CN108133819A - A kind of reuse method of sintered NdFeB band oil waste material - Google Patents
A kind of reuse method of sintered NdFeB band oil waste material Download PDFInfo
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- CN108133819A CN108133819A CN201711293901.4A CN201711293901A CN108133819A CN 108133819 A CN108133819 A CN 108133819A CN 201711293901 A CN201711293901 A CN 201711293901A CN 108133819 A CN108133819 A CN 108133819A
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- waste material
- sintered ndfeb
- band oil
- neodymium iron
- iron boron
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
A kind of method that sintered NdFeB band oil waste material recycles, includes the following steps：It deoils, abrasive material is vibrated in pickling, rinses, and drying, hydrogen is broken, dispensing, and airflow milling milling is suppressed, sintering, die mould and secondary ageing processing.The present invention selects degreaser to deoil, again surface scale is removed with pickle pickling, and increase the pretreatment mode that vibration grinds off deep layer oxide skin, the processing of neodymium iron boron magnetic body scraped surface is clean, a certain proportion of rare earth oxide is added in the powder stage processed to improve magnet performance, and through die mould and ageing treatment, the neodymium iron boron magnetic body comprehensive performance of preparation is suitable with original magnet performance, and coercivity significantly improves.
Description
Technical field
The present invention relates to the reuse methods of neodymium iron boron waste material, and in particular to a kind of to prepare sintering neodymium iron using the oily waste material of band
The method of boron magnet steel.
Background technology
Sintered NdFeB magnet is the most strong permanent-magnet material of current composite magnetic property.In consumer electronics, energy saving household electrical appliances, doctor
The fields such as equipment and new-energy automobile are treated to be more and more widely used.Due to the meeting pair of exploitation wantonly of rare earth raw material
Environment causes irremediable consequence, and rare earth permanent-magnetic material is a kind of important strategic resource, can be widely used for civilian and army
With field, protection of resources has been carried out rare earth permanent-magnetic material both at home and abroad, save rare earth resources to China's development with great
Strategic importance.
At present, the process for machining of sintered NdFeB is to be sliced, based on the manufacturing procedures such as wire cutting.These processing apparatus are all
It needs to lubricate using oil as medium.All material head material skins processed all are with oil, and very big shadow is generated to later use
It rings.As directly using that impurity can be made to bring into matrix, properties of product caused to deteriorate.
Currently, neodymium iron boron magnetic body processing enterprise in part gradually adopts the mode of ball blast after boiling or high temperature evaporation, although
Available standard is reached, but magnet performance is relatively low.It is given up as Chinese patent 200910003955.1 is disclosed with neodymium iron boron powder
The method that material makes Nd-Fe-B permanent magnet material, invention heating remove oil and moisture in powder scrap.Using heating
If method removal oil, surface treatment is not clean enough and big with oxygen amount, and subsequent product performance is relatively low.
Chinese patent 99101105.8 discloses the method that Nd-Fe-B series permanent magnet is made of leftover bits and pieces of material, by leftover bits and pieces of material powder
10-95%, Fu Tie, rich rare earth alloy powder press 0-20% respectively（The low trade mark）, 20-50%（The high trade mark）, 40-80%（The superelevation trade mark）Match
Material ratio is weighed.Cleaned in waste powder preparation process using cleaning agent, pickling, roasting pretreatment mode, not except deep layer oxide skin,
Waste material pretreatment is not thorough enough.
Invention content
The technical problem to be solved by the present invention is to be handled sintered NdFeB band oil waste material, by adding certain ratio
The rare earth oxide of example, it is suitable with original magnet performance or increase to make to re-sinter magnet, solves to re-sinter magnet performance inclined
The problem of low.
