CN106141163A - Molding neodymium iron boron waste recovery Application way - Google Patents
Molding neodymium iron boron waste recovery Application way Download PDFInfo
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- CN106141163A CN106141163A CN201510193474.7A CN201510193474A CN106141163A CN 106141163 A CN106141163 A CN 106141163A CN 201510193474 A CN201510193474 A CN 201510193474A CN 106141163 A CN106141163 A CN 106141163A
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Abstract
The invention provides one and can recycle neodymium iron boron waste material production end grade neodymium-iron-boron blank, solve the molding neodymium iron boron waste recovery Application way of waste of raw materials problem, it is intended to overcome neodymium iron boron waste material in prior art to be difficult to recycle, the problem causing waste of raw materials.It is included in heating, drying process in demagnetization kiln, and hydrogen tear is managed, and ICP detector detects, and liquid phase hydrogen breaks the step such as powder and antioxidant mixing, airflow milling fine grinding, molding, isostatic pressed, sintering and Ageing Treatment, obtains neodymium iron boron blank.There is advantages that (1) recycles molding neodymium iron boron waste-material-preparing card in one's hand neodymium iron boron product；(2) recycle neodymium iron boron waste material, reduce waste of raw materials；(3) production cost is effectively reduced.
Description
Technical field
The present invention relates to a kind of neodymium iron boron product production field.
Background technology
Due to technical limitations and the impact of uncontrollable factor, inevitable in the course of processing of neodymium iron boron product
Meeting produce a certain amount of waste material, including out-of-size blank, cracking blank, the blank etc. of damage,
This kind of waste material is difficult to directly use, and causes a large amount of raw-material waste.Along with carrying of neodymium iron boron product production capacity
Height, produces neodymium iron boron waste material and is also greatly increased, and processing neodymium iron boron waste material the most economically is that neodymium iron boron product is raw
The technical barrier of solution is needed in product field badly.
Summary of the invention
The present invention is to overcome neodymium iron boron waste material in prior art to be difficult to recycle, causing waste of raw materials
Problem, it is provided that one can recycle neodymium iron boron waste material produce end grade neodymium-iron-boron blank, solve former
The molding neodymium iron boron waste recovery Application way of waste of material problem.
For achieving the above object, the present invention is by the following technical solutions:
The present invention provides a kind of molding neodymium iron boron waste recovery Application way, comprises the following steps:
A, by molding neodymium iron boron waste material heating, drying in demagnetization kiln, heating-up temperature 380 450 DEG C, during process
A length of 4 hours, come out of the stove after cooling, sieve, obtain neodymium iron boron waste material；
B, the neodymium iron boron waste material obtaining step a carry out hydrogen tear reason, and suction hydrogen is after 35 hours, and heating is de-
Hydrogen temperature is 550 DEG C, dehydrogenation time 3.5 5.5 hours, and particle size after cracking is 0.1-0.8mm, crosses 100-200
Mesh sieve, obtains sieving the hybrid particles of decontamination；
C, the hybrid particles using ICP detector to obtain step b carry out in detection detection hybrid particles main
Content Pr, Nd, Dy, Tb, Ho, Gd, Ga, B, Fe, Al, Cu, Nb, Zr, Co of element；
D, in the hybrid particles that step b obtains, add the waste granules that step c obtained and break with liquid phase hydrogen
Powder and antioxidant mixing, mixing duration 4 hours, obtain mixed powder, the detection obtained according to step c
Result, the trade mark of molding neodymium iron boron waste material and properties of product requirement, in described mixed powder, liquid phase hydrogen breaks opaque
Amount accounting is 10%-30%, and antioxidant quality accounting is 1.0 ‰ 2 ‰, and remaining composition is waste granules；
Fine grinding in e, the compound that step c is obtained addition airflow milling, oxygen content ＜ 20ppm in described airflow milling system,
Rotating speed 2500-3000r/min, operating pressure 0.55-0.65MPa, preparing particle mean size is 3.2 3.6 μm
Mixing fine powders；
F, mixing fine powders step d obtained add molding in shaped device, after isostatic pressed, obtain neodymium iron boron
Pressed compact；
G, neodymium iron boron pressed compact shove charge step e obtained sintering, obtain neodymium iron boron blank.
