CN103426579B - A kind of reuse method of nickel plating sintered NdFeB waste material - Google Patents
A kind of reuse method of nickel plating sintered NdFeB waste material Download PDFInfo
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Abstract
A kind of reuse method of nickel plating sintered NdFeB waste material, crushing material becomes the powder of below 3mm particle diameter, sieve in the nitrogen box of sealing, remove most of nickel coating tablet, rare earth hydride is added in the powder sieved, after stirring, airflow milling is adopted preparation to be become 3-5 μm of fine powder, get appropriate powder pressing shaping, sintered sample carries out Performance Detection, testing result and properties of product requirement per sample, adds 0-60wt% trade mark powder of being correlated with and stirs, qualified powder pressing forming and sintering is become neodymium iron boron magnetic body.Do not need through roasting and melting again to the recycling of nickel plating sintered NdFeB waste material, only sieve after broken process, add rare earth hydride and carry out powder process, after first pilot sample detects its performance, then according to the properties of product requirement that will produce, add a certain amount of relevant trade mark powder, the sintered NdFeB product of various different performance requirement can be produced, technical process is simple, has both improved NdFeB material and rare earth material utilance, and has been conducive to energy-conserving and environment-protective again.
Description
Technical field
The present invention relates to neodymium iron boron waste material reuse method, especially a kind of reuse method of nickel plating sintered NdFeB waste material.
Background technology
Its anti-corrosion capability need be improved by surface treatment methods such as plating, applications usually in the surface of sintered NdFeB finished product.Nickel plating is a kind of surface treatment method comparatively commonly used.Nickel plating sintered NdFeB waste material how is effectively utilized to be a difficult problem.CN103117143A has announced a kind of neodymium iron boron magnetic body of neodymium iron boron nickel plating waste material sintering, the compound that it is formed by neodymium iron boron nickel plating waste material and rich rare earth formulation is prepared from by sintering process, and its preparation method is: roasting neodymium iron boron nickel plating waste material; Prepare neodymium iron boron nickel plating waste powder; Preparation compound; Compressing; Sintering.This method has the following disadvantages: (1) nickel plating waste material recycling needs in sintering furnace, roasting neodymium iron boron nickel plating waste material under nitrogen protection, consuming time, power consumption; (2) the nickel plating neodymium iron boron waste material after roasting needs to put into vacuum melting furnace melting again, the then broken use of hydrogen, consuming time, power consumption." research of sintering type Nd iron boron nickel coating stripping technique " literary composition gives the more preferably method of electrolytic removal nickel coating, by strip part being sent back to nickel plating again in former coating bath again after strip.But the method also exists the problem such as matrix corrosion, environmental pollution, and it is applicable to the underproof product of coating, is not suitable for the recycling of the scrap products that nickel plating finished product causes because unfilled corner, magnetic property are defective etc.Therefore the reuse method of nickel plating sintered NdFeB waste material also needs further improvement.
Summary of the invention
The present invention be directed to the above-mentioned state of the art and the reuse method of the nickel plating sintered NdFeB waste material that a kind of technique is simple, energy conservation, stock utilization are high, be convenient to scheduling of production is provided.
Technical scheme of the present invention is: a kind of reuse method of nickel plating sintered NdFeB waste material, and its step comprises:
A, first adopt jaw crusher coarse crushing to become the particle of below 25mm in nickel plating sintered NdFeB waste material, then with intermediate crusher, crushing material is become the powder of below 3mm particle diameter;
B, by powder sealing nitrogen glove box in use 30-60 mesh sieve sieve, remove most of nickel coating tablet;
Add the rare earth hydride of 2wt%-10wt% in c, powder after sieving through b step, stirs 1-3 hours, then preparation is become the fine powder of 3-5 μm by employing airflow milling, then adds 1wt ‰-5wt ‰ powder process additive, then stirs 1-3 hour;
D, get and walk through c the powder pressing forming and sintering made in right amount, neodymium iron boron magnetic body sample will be made and carry out Performance Detection;
E, walk the performance requirement of properties of sample testing result and product according to d, add the relevant trade mark powder of 0-60wt%, then add 1wt ‰-5wt ‰ powder process additive, stirring 1-3 hour, makes uniform composition;
F, by walk through e the powder pressing made shaping, sintering, make neodymium iron boron magnetic body.