To achieve the above object, the present invention uses following technical scheme：
The band oil waste material that waste material of the present invention is generated for neodymium iron boron magnetic body after machined；
A kind of method that sintered NdFeB band oil waste material recycles, includes the following steps：
（1）It deoils, neodymium iron boron magnetic body band oil waste material is positioned in the degreaser being configured, heat, 50 ~ 60 DEG C of heating temperature,
2 ~ 3h of time, removal are attached to the part greasy dirt of scraped surface；
（2）Pickling, the neodymium iron boron magnetic body waste material after deoiling are positioned in pickle, and pickling time 1-2h removes step of deoiling
The greasy dirt that does not remove completely simultaneously eliminates partial surface oxidation object；
（3）Abrasive material is vibrated, the neodymium iron boron magnetic body waste material after pickling is put into vibrating ball-mill, pours into abrasive material, vibration frequency 40-
60HZ, time are 1-2 h, grind off deep layer oxide skin；
（4）It rinses, the waste material giant of the neodymium iron boron magnetic body after abrasive material is rinsed；
（5）Drying, oven temperature are 100-120 DEG C, time 1-2h；
（6）Hydrogen is broken, and waste material hydrogen is broken into -200 mesh powder of 150 mesh, and Dehydroepiandrosterone derivative, and desorption temperature is 550-580 DEG C, the time
5-6 h（Normal 600 ~ 610 DEG C of desorption temperature）；
（7）Dispensing, the rare earth oxide and waste material for adding in 5-7% weight are mixed, while add antioxidant and lubricant；
（8）Airflow milling is milled, and powder particles is controlled, mixed powder is carried out at 2.7 ~ 3.2 μm, after milling, add lubricant；
（9）Powder is pressed into the specification of needs by moulding press, and then green compact are put into vacuum sintering furnace and are sintered, sintering temperature
1020-1040 DEG C of degree, time 4-5h obtains Nd-Fe-B magnet steel；
（10）The Nd-Fe-B magnet steel that die mould is obtained carries out two sections of ageing treatments, and aging technique is 880-900 DEG C of * 1.5-3h,
450-500℃*3.5 -5h。
The rare earth oxide is Gd2O3,Wherein Gd contents are 75% ~ 80% weight.
Sodium hydroxide of the degreaser composition proportion for 2-8%, the sodium carbonate of 3-10%, the OP-10 of 1-5%, surplus are
Water.
The nitric acid of a concentration of 5-8% of pickle.
The vibrating ball-mill is disk vibrating ball-mill.
The abrasive material and neodymium iron boron magnetic body waste material ratio are 1:1-1:2.
The abrasive material is spherical or triangle abrasive material, and preferably with triangle abrasive material, the abrasive material proportioning is 60-70%'s
The black corundum of silicon carbide and 30-40%.
The antioxidant additive amount is the 0.05%-0.2% of dispensing total weight, and the antioxidant is by hydroxyl phenol and gasoline
Mixing composition.
The lubricant additive amount is the 0.05%-0.2% of dispensing total weight, and the lubricant is by barium stearate, stearic acid
Sodium lactate, ammonium persulfate and paraffin composition.
The present invention compared with prior art, is had the following technical effect that using above-mentioned technical proposal：
Original not surface treated waste material, surface is impurity entirely, cannot be recycled at all.The use occurred in later industry is straight
Water receiving is washed, boiling, after high temperature evaporation ball blast waste material pretreatment mode, though waste utilization rate can be improved, adding proportion cannot
More, properties of product cannot be guaranteed.The present invention selects degreaser to deoil, then removes surface scale with pickle pickling, and increase
Vibration is added to grind off the pretreatment mode of deep layer oxide skin, the processing of neodymium iron boron magnetic body scraped surface is clean, it is added in the powder stage processed
A certain proportion of rare earth oxide improves magnet performance, and through die mould and ageing treatment, and the neodymium iron boron magnetic body of preparation is comprehensive
Can be suitable with original magnet performance, coercivity significantly improves.
Specific embodiment
It is described with reference to embodiment is further to the present invention.
Embodiment 1
A kind of method that sintered NdFeB band oil waste material recycles, including step successively as follows：
（1）It deoils, the layering of neodymium iron boron magnetic body waste material is positioned over the sodium hydroxide that ingredient is 5%, 8% sodium carbonate, 2% OP-
10, for surplus in the degreaser of water, and to be heated, 60 DEG C, time 2h of heating temperature, removal is attached to the part of scraped surface
Greasy dirt；
（2）Pickling, the neodymium iron boron magnetic body waste material layering after deoiling are positioned in a concentration of 5% nitric acid acidwashing liquid, pickling time
1h, the greasy dirt not removed completely in step of deoiling, and eliminate partial surface oxidation object；
（3）Abrasive material is vibrated, the complete neodymium iron boron magnetic body waste material of pickling is put into vibrating ball-mill, pours into abrasive material, abrasive material and waste material ratio
It is 1:1, abrasive material selection triangle abrasive material, the silicon carbide and 30% black corundum that the abrasive material proportioning is 70%, using disk vibration
Machine, vibration frequency 40HZ, time 1h grind off deep layer oxide skin；
（4）It rinses, the neodymium iron boron magnetic body waste material of step 3 is rinsed with giant；
（5）Drying, is dried using baking oven, and oven temperature is 100 DEG C, time 1h；
（6）Hydrogen is broken, and broken using the broken hydrogen that carries out of hydrogen crushing furnace hydrogen, wasted powder size is 150 mesh after hydrogen is broken, then carries out Dehydroepiandrosterone derivative,
Desorption temperature is 550 DEG C, time 5h；
（7）Dispensing adds in 5% Gd2O3Wherein the content of Gd is mixed for 80% weight and waste material, while adds 0.1%
Antioxidant and 0.1% lubricant；
（8）Milling and mixed powder carry out airflow milling milling to dispensing using not passivation technology, make powder particles at 3 μm.It is adopted after milling
Mixed powder is carried out with three-dimensional blender machine equipment, adds lubricant；
（9）Die mould and sintering, powder is pressed into the magnet that specification is 52mm*52mm*27mm by moulding press, then by green compact
It is put into vacuum sintering furnace and is sintered, 1035 DEG C of sintering temperature, time 5h obtains Nd-Fe-B magnet steel；
（10）Ageing treatment, the Nd-Fe-B magnet steel that die mould is obtained carry out two sections of ageing treatments, and aging technique is 900 DEG C of * 2h,
490℃*4h。
Nd-Fe-B magnet steel obtained is according to 3217 permanent magnetism of GB/T（Hard Magnetic）Magnetism of material test method is detected, and is measured
Performance indicator with a collection of waste material the waste material pretreating process of ball blast and original magnet performance after high temperature evaporation with being compared, such as
Shown in table 1：
Table 1
In table 1,1 performance of embodiment reaches the 35H trades mark, and all indicators are better than the waste material by ball blast after high temperature evaporation is pre-
Treatment process, the present embodiment magnet performance are suitable with original magnet performance.
The present embodiment is deoiled using the degreaser of special composition, the pretreatment mode of pickling and vibromill oxide skin, will
The processing of neodymium iron boron magnetic body scraped surface is clean, compared to the waste material pretreatment mode of ball blast after high temperature evaporation, present invention surface treatment
It is cleaner, while increase a certain proportion of rare earth oxide and carry out powder processed and sintering and ageing treatment, the present invention oily waste material to band
Reprocessing, the neodymium iron boron magnetic body comprehensive performance of preparation accordingly improve.
Embodiment 2
A kind of method that sintered NdFeB band oil waste material recycles, including step successively as follows：
（1）Deoil, by the layering of neodymium iron boron magnetic body waste material be positioned over the sodium hydroxide that ingredient is 6%, 10% sodium carbonate, 2%
OP-10, for surplus in the degreaser of water, and to be heated, 60 DEG C, 2 ~ 3h of time of heating temperature, removal is attached to scraped surface
Part greasy dirt；
（2）Pickling, the neodymium iron boron magnetic body waste material layering after deoiling are positioned in a concentration of 8% nitric acid acidwashing liquid, pickling time
1.5h, the greasy dirt that step of deoiling does not remove completely, and eliminate partial surface oxidation object；
（3）Abrasive material is vibrated, the complete neodymium iron boron magnetic body waste material of pickling is put into vibrating ball-mill, pours into abrasive material, abrasive material and waste material ratio
It is 1:2, abrasive material selection triangle abrasive material, the silicon carbide and 35% black corundum that the abrasive material proportioning is 65%, using disk vibration
Machine, vibration frequency 50HZ, time 1.5h grind off deep layer oxide skin；
（4）It rinses, the neodymium iron boron magnetic body of step 3 is rinsed with giant；
（5）Drying, oven temperature are 100 DEG C, time 1.5h；
（6）Hydrogen is broken, and professional hydrogen is broken because waste material produces, and desorption temperature is 565 DEG C, time 4h；
（7）Dispensing adds in 6% Gd2O3Wherein Gd contents are mixed for 75% weight and waste material, while addition 0.1% is anti-
Oxidant and 0.1% lubricant；
（8）Milling and mixed powder carry out airflow milling milling to dispensing using not passivation technology, make powder particles at 2.7 μm.After milling
Mixed powder is carried out using three-dimensional blender machine equipment, adds lubricant；
（9）Die mould and sintering, powder is pressed into the magnet that specification is 52mm*52mm*27mm by moulding press, then by green compact
It is put into vacuum sintering furnace and is sintered, 1030 DEG C of sintering temperature, time 4.5h obtains Nd-Fe-B magnet steel；
（10）Ageing treatment, the Nd-Fe-B magnet steel that die mould is obtained carry out two sections of ageing treatments, aging technique 900*2h, 490*
4h。
Nd-Fe-B magnet steel obtained is according to 3217 permanent magnetism of GB/T（Hard Magnetic）Magnetism of material test method is detected, and is measured
Performance indicator with a collection of waste material pretreating process and original magnet performance of the waste material through directly washing with being compared, such as 2 institute of table
Show：
Table 2
In table 2,2 performance of embodiment reaches the 35H trades mark, and all indicators are better than the waste material pretreating process being directly washed with water
The magnet of acquisition, the present embodiment magnet performance is suitable with original magnet performance, and particularly coercivity significantly improves.
The present embodiment is deoiled using the degreaser of special composition, the pretreatment mode of pickling and vibromill oxide skin, will
The processing of neodymium iron boron magnetic body scraped surface is clean, compared to the waste material pretreatment mode of ball blast after high temperature evaporation, present invention surface treatment
It is cleaner, while increase a certain proportion of rare earth oxide and carry out powder processed and sintering and ageing treatment, the present invention oily waste material to band
Reprocessing, the neodymium iron boron magnetic body comprehensive performance of preparation accordingly improve.
Claims (9)
1. a kind of method that sintered NdFeB band oil waste material recycles, feature include the following steps：
（1）It deoils, neodymium iron boron magnetic body waste material is positioned in the degreaser being configured, heat, 50 ~ 60 DEG C of heating temperature, the time 2
~ 3h, removal are attached to the part greasy dirt of scraped surface；
（2）Pickling, the neodymium iron boron magnetic body waste material after deoiling are positioned in pickle, and pickling time 1-2h removes step of deoiling
The greasy dirt that does not remove completely simultaneously eliminates partial surface oxidation object；
（3）Abrasive material is vibrated, the neodymium iron boron magnetic body waste material after pickling is put into vibrating ball-mill, pours into abrasive material, vibration frequency 40-
60HZ, time are 1-2 h, grind off deep layer oxide skin；
（4）It rinses, the waste material giant of the neodymium iron boron magnetic body after abrasive material is rinsed；
（5）Drying, oven temperature are 100-120 DEG C, time 1-2h；
（6）Hydrogen is broken, and waste material hydrogen is broken into -200 mesh powder of 150 mesh, and Dehydroepiandrosterone derivative, and desorption temperature is 550-580 DEG C, the time
5-6 h（Normal 600 ~ 610 DEG C of desorption temperature）；
（7）Dispensing, the rare earth oxide and waste material for adding in 5-7% weight are mixed, while add antioxidant and lubricant；
（8）Airflow milling is milled, and powder particles is controlled, mixed powder is carried out at 2.7 ~ 3.2 μm, after milling, add lubricant；
（9）Powder is pressed into the specification of needs by moulding press, and then green compact are put into vacuum sintering furnace and are sintered, sintering temperature
1020-1040 DEG C of degree, time 4-5h obtains Nd-Fe-B magnet steel；
（10）The Nd-Fe-B magnet steel that die mould is obtained carries out two sections of ageing treatments, and aging technique is 880-900 DEG C of * 1.5-3h,
The content of 450-500 DEG C of * 3.5-5h, heavy rare earth Dy or Tb present in magnet thickness direction and arrive the high period again from high to low
Property distribution.
2. the method that sintered NdFeB band oil waste material recycles according to claim 1, it is characterized in that the rare earth oxide
For Gd2O3Wherein Gd contents are 75% ~ 80% weight.
3. the method that sintered NdFeB band oil waste material recycles according to claim 1, it is characterized in that the degreaser ingredient
The sodium hydroxide for 2-8% is matched, the sodium carbonate of 3-10%, the OP-10 of 1-5%, surplus is water.
4. the method that sintered NdFeB band oil waste material recycles according to claim 1, it is characterized in that the pickle concentration
Nitric acid for 5-8%.
5. the method that sintered NdFeB band oil waste material recycles according to claim 1, it is characterized in that the vibrating ball-mill is circle
Disk vibrating ball-mill.
6. the method that sintered NdFeB band oil waste material recycles according to claim 1, it is characterized in that the abrasive material and neodymium iron
Boron magnet waste material ratio is 1:1-1:2.
7. the method that sintered NdFeB band oil waste material recycles according to claim 1, it is characterized in that the abrasive material is spherical shape
Or triangle abrasive material, preferably with triangle abrasive material, the abrasive material proportioning is the silicon carbide of 60-70% and the black corundum of 30-40%.
8. according to claim 1 sintered NdFeB band oil waste material recycle method, it is characterized in that the antioxidant by
Hydroxyl phenol and gasoline mixing composition, the antioxidant additive amount are the 0.05%-0.2% of dispensing total weight.
9. the method that sintered NdFeB band oil waste material recycles according to claim 1, it is characterized in that the lubricant is by hard
Resin acid barium, stearic acid sodium lactate, ammonium persulfate and paraffin composition, the lubricant additive amount are the 0.05%- of dispensing total weight
0.2%。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109003798A (en) * | 2018-07-06 | 2018-12-14 | 杭州永磁集团振泽磁业有限公司 | A kind of sintered NdFeB mixes the recycling and reusing method of waste material |
| CN109551357A (en) * | 2018-11-09 | 2019-04-02 | 包头中科泰磁涂层科技有限责任公司 | One kind being used for the ironing surface derusting method of small size magnetic |
| CN110480020A (en) * | 2019-09-12 | 2019-11-22 | 山东上达稀土材料有限公司 | A kind of method that sintered NdFeB waste material recycles |
| CN112791765A (en) * | 2020-12-04 | 2021-05-14 | 横店集团东磁股份有限公司 | Bonded neodymium iron boron magnet recycling method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109003798A (en) * | 2018-07-06 | 2018-12-14 | 杭州永磁集团振泽磁业有限公司 | A kind of sintered NdFeB mixes the recycling and reusing method of waste material |
| CN109003798B (en) * | 2018-07-06 | 2020-12-01 | 杭州永磁集团振泽磁业有限公司 | Recycling method of sintered neodymium iron boron mixed waste |
| CN109551357A (en) * | 2018-11-09 | 2019-04-02 | 包头中科泰磁涂层科技有限责任公司 | One kind being used for the ironing surface derusting method of small size magnetic |
| CN110480020A (en) * | 2019-09-12 | 2019-11-22 | 山东上达稀土材料有限公司 | A kind of method that sintered NdFeB waste material recycles |
| CN112791765A (en) * | 2020-12-04 | 2021-05-14 | 横店集团东磁股份有限公司 | Bonded neodymium iron boron magnet recycling method |
| CN112791765B (en) * | 2020-12-04 | 2022-05-20 | 横店集团东磁股份有限公司 | Recycling method of bonded neodymium iron boron magnet |
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