In above-mentioned technique, a step is used for removing molding neodymium iron boron waste material magnetic, and by adding in heat abstraction waste material
Ground moisture makes greasy dirt carbonization simultaneously, removes the carbonization granule that degreases after sieving.In b step, neodymium iron boron is managed by hydrogen tear
And crush, and the material in other waste materials is unbroken, can sift out neodymium iron boron hybrid particles the most after sizing.
Testing result, the trade mark of molding neodymium iron boron waste material and the properties of product requirement obtained according to step c, adjusts hydrogen
After broken, the blended liquid phase hydrogen of neodymium iron boron hybrid particles sum breaks powder ratio, obtains mixing thin after airflow milling fine grinding
Powder.Be shaped by the mixing fine powders obtained, isostatic pressed and sintering circuit make neodymium iron boron blank again.Pass through
Above-mentioned technique can make full use of the molding neodymium iron boron waste-material-preparing of recovery and go out the neodymium iron boron hair that the low trade mark is serial
Base, thus the problem that effectively solution neodymium iron boron waste of raw materials and waste material are difficult to recycle.
As preferably, the antioxidant in step d is polyethylene oxide alkyl ethers or the bright base of poly(ethylene oxide) alkene
Ether.
As preferably, in step f, during molding, die cavity central point magnetic field intensity ＞ 1.4T, green density is
3.8—4.2g/cm3；Green density after isostatic pressed is 4.4 4.8g/cm3。
As preferably, in step g, sintering process is stagewise sintering, is provided with one before sintering temperature section
Or multiple insulation degassing stages, sintering stage temperature is between 1,065 1095 DEG C, and sintering stage temperature retention time is 4h
6.5h, applying argon gas or nitrogen after sintering, it is quickly cooled to less than 80 DEG C.
As preferably, described insulation degassing stages is 3 sections, and first paragraph insulation degassing stages holding temperature is 250 350
DEG C, during insulation a length of 0.5 1 hours, second segment insulation degassing stages holding temperature was 550 650 DEG C, insulation
Shi Changwei 1 1.5 hours, the 3rd section of insulation degassing stages holding temperature is 850 920 DEG C, during insulation a length of 3
5 hours.
As preferably, being additionally included in step f, neodymium iron boron blank step g obtained carries out Ageing Treatment, time
It is 880 920 DEG C that effect process is divided into one-level timeliness and secondary time effect, one-level aging temp, and temperature retention time is 2.5
3.5h, applying argon gas or nitrogen, be quickly cooled to less than 60 DEG C.Then upgrade and carry out secondary time effect, two grades
Aging temp is 480 530 DEG C, and temperature retention time is 3 5h, applying argon gas or nitrogen, is quickly cooled to 50 DEG C
Hereinafter come out of the stove.
As preferably, described liquid phase hydrogen breaks meal component and includes: rare earth 35 42%, Dy content 0 10%,
Tb content 0 5%, Ho content 0 10%, Gd content 0 10%, Co content 0 8%, Al content
0 2%, Cu content 0 0.8%, Nb content 0 0.5%, Zr content 0 0.1%, Ga content 0
0.4%, B content 0.93 1.05%, surplus is Fe.
High owing to reclaiming waste material oxygen content, rare earth is combined with oxygen and can not play a role, therefore need to add corresponding than
The liquid phase hydrogen of example breaks powder, increases total amount of rare earth.
Therefore, there is advantages that (1) recycles molding neodymium iron boron waste-material-preparing card in one's hand
Number neodymium iron boron product；(2) recycle neodymium iron boron waste material, reduce waste of raw materials；(3) life is effectively reduced
Produce cost.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described further.
Embodiment 1: first the molding neodymium iron boron waste material reclaimed is roughly selected, select the N series trade mark therein
Molding neodymium iron boron waste material.
By molding neodymium iron boron waste material heating, drying in demagnetization kiln, heating-up temperature 380 450 DEG C, handling duration
It is 4 hours, comes out of the stove after cooling, sieve, obtain neodymium iron boron waste material.
The neodymium iron boron waste material obtaining step a carries out hydrogen tear reason, inhales hydrogen after 35 hours, Heating Dehydrogenation temperature
Degree is 550 DEG C, dehydrogenation time 3.5 5.5 hours, and particle size after cracking is 0.1-0.8mm, crosses 100-200 mesh sieve,
Obtain sieving the hybrid particles of decontamination.
Use ICP detector that the hybrid particles obtained is detected, essential element in detection hybrid particles
Content Pr, Nd, Dy, Tb, Ho, Gd, Ga, B, Fe, Al, Cu, Nb, Zr, Co.
In the hybrid particles obtained, add liquid phase hydrogen and break powder and antioxidant mixing, a length of 4 little during mixing
Time, obtaining mixed powder, it is rare earth 35% that liquid phase hydrogen breaks the concrete composition of powder, and Fe is 65%.
In described mixed powder, liquid phase hydrogen breaks opaque amount accounting is 10%-20%；Antioxidant quality accounting is
1%-2%, remaining composition is waste granules.
Compound will be obtained and add fine grinding in airflow milling, oxygen content ＜ 20ppm, rotating speed in described airflow milling system
2500-3000r/min, operating pressure 0.55-0.65MPa, preparing particle mean size is the mixed of 3.2 3.6 μm
Close fine powder.
Mixing fine powders is added molding in shaped device, after isostatic pressed, obtains neodymium iron boron pressed compact.Neodymium iron boron pressure
Base shove charge sinters, and obtains neodymium iron boron blank.Sintering process is stagewise sintering, is provided with before sintering temperature section
Three insulation degassing stages, sintering stage temperature is between 1,065 1095 DEG C, and sintering stage temperature retention time is 4h
6.5h, applying argon gas or nitrogen after sintering, it is quickly cooled to less than 80 DEG C.
Described insulation degassing stages is 3 sections, and first paragraph insulation degassing stages holding temperature is 250 350 DEG C, insulation
Shi Changwei 0.5 1 hours, second segment insulation degassing stages holding temperature is 550 650 DEG C, during insulation a length of 1
1.5 hours, the 3rd section of insulation degassing stages holding temperature was 850 920 DEG C, during insulation a length of 35 hours.
The neodymium iron boron blank obtained is carried out Ageing Treatment.Described Ageing Treatment is divided into one-level timeliness and when two grades
Effect, one-level aging temp is 880 920 DEG C, and temperature retention time is 2.5 3.5h, applying argon gas or nitrogen, quickly
It is cooled to less than 60 DEG C.Then upgrading carries out secondary time effect, and secondary time effect temperature is 480 530 DEG C, insulation
Time is 3 5h, applying argon gas or nitrogen, is quickly cooled to less than 50 DEG C and comes out of the stove.
In the present embodiment, the test data of product are Br:10.8-14kGs, Hcb:10-10.5kOe, Hcj:
12-14kOe, (BH) max:28-49MGOe.
Embodiment 2: the present embodiment is first to carry out the molding neodymium iron boron waste material reclaimed with the difference of embodiment 1
Roughly select, select the molding neodymium iron boron waste material of the M series trade mark therein.It is dilute that liquid phase hydrogen breaks the concrete composition of powder
Soil 35 42%, Dy content 0 10%, Tb content 0 5%, Ho content 0 10%, Gd content 0
10%, Co content 0 8%, Al content 0 2%, Cu content 0 0.8%, Nb content 0 0.5%,
Zr content 0 0.1%, Ga content 0 0.4%, B content 0.93 1.05%, surplus is Fe.
In described mixed powder, liquid phase hydrogen breaks opaque amount accounting is 10%-20%.
In the present embodiment, the test data of product are Br:10.8-13.7kGs, Hcb:10-12.9kOe, Hcj:
14-17kOe, (BH) max:28-45MGOe.
Other are same as in Example 1, therefore omit.
Embodiment 3: the present embodiment is first to roughly select the molding neodymium iron boron waste material reclaimed with the difference of embodiment 1,
Select the molding neodymium iron boron waste material of the H series trade mark therein.It is rare earth 35 that liquid phase hydrogen breaks the concrete composition of powder
42%, Dy content 0 10%, Tb content 0 5%, Ho content 0 10%, Gd content 0 10%,
Co content 0 8%, Al content 0 2%, Cu content 0 0.8%, Nb content 0 0.5%, Zr content
0 0.1%, Ga content 0 0.4%, B content 0.93 1.05%, surplus is Fe.
In described mixed powder, liquid phase hydrogen breaks opaque amount accounting is 10%-25%.
