CN102912134A - Neodymium, iron and boron waste recycling process with approximately zero wastewater discharge - Google Patents
Neodymium, iron and boron waste recycling process with approximately zero wastewater discharge Download PDFInfo
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- CN102912134A CN102912134A CN2012103688419A CN201210368841A CN102912134A CN 102912134 A CN102912134 A CN 102912134A CN 2012103688419 A CN2012103688419 A CN 2012103688419A CN 201210368841 A CN201210368841 A CN 201210368841A CN 102912134 A CN102912134 A CN 102912134A
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- neodymium
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a neodymium, iron and boron waste recycling process with approximately zero wastewater discharge. The method is characterized in that recycling and separating for neodymium, terbium, dysprosium and cobalt in neodymium, iron and boron waste are researched, means such as fine grinding and crushing for the waste, oxidizing roasting, prior dissolution in hydrochloric acid, neutralization and impurity removal, double-salt iron settling and extraction separation are selected according to chemical properties of elements contained in the waste, valuable elements in the neodymium, iron and boron waste are successfully extracted, and neodymium oxide, terbium oxide, dysprosium oxide and cobalt oxide which are high in purity are obtained. The neodymium, iron and boron waste recycling process is simple, the production cost is low, an obvious economical benefit is realized, environmental pollution is prevented, and the process is applicable to industrial continuous production. Besides, the extraction rates of manufactured neodymium oxide, terbium oxide, dysprosium oxide and cobalt oxide products are maximized, and quality indexes of the manufactured neodymium oxide, terbium oxide, dysprosium oxide and cobalt oxide products meet industrial standards or customer standards.
Description
Technical field
The present invention relates to a kind of neodymium iron boron waste material near wastewater zero discharge and reclaim technique.
Background technology
Neodymium iron boron is a kind of permanent magnet material of superior performance, is widely used in every field, because the factor of production technique can produce about 20% waste material in the production and application process.Contain 30% the rare earth element of having an appointment (it is about 90% wherein to contain neodymium, and all the other are terbium, dysprosium etc.) in the NdFeB material, some NdFeB material contains 2% in addition
~3% cobalt element.The recovery of NdFeB material has not only rationally utilized resource, has also reduced environmental pollution simultaneously.The employing that has at present double salt precipitation, alkali the technique such as turn and reclaimed rare earth; but the heavy rare earths rate of recovery is low: the employing that also has sulfuric acid dissolution, double salt precipitation rare earth, alkali transform again method recovering rare earth through dissolving with hydrochloric acid, extracting and separating; but low because of its metal recovery rate, the chemical materials consumption is large, cost is high; in acidolysis and alkaline hydrolysis process, produce a large amount of liquid debris and solid waste; caused secondary pollution to environment, also restricted this Process Planning modelling and used.
Summary of the invention
A kind of neodymium iron boron waste material near wastewater zero discharge reclaims technique, adopts following processing method: it is 100 that neodymium iron boron waste material is carried out first the fine grinding pulverizing
~400 purpose powder are again 400
~Calcination 60 under 800 ℃ of temperature condition
~Making the ferrous iron complete oxidation in 180 minutes is ferric iron, then with the useless powder after the roasting and an acidic catalyst, water 1:0.1 by weight
~2.0:0.8
~1.5 ratio add in the retort, heating makes temperature reach 55
~1 100 ℃, stirring reaction 4
~9 hours, be cooled to 20
~30 ℃ of filtrations make solids separate with liquids, get liquids A, solids X; With liquids A, oxygenant, neutralizing agent are by weight 0.2
~4: 0.01
~0.2:0.01
~0.5 ratio mix, reach 75 in temperature
~110 ℃ of lower stirrings 30
~50 minutes, heat was filtered to get solids Y and liquids B; Liquids B has been obtained higher Neodymium trioxide, terbium sesquioxide and the dysprosium oxide of purity through extracting and separating, precipitation and calcination operation again.
Solids Y gets back to calcining process and repeats above-mentioned processing step.
The heavy iron of molten, double salt, precipitate and separate can obtain the higher oxidation brill of purity to solids X entirely through acid again.
An acidic catalyst that adds is following one or more mixtures: sulfuric acid, phosphoric acid, hydrochloric acid, nitric acid, hydrofluoric acid, acetic acid.