Rare earth hydride can be chosen as praseodymium hydride neodymium or hydrogenation gadolinium iron; The amount detection of neodymium iron boron magnetic body sample is 5-20; The relevant trade mark that relevant trade mark powder can be produced for existing common process, as N30,30M, 30H, 30SH, 30UH, 30EH, 30AH and the similar trade mark.
Powder process additive comprises gasoline and protection against oxidation agent, and the mass ratio of gasoline and protection against oxidation agent is 5:2, and protection against oxidation agent is poly(ethylene oxide) allyl ether or poly(ethylene oxide) allyl glycidyl ether.
The invention has the beneficial effects as follows: do not need to carry out roasting and melting again to the recycling of nickel plating sintered NdFeB, only need sieve after broken process, then add rare earth hydride and carry out powder process, when expecting to produce low-coercivity high energy product product, rare earth hydride adding proportion controls by a small amount of; When producing the low magnetic energy product product of high-coercive force, the ratio that rare earth hydride adds increases in right amount.Whole technical process is simple, has significantly saved energy consumption and man-hour.The nickel plating sintered NdFeB garbage collection of the different trade mark can also recycle by the present invention together, after first manufacturing experimently its performance of several sample detection, again according to the properties of product requirement that will produce, add the powder of other trade mark a certain amount of, the sintered NdFeB product of various different performance requirement can be produced, waste utilization rate is high, is conducive to scheduling of production.
Accompanying drawing explanation
The process route chart of the reuse method of Fig. 1, nickel plating sintered NdFeB waste material.
Embodiment
Embodiment one
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, then with intermediate crusher, crushing material is become the powder of below 3mm particle diameter, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the praseodymium hydride neodymium of 2wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block neodymium iron boron magnetic body sample, carry out Performance Detection, test data is: Br:12.8-13.2KGS, Hcb:11.8-12.5KOe, Hcj:14.2-15.3KOe, (BH) max:40.5-43.0MGOe, according to
gB/T13560-2000 judges that its performance meets the performance requirement of the 42M trade mark, and this batch of powder may be used for batch production 42M trade mark product.
Embodiment two
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, then with intermediate crusher, crushing material is become the powder of below 3mm particle diameter, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the hydrogenation gadolinium iron of 2wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:12.2-12.6KGS, Hcb:11.5-12.2KOe, Hcj:13.4-14.7KOe, (BH) max:36.7-38.4MGOe, according to
gB/T13560-2000 judges that its performance meets the performance requirement of the N38 trade mark, and this batch of powder may be used for batch production N38 trade mark product.
Embodiment three
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, then with intermediate crusher, crushing material is become the powder of below 3mm particle diameter, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the praseodymium hydride neodymium of 3wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:12.6-12.9KGS, Hcb:11.5-12.2KOe, Hcj:14.8-16.1KOe, (BH) max:38.8-41.3MGOe, according to
gB/T13560-2000 judges that its performance meets the performance requirement of the 40M trade mark, and this batch of powder may be used for batch production 40M trade mark product.
Embodiment four
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, then with intermediate crusher, crushing material is become the powder of below 3mm particle diameter, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the praseodymium hydride neodymium of 5wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:12.2-12.6KGS, Hcb:11.3-11.8KOe, Hcj:17.6-18.5KOe, (BH) max:36.7-38.6MGOe, according to
gB/T13560-2000 judges that its performance meets the performance requirement of the 38H trade mark, and this batch of powder may be used for batch production 38H trade mark product.
Embodiment five
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, then with intermediate crusher, crushing material is become the powder of below 3mm particle diameter, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the praseodymium hydride neodymium of 10wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:11.8-