In the present embodiment, the test data of product are Br:10.8-13.7kGs, Hcb:10-12.1kOe, Hcj:
17-20kOe, (BH) max:28-45MGOe.
Other are same as in Example 1, therefore omit.
Embodiment 4: the present embodiment is first to roughly select the molding neodymium iron boron waste material reclaimed with the difference of embodiment 1,
Select the molding neodymium iron boron waste material of the SH series trade mark therein.It is rare earth rare earth that liquid phase hydrogen breaks the concrete composition of powder
40%, Ho content 5%, Dy content 5%, Tb content 2.5%, Gd content 5%, Co content 4%, Al
Content 1%, Cu content 0.4%, Nb content 0.25%, Zr content 0.05%, Ga content 0.2%, B contains
Amount 1%, surplus is Fe.
In described mixed powder, liquid phase hydrogen breaks opaque amount accounting is 10%-25%.
In the present embodiment, the test data of product are Br:10.8-12.9kGs, Hcb:10.1-11.8kOe,
Hcj:20-25kOe, (BH) max:28-40MGOe.
Other are same as in Example 1, therefore omit.
Embodiment 5: the present embodiment is first to roughly select the molding neodymium iron boron waste material reclaimed with the difference of embodiment 1,
Select the molding neodymium iron boron waste material of the UH series trade mark therein.It is rare earth that liquid phase hydrogen breaks the concrete composition of powder
42%, Dy content 10%, Tb content 5%, Ho content 10%, Gd content 10%, Co content 8%,
Al content 2%, Cu content 0.8%, Nb content 0.5%, Zr content 0.1%, Ga content 0.4%, B
Content 1.05%, surplus is Fe.
In described mixed powder, liquid phase hydrogen breaks opaque amount accounting is 10%-30%.
In the present embodiment, the test data of product are Br:10.8-12.2kGs, Hcb:10.2-10.8kOe,
Hcj:25-30kOe, (BH) max:28-36MGOe.
Claims (7)
1. a molding neodymium iron boron waste recovery Application way, is characterized in that, comprises the following steps:
A, by molding neodymium iron boron waste material heating, drying in demagnetization kiln, heating-up temperature 380 450 DEG C, handling duration is 4 hours, comes out of the stove after cooling, sieves, and obtains neodymium iron boron waste material；
B, the neodymium iron boron waste material obtaining step a carry out hydrogen tear reason, and suction hydrogen is after 35 hours, and Heating Dehydrogenation temperature is 550 DEG C, dehydrogenation time 3.5 5.5 hours, and particle size after cracking is 0.1-0.8mm, crosses 100-200 mesh sieve, obtain sieving the hybrid particles of decontamination；
C, the hybrid particles using ICP detector to obtain step b carry out content Pr, Nd, Dy, Tb, Ho, Gd, Ga, B, Fe, Al, Cu, Nb, Zr, Co of essential element in detection detection hybrid particles；
D, in the hybrid particles that step b obtains, the waste granules that step c is obtained by addition breaks powder with liquid phase hydrogen and antioxidant mixes, mixing duration 4 hours, obtain mixed powder, testing result, the trade mark of molding neodymium iron boron waste material and the properties of product requirement obtained according to step c, in described mixed powder, liquid phase hydrogen breaks opaque amount accounting is 10%-30%, and antioxidant quality accounting is 1.0 ‰ 2 ‰, and remaining composition is waste granules；
E, compound step c obtained add fine grinding in airflow milling, oxygen content ＜ 20ppm, rotating speed 2500-3000r/min, operating pressure 0.55-0.65MPa in described airflow milling system, prepare the mixing fine powders that particle mean size is 3.2 3.6 μm；
F, mixing fine powders step d obtained add molding in shaped device, after isostatic pressed, obtain neodymium iron boron pressed compact；
G, neodymium iron boron pressed compact shove charge step e obtained sintering, obtain neodymium iron boron blank.
Molding neodymium iron boron waste recovery Application way the most according to claim 1, is characterized in that, the antioxidant in step d is polyethylene oxide alkyl ethers or poly(ethylene oxide) alkene bright base ether.
Molding neodymium iron boron waste recovery Application way the most according to claim 1, is characterized in that, in step f, during molding, die cavity central point magnetic field intensity ＞ 1.4T, green density is 3.8 4.2g/cm3；Green density after isostatic pressed is 4.4 4.8g/cm3。
Molding neodymium iron boron waste recovery Application way the most according to claim 1, it is characterized in that, in step g, sintering process is stagewise sintering, being provided with one or more insulation degassing stages before sintering temperature section, sintering stage temperature is between 1,065 1095 DEG C, and sintering stage temperature retention time is 4h 6.5h, applying argon gas or nitrogen after sintering, be quickly cooled to less than 80 DEG C.
Molding neodymium iron boron waste recovery Application way the most according to claim 3, it is characterized in that, described insulation degassing stages is 3 sections, first paragraph insulation degassing stages holding temperature is 250 350 DEG C, during insulation a length of 0.5 1 hours, second segment insulation degassing stages holding temperature was 550 650 DEG C, during insulation a length of 1 1.5 hours, 3rd section of insulation degassing stages holding temperature is 850 920 DEG C, during insulation a length of 35 hours.
6. according to the molding neodymium iron boron waste recovery Application way described in claim 1 or 2 or 3 or 4 or 5, it is characterized in that, it is additionally included in step f, neodymium iron boron blank step g obtained carries out Ageing Treatment, described Ageing Treatment is divided into one-level timeliness and secondary time effect, one-level aging temp to be 880 920 DEG C, and temperature retention time is 2.5 3.5h, applying argon gas or nitrogen, be quickly cooled to less than 60 DEG C.Then upgrading carries out secondary time effect, and secondary time effect temperature is 480 530 DEG C, and temperature retention time is 3 5h, applying argon gas or nitrogen, is quickly cooled to less than 50 DEG C and comes out of the stove.
Molding neodymium iron boron waste recovery Application way the most according to claim 1, is characterized in that, described liquid phase hydrogen breaks meal component and includes: rare earth 35 42%, Dy content 0 10%, Tb content 0 5%, Ho content 0 10%, Gd content 0 10%, Co content 0 8%, Al content 0 2%, Cu content 0 0.8%, Nb content 0 0.5%, Zr content 0 0.1%, Ga content 0 0.4%, B content 0.93 1.05%, surplus is Fe.
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Cited By (5)
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| CN107739949A (en) * | 2017-10-20 | 2018-02-27 | 江西金力永磁科技股份有限公司 | A kind of method of the rich phase alloy utilized for magnet scrap loop and waste and old magnet cycling and reutilization |
| CN109192486A (en) * | 2018-08-13 | 2019-01-11 | 湖南航天磁电有限责任公司 | A kind of recycling and reusing method of sintering and molding neodymium iron boron molding die cleaning materials |
| 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 |
| CN112216463A (en) * | 2020-09-29 | 2021-01-12 | 杭州电子科技大学 | Method for improving corrosion resistance of neodymium iron boron waste recovered magnet |
| RU2818933C1 (en) * | 2023-09-23 | 2024-05-07 | Федеральное государственное автономное образовательного учреждение высшего образования "Национальный исследовательский ядерный университет "МИФИ" | Method of producing a powder of an alloy based on a rare-earth metal from secondary magnetic materials based on a rare-earth metal-iron-boron system |
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| CN107739949A (en) * | 2017-10-20 | 2018-02-27 | 江西金力永磁科技股份有限公司 | A kind of method of the rich phase alloy utilized for magnet scrap loop and waste and old magnet cycling and reutilization |
| CN107739949B (en) * | 2017-10-20 | 2020-08-25 | 江西金力永磁科技股份有限公司 | Phase-rich alloy for recycling magnet waste and method for recycling waste magnet |
| CN109192486A (en) * | 2018-08-13 | 2019-01-11 | 湖南航天磁电有限责任公司 | A kind of recycling and reusing method of sintering and molding neodymium iron boron molding die cleaning materials |
| 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 |
| CN112216463A (en) * | 2020-09-29 | 2021-01-12 | 杭州电子科技大学 | Method for improving corrosion resistance of neodymium iron boron waste recovered magnet |
| RU2818933C1 (en) * | 2023-09-23 | 2024-05-07 | Федеральное государственное автономное образовательного учреждение высшего образования "Национальный исследовательский ядерный университет "МИФИ" | Method of producing a powder of an alloy based on a rare-earth metal from secondary magnetic materials based on a rare-earth metal-iron-boron system |
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Application publication date: 20161123 |