The neutralizing agent that adds is following one or more mixtures: bicarbonate of ammonia, sodium hydroxide, ammoniacal liquor, fluorine
Change hydrogen ammonium, unslaked lime, magnesium oxide, yellow soda ash.
The oxygenant that adds is following one or more mixtures: hydrochloric acid, potassium permanganate, hydrogen peroxide, sodium chlorate.
Technique of the present invention is simple, production cost is low, has significant economic benefit.Do not produce environmental pollution, be applicable to industrialization and produce continuously; It is high that prepared oxidation money, oxidation examination, oxidation are plucked, the product extracted amount is bored in oxidation, and quality index all meets industry standard or Customer Standard.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
A kind of neodymium iron boron waste material near wastewater zero discharge reclaims technique, adopts following processing method: it is 100 that neodymium iron boron waste material is carried out first the fine grinding pulverizing
~400 purpose powder are again 400
~Calcination 60 under 800 ℃ of temperature condition
~Making the ferrous iron complete oxidation in 180 minutes is ferric iron, then with the useless powder after the roasting and an acidic catalyst, water 1:0.1 by weight
~2.0:0.8
~1.5 ratio add in the retort, heating makes temperature reach 55
~1 100 ℃, stirring reaction 4
~9 hours, be cooled to 20
~30 ℃ of filtrations make solids separate with liquids, get liquids A, solids X; With liquids A, oxygenant, neutralizing agent are by weight 0.2
~4: 0.01
~0.2:0.01
~0.5 ratio mix, reach 75 in temperature
~110 ℃ of lower stirrings 30
~50 minutes, heat was filtered to get solids Y and liquids B; Liquids B has been obtained higher Neodymium trioxide, terbium sesquioxide and the dysprosium oxide of purity through extracting and separating, precipitation and calcination operation again.
Solids Y gets back to calcining process and repeats above-mentioned processing step.
The heavy iron of molten, double salt, precipitate and separate can obtain the higher oxidation brill of purity to solids X entirely through acid again.
An acidic catalyst that adds is following one or more mixtures: sulfuric acid, phosphoric acid, hydrochloric acid, nitric acid, hydrofluoric acid, acetic acid.
The neutralizing agent that adds is following one or more mixtures: bicarbonate of ammonia, sodium hydroxide, ammoniacal liquor, ammonium bifluoride, unslaked lime, magnesium oxide, yellow soda ash.
The oxygenant that adds is following one or more mixtures: hydrochloric acid, potassium permanganate, hydrogen peroxide, sodium chlorate.
Following the present invention is further described in connection with native process flow figure and embodiment, but not only comprises following examples.
Embodiment 1:
Be 300 purpose powder with 1OOOKG neodymium iron boron waste material refinement grinding particle size, through 150 minutes after oxidation calcination under 550 ℃ of temperature condition, in the input retort, add water 15OOKG and 500KG hydrochloric acid, the making beating heating makes temperature of reactor reach 100 ℃, and stirring reaction 5 hours is cooled to 25 ℃ of filtrations, make solid-liquid separation, get solids X and liquids A.Liquids A is added hydrogen peroxide 20KG bicarbonate of ammonia 1OOKG under 90 ℃ of conditions, stir in 35 minutes He after the removal of impurities and filter, get solids Y and liquids B.Solids Y comes back to calcining process and repeats above-mentioned step; Liquids B separates through 40 grades of neodymium terbiums of PS07 one sulfonated kerosene one hydrochloric acid system and 70 grades of terbium dysprosiums obtain respectively Neodymium trichloride, terbium chloride, Dysprosium trichloride solution after separating, and precipitates respectively, just obtains satisfactory Neodymium trioxide, terbium sesquioxide, dysprosium oxide product after the calcination.Detect by the GB index, it is qualified that product detects, and packs, puts in storage for sale.
The solids X that solid-liquid separation obtains adds 5OOKG hydrochloric acid when adding 1OOKG water making beating post-heating to 110 ℃ again, carries out stirring reaction 2 hours, then filters, and gets solids Z (abandoning) and liquids C; Filter to get cobalt chloride solution through double salt is heavy assorted again, precipitate respectively again, just obtain satisfactory oxidation after the calcination and bore product.Detect by the GB index, it is qualified that product detects, and packs, puts in storage for sale.
Embodiment 2:
Be 200 purpose powder with 1 OOOKG neodymium iron boron waste material refinement grinding particle size, through 100 minutes after oxidation calcination under 650 ℃ of temperature condition, in the input retort, add water 800KG and 300KG oxalic acid, the making beating heating makes temperature of reactor reach 100 ℃, and stirring reaction 7 hours is cooled to 25 ℃ of filtrations, make solid-liquid separation, get solids X and liquids A.Liquids A is added unslaked lime 3OKG, and sodium chlorate 60KG stirs in 45 minutes He after the removal of impurities under 90 ℃ of conditions and filters, and gets solids Y and liquids B.Solids Y comes back to calcining process and repeats above-mentioned step; Liquids B separates through 40 grades of neodymium terbiums of P507 one sulfonated kerosene one hydrochloric acid system and 70 grades of terbium dysprosiums obtain respectively Neodymium trichloride, terbium chloride, Dysprosium trichloride solution after separating, and precipitates respectively, just obtains satisfactory Neodymium trioxide, terbium sesquioxide, dysprosium oxide product after the calcination.Detect by the GB index, it is qualified that product detects, and packs, puts in storage for sale.
The solids X that solid-liquid separation obtains adds 5OOKG hydrochloric acid when adding 100 KG water making beating post-heating to 110 ℃ again, carries out stirring reaction 2 hours, then filters, and gets solids Z (abandoning) and liquids C; Filter to get cobalt chloride solution through double salt is heavy assorted again, precipitate respectively again, just obtain satisfactory oxidation after the calcination and bore product.Detect by the GB index, it is qualified that product detects, and packs, puts in storage for sale.
The experiment proved that an acidic catalyst of adding can be following one or more mixtures: sulfuric acid, phosphoric acid, hydrochloric acid, nitric acid, hydrofluoric acid, acetic acid, oxalic acid.The neutralizing agent that adds is following one or more mixtures: hydrochloric acid, sodium chlorate, sodium hydroxide, ammoniacal liquor, ammonium acid fluoride; The oxygenant that adds is following one or more mixtures: potassium permanganate, hydrogen peroxide, unslaked lime, magnesium oxide, yellow soda ash.
Mass analysis: the oxide product quality that obtains through various separation, precipitation, calcination is as follows
Conclusion:
Adopt dispersion and fining, oxidizing roasting, hydrochloric acid excellent molten, in and the operations such as removal of impurities, extracting and separating, precipitation and calcination, can reclaim preferably the metal values elements such as neodymium in the neodymium iron boron waste material, terbium, dysprosium, cobalt, and the rare earth total recovery has surpassed more than 90%, can find out that by the mass analysis result Neodymium trioxide, terbium sesquioxide, oxidation are plucked dysprosium, cobalt oxide and all met GB control requirement.So conclude that this processing method advanced person is feasible, reach advanced international level.
Claims (4)
1. the neodymium iron boron waste material near wastewater zero discharge reclaims technique, it is characterized in that adopting following processing method: it is 100 that neodymium iron boron waste material is carried out first the fine grinding pulverizing
~400 purpose powder are again 400
~Calcination 60 under 800 ℃ of temperature condition
~Making the ferrous iron complete oxidation in 180 minutes is ferric iron, then with the useless powder after the roasting and an acidic catalyst, water 1:0.1 by weight
~2.0:0.8
~1.5 ratio add in the retort, heating makes temperature reach 55
~1 100 ℃, stirring reaction 4
~9 hours, be cooled to 20
~30 ℃ of filtrations make solids separate with liquids, get liquids A, solids X; With liquids A, oxygenant, neutralizing agent are by weight 0.2
~4: 0.01
~0.2:0.01
~0.5 ratio mix, reach 75 in temperature
~110 ℃ of lower stirrings 30
~50 minutes, heat was filtered to get solids Y and liquids B; Liquids B has been obtained higher Neodymium trioxide, terbium sesquioxide and the dysprosium oxide of purity through extracting and separating, precipitation and calcination operation again.
2. a kind of neodymium iron boron waste material near wastewater zero discharge according to claim 1 reclaims technique, and an acidic catalyst that it is characterized in that described adding is following one or more mixtures: sulfuric acid, phosphoric acid, hydrochloric acid, nitric acid, hydrofluoric acid, acetic acid.
3. a kind of neodymium iron boron waste material near wastewater zero discharge according to claim 1 reclaims technique, and the neutralizing agent that it is characterized in that described adding is following one or more mixtures: bicarbonate of ammonia, sodium hydroxide, ammoniacal liquor, ammonium bifluoride, unslaked lime, magnesium oxide, yellow soda ash.
4. a kind of neodymium iron boron waste material near wastewater zero discharge according to claim 1 reclaims technique, and the oxygenant that it is characterized in that described adding is following one or more mixtures: hydrochloric acid, potassium permanganate, hydrogen peroxide, sodium chlorate.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103343234A (en) * | 2013-07-19 | 2013-10-09 | 北京工业大学 | Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation |
| 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 |
| CN104404255A (en) * | 2014-11-04 | 2015-03-11 | 连云港市兆昱新材料实业有限公司 | Simplified method for pretreatment-acid leaching of neodymium iron boron waste material |
| CN104480316A (en) * | 2014-12-24 | 2015-04-01 | 连云港市兆昱新材料实业有限公司 | Simple and convenientindustrial method for recovering Co element from NdFeBmagnetwaste materials |
| WO2016019044A1 (en) * | 2014-07-29 | 2016-02-04 | Trustees Of The University Of Pennsylvania | Simple chemical method for the separation of rare earth metals |
| CN105886776A (en) * | 2016-04-23 | 2016-08-24 | 赣州齐飞新材料有限公司 | Technological method for recycling rare earth from neodymium-iron-boron multi-line cutting waste |
| CN107758679A (en) * | 2017-10-10 | 2018-03-06 | 北京工业大学 | A kind of technique that boron is reclaimed from waste and old NdFeB material |
| CN108295864A (en) * | 2018-02-08 | 2018-07-20 | 北京科技大学 | A kind of method that neodymium iron boron secondary resource prepares denitrating catalyst |
| CN109593977A (en) * | 2018-11-07 | 2019-04-09 | 东北师范大学 | A method of removal is containing iron ion in neodymium, praseodymium, dysprosium and ferrous solution |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103146925B (en) * | 2013-03-25 | 2014-07-09 | 安徽天泽矿业科技发展有限公司 | Method of recycling rear earth from neodymium iron boron waste |
| 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 |
| CN103343234A (en) * | 2013-07-19 | 2013-10-09 | 北京工业大学 | Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation |
| 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 |
| 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 |
| US10704122B2 (en) | 2014-07-29 | 2020-07-07 | The Trustees Of The University Of Pennsylvania | Simple chemical method for the separation of rare earth metals |
| WO2016019044A1 (en) * | 2014-07-29 | 2016-02-04 | Trustees Of The University Of Pennsylvania | Simple chemical method for the separation of rare earth metals |
| CN104404255A (en) * | 2014-11-04 | 2015-03-11 | 连云港市兆昱新材料实业有限公司 | Simplified method for pretreatment-acid leaching of neodymium iron boron waste material |
| CN104480316A (en) * | 2014-12-24 | 2015-04-01 | 连云港市兆昱新材料实业有限公司 | Simple and convenientindustrial method for recovering Co element from NdFeBmagnetwaste materials |
| CN104480316B (en) * | 2014-12-24 | 2016-12-07 | 连云港市兆昱新材料实业有限公司 | A kind of simplified industrial method reclaiming Co element from neodymium iron boron magnetic materials waste material |
| CN105886776A (en) * | 2016-04-23 | 2016-08-24 | 赣州齐飞新材料有限公司 | Technological method for recycling rare earth from neodymium-iron-boron multi-line cutting waste |
| CN107758679B (en) * | 2017-10-10 | 2020-01-24 | 北京工业大学 | Process for recovering boron from waste neodymium iron boron material |
| CN107758679A (en) * | 2017-10-10 | 2018-03-06 | 北京工业大学 | A kind of technique that boron is reclaimed from waste and old NdFeB material |
| CN108295864A (en) * | 2018-02-08 | 2018-07-20 | 北京科技大学 | A kind of method that neodymium iron boron secondary resource prepares denitrating catalyst |
| CN109593977A (en) * | 2018-11-07 | 2019-04-09 | 东北师范大学 | A method of removal is containing iron ion in neodymium, praseodymium, dysprosium and ferrous solution |
| CN109593977B (en) * | 2018-11-07 | 2021-11-23 | 东北师范大学 | Method for removing iron ions in neodymium, praseodymium, dysprosium and iron-containing solution |
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Application publication date: 20130206 |