |
| Yang et al. | Solvent extraction and separation of cobalt from leachate of spent lithium-ion battery cathodes with N263 in nitrite media | |
| CN105642448A (en) | Method for efficiently separating wolframite concentrate and scheelite concentrate from tungsten ore | |
| CN103898327A (en) | Method for extracting nickel from manganese cobalt nickel waste slag | |
| CN102828020A (en) | Method for closed cycle high-efficiency comprehensive recovery of multiple elements of gold concentrate | |
| CN102755892A (en) | Method and application of preparing high-level oxidation catalyst through cobalt ore smelting slag | |
| CN102417980B (en) | Method for producing nickel sulfate by leaching Lateritic nickle ores with both sulfuric acid and ammonia | |
| CN109879323A (en) | It is a kind of to prepare ferritic method using electric furnace dust and mill scale | |
| CN103264997B (en) | Method for extracting tellurium from low-concentration tellurium solution | |
| CN109264751A (en) | A method of extracting lithium carbonate and ammonium metavanadate from lepidolite and vanadium-containing shale |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |