CN101871072A - Method for recovering, smelting and reusing base material in jet mill procedure for sintered NdFeB production - Google Patents
Method for recovering, smelting and reusing base material in jet mill procedure for sintered NdFeB production Download PDFInfo
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- CN101871072A CN101871072A CN201010193011A CN201010193011A CN101871072A CN 101871072 A CN101871072 A CN 101871072A CN 201010193011 A CN201010193011 A CN 201010193011A CN 201010193011 A CN201010193011 A CN 201010193011A CN 101871072 A CN101871072 A CN 101871072A
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- base material
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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
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Abstract
The invention relates to a processing technology of a base material generated in a sintered NdFeB production process, in particular to a method for recovering, smelting and reusing a base material in a jet mill procedure for sintered NdFeB production, which solves the problem of the prior art that the base material generated in the jet mill procedure in the sintered NdFeB production process can not be processed. The method comprises the following steps: collecting, sealing and storing the base material from a jet mill; adding the collected base material from the jet mill to normal materials according to a certain ratio in the process of steel ingot batching, and then smelting the mixture to obtain steel ingot; crushing and shaping in a static pressure manner; and finally tempering and sintering. The processing method of the invention breaks through the traditional thinking of the existing processing method, and turns the existing traditional processing mode of recovering the directly scraped powder by a rare earth manufacturer and then purifying the rare earth material in the recovered powder by a chemical method into the mode of directly utilizing the powder.
Description
Technical field
The present invention relates to the treatment technology of the bed material that produced in a kind of sintered NdFeB production process, the recovery melting that is specially a kind of base material in jet mill procedure for sintered NdFeB production utilizes method again.
Background technology
Sintered NdFeB had obtained development rapidly in recent years as a kind of important functional material, but be accompanied by the swift and violent development of sintered NdFeB, produce the employed starting material of neodymium iron boron, especially the usage quantity of rare earth material is also increasing with surprising rapidity, though China's rare earth resources reserves account for about 55% of world's total reserves, be genuine rare earth resources big country, if but do not consider the starting material regeneration and effectively utilize, will face the serious consequence of scarcity of resources.
In the sintered NdFeB production process, generally adopt airflow milling powder process.In this operation, every batch of material always produces a certain proportion of bed material after airflow milling, the generation of these bed materials, a part is because the accumulated powder of airflow milling system self, and being the prepared steel ingot of melting operation, prior reason always has certain component segregation, the relatively poor part of crystallization has more α-Fe, make steel ingot be difficult to fragmentation, final generation a certain proportion of (generally between 2~10%) is difficult to the residual mill of the thicker powder of ground grains chamber, scrap after clearing, all the more so when especially producing the high energy product magnet.Though contained α-Fe is more for this part bed material, (normal powder content of rare earth is generally 28~35% but still have the significant proportion rare earth composition, this part powder content of rare earth general about 20~30%), if directly scrap, then to cause resource to waste greatly, especially China advocates at present and builds saving type country, and we more should pay attention to the recycling problem of this type of resource.
Summary of the invention
Present method can't be handled the problem of utilizing again in order to solve the bed material that at present the airflow milling operation in the sintered NdFeB process is produced, and the recovery melting that has proposed a kind of base material in jet mill procedure for sintered NdFeB production utilizes method again.
The present invention adopts following technical scheme to realize: a kind of recovery melting of base material in jet mill procedure for sintered NdFeB production utilizes method again, may further comprise the steps:
(1), the airtight preservation of the collection of airflow milling bed material:
In the sintered NdFeB production process,, put into the stainless steel sealed can and preserve every batch of material bed material that is difficult to fragmentation in the residual mill chamber after airflow milling powder process.
(2). the airflow milling bed material of collecting added to when steel ingot is prepared burden carry out melting in the orthodox material together, addition means: select the thick plain aluminium foil of web-like industry 0.1-0.2mm for use, be cut into the aluminium-foil paper of 250-500 * 250-500mm size, bed material is coated; The bed material adding proportion is 30% to the maximum.
Because during the smelting furnace continuous smelting, crucible temperature is higher, powder is directly joined starting material with institute and is put into crucible, the bed material crucible bottom of will directly bleeding, and obvious oxidation can take place in local fine powder in very short time, even burning.So select for use medium in advance bed material to be wrapped up; Owing to all need to add the metal A l of 0.1-1% in the neodymium iron boron production, normal batching generally selects for use aluminium sheet or aluminium bar to be cut into the suitable dimension interpolation.Like this for flow of process air mill bed material, our aluminium foil paper is as lapping, and the weight of aluminium foil just in time can count ingredients by weight, and the insufficient section of metal A l is still with the aluminium sheet or the aluminium bar that are cut into suitable dimension in the batching; The aluminium, the bed material that prepare are smelted into steel ingot with other starting material to melting operation.Bed material is coated with aluminium-foil paper, both be difficult for when vacuumizing, being taken away, avoid powder directly to contact sidewall of crucible again and cause the powder temperature to raise rapidly, abrupt oxidization even burning by the melting vacuum system; And do not have other impurity outside the food ingredient to bring alloy into, can not cause alloying constituent and Effect on Performance.
The bed material adding proportion is 30% to the maximum.Add very fewly, the bed material utilization ratio descends; Add too much, can influence normal ingot quality, product performance height and consistence, and slag is too much.The present invention determines following adding proportion principle:
(a) whether add and addition is determined according to the product performance class: (be generally H making high trade mark product
Cj+ BH
Max>55 product, H
Cj, BH
MaxUnit is respectively KOe, MGOe) time since oxygen level and Composition Control are required tighter, so the bed material addition to add less or not add, on the make, the bed material add-on then can be morely during low-grade product.Ratio is improper, can bring the variation of final Nd-Fe-B permanent magnet product magnetic property, promptly produces certain deviation owing to factors such as addition is bigger can make the magnetic property (trade mark) of final permanent magnet and design, even unacceptable product occurs.In the production reality, how many ratio bed materials those trades mark can add and can produce great influence to the final magnet performance, need the technician to determine by the experiment of limited number of time according to self enterprise practical.The present invention provides following technical parameter: aborning, during low-grade sintered ndfeb permanent magnet body, the NdFeB bed material powder with 3%-10% adds in the normal batching, can obtain the neodymium iron boron magnetic body with the component design basically identical; As the middle-weight rare earths amount of filling a prescription designs to 33-34wt%, and the adding proportion maximum can increase to 30%.The bed material that realization is produced the airflow milling operation is directly used in the purpose of sintered Nd Fe B industrialized production.
(b) to a certain concrete trade mark product, adding proportion also will suitably be adjusted according to interpolation bed material quality quality (content of rare earth height).
(3). obtain steel ingot then;
(4). steel ingot is adopted hydrogen fragmentation or Mechanical Crushing, and airflow milling powder process, the powder of one-tenth 3-5 μ m;
(5). powder is orientated in the Magnetic field press of 1280-1440KA/m, uses vertical steel mill pressure and adds the moulding of isostatic cool pressing mode;
(6). green compact are 10
-2~10
-3Under the Pa vacuum condition behind 1333~1383K sintering, 3~5h the gas quenching but,, finally make sintered compact in 733~873k temper, 2~3h in 1073~1173k temper 3h.
Treatment process of the present invention has broken through traditional thinking of existing treatment process, and existing traditional back of directly scrapping is changed into directly to the powder utilization with the rare earth material in the chemical process purification powder by the recovery of rare earth producer.Because what this treatment process adopted is physical method, the technology of treatment process is simple, need not to add separately equipment, turns waste into wealth, and has reduced the waste of material, has saved the cost that feeds intake.This method makes sintered Nd Fe B manufacturer oneself just can handle the bed material that digestion is produced, and realizes that the bed material material digests on the spot, has shortened the regeneration cycle greatly.Compare with existing chemical treatment method, this treatment process can not brought new " three wastes " emission problem.And the control adding proportion can not produce big influence to the product performance of permanent magnet, and the permanent magnet that promptly adds behind the bed material is compared with the permanent magnet that does not add bed material with the trade mark, and product performance are basic identical.
Embodiment
The recovery melting of embodiment 1, a kind of base material in jet mill procedure for sintered NdFeB production utilizes method again, may further comprise the steps:
(1), the airtight preservation of the collection of airflow milling bed material:
The broken bed material that is difficult to that the airflow milling operation is produced is left concentratedly, deposited and to seal nitrogen filled protection, prevent the increase of put procedure oxygen level.For preventing the powder oxidation, charge into nitrogen protection in the sealed can; Be fit to during general powder oxygen content≤5000ppm add and utilize (deposit within 10 days under the bed material inflated with nitrogen condition and can both satisfy this condition) with this method.
(2). the airflow milling bed material collected added in 10% ratio when steel ingot is prepared burden carry out melting in the orthodox material together, addition means: select the thick plain aluminium foil of web-like industry 0.1mm for use, be cut into the aluminium-foil paper of 400 * 400mm size, bed material is coated; During operation, bed material is deposited in the stainless cylinder of steel, fills small amount of nitrogen in jar, prevents a jar interior powder oxidation; Action wants fast during coating, and simultaneously, the material for preparing will in time carry out melting, and storage period is not above eight hours.During batching, add the Pr-Nd alloy of 0.3wt% by the N35 trade mark prescription of design; The aluminium sheet of the insufficient section of metal A l after with cutting supplied.
The together normal sintered NdFeB production technique of subsequent handling after the melting: powder process, moulding, sintering, tempering, detection magnetic property.
The magnet that adds bed material from the result of following table 1 is as can be seen compared with the magnet that does not add bed material, and every performance index are suitable substantially.
Table 1
Embodiment 2, and a kind of recovery melting of base material in jet mill procedure for sintered NdFeB production utilizes method again, may further comprise the steps: the airtight preservation of the collection of airflow milling bed material:
Add the Pr-Nd alloying ingredient of 0.15% (weight ratio) by the 35H trade mark prescription of design, select the thick plain aluminium foil of web-like industry 0.2mm for use, be cut into the aluminium-foil paper of 300 * 300mm size, the bed material of raw material weight 5% is coated, the aluminium sheet of the insufficient section of metal A l after with cutting supplied; Carry out melting after preparing together, the together normal sintered NdFeB production technique of subsequent handling: powder process, moulding, sintering, tempering, detection magnetic property.The magnet that adds bed material is as can be seen from Table 2 compared with the magnet that does not add bed material, and every performance index are suitable substantially.
Table 2
Claims (1)
1. the recovery melting of a base material in jet mill procedure for sintered NdFeB production utilizes method again, may further comprise the steps:
(1), the airtight preservation of the collection of airflow milling bed material;
(2), the airflow milling bed material of collecting is added to when steel ingot is prepared burden carry out melting in the orthodox material together, addition means: select the thick aluminium foil of 0.1-0.2mm for use, be cut into the aluminium-foil paper of 250-500 * 250-500mm size, bed material is coated, the bed material adding proportion is 30% to the maximum;
(3), obtain steel ingot then;
(4), with the steel ingot fragmentation, and airflow milling powder process becomes the powder of 3-5 μ m;
(5), powder is orientated in the Magnetic field press of 1280-1440KA/m, use the vertical steel mill and press and add the moulding of isostatic cool pressing mode;
(6), green compact are 10
-2~10
-3Under the Pa vacuum condition behind 1333~1383K sintering, 3~5h the gas quenching but,, finally make sintered compact in 733~873k temper, 2~3h in 1073~1173k temper 3h.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102719725A (en) * | 2012-07-10 | 2012-10-10 | 宁波科田磁业有限公司 | Sintered neodymium iron boron waste remoulding method |
CN103551563A (en) * | 2013-10-11 | 2014-02-05 | 南通万宝磁石制造有限公司 | REPM (rear earth permanent magnet) material recycling method |
CN104190943A (en) * | 2014-08-04 | 2014-12-10 | 中磁科技股份有限公司 | Method for recycling sintered neodymium-iron-boron waste materials |
CN104907560A (en) * | 2015-06-18 | 2015-09-16 | 包头金山磁材有限公司 | Sintering method capable of reducing cracks of neodymium iron boron products |
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CN1031863A (en) * | 1988-04-30 | 1989-03-22 | 大冶钢厂 | A kind of method that in molten steel, adds selenium |
CN1687470A (en) * | 2005-05-18 | 2005-10-26 | 西北有色金属研究院 | Method for preparing Nd-Fe-B alloys by using waste |
CN101407896A (en) * | 2008-11-06 | 2009-04-15 | 山西金山磁材有限公司 | Method for improving toughness of Nd-Fe-B permanent magnetic material by adding metal |
-
2010
- 2010-06-02 CN CN201010193011A patent/CN101871072A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1031863A (en) * | 1988-04-30 | 1989-03-22 | 大冶钢厂 | A kind of method that in molten steel, adds selenium |
CN1687470A (en) * | 2005-05-18 | 2005-10-26 | 西北有色金属研究院 | Method for preparing Nd-Fe-B alloys by using waste |
CN101407896A (en) * | 2008-11-06 | 2009-04-15 | 山西金山磁材有限公司 | Method for improving toughness of Nd-Fe-B permanent magnetic material by adding metal |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102719725A (en) * | 2012-07-10 | 2012-10-10 | 宁波科田磁业有限公司 | Sintered neodymium iron boron waste remoulding method |
CN103551563A (en) * | 2013-10-11 | 2014-02-05 | 南通万宝磁石制造有限公司 | REPM (rear earth permanent magnet) material recycling method |
CN104190943A (en) * | 2014-08-04 | 2014-12-10 | 中磁科技股份有限公司 | Method for recycling sintered neodymium-iron-boron waste materials |
CN104907560A (en) * | 2015-06-18 | 2015-09-16 | 包头金山磁材有限公司 | Sintering method capable of reducing cracks of neodymium iron boron products |
CN104907560B (en) * | 2015-06-18 | 2019-11-08 | 包头金山磁材有限公司 | A kind of sintering method reducing neodymium iron boron product crackle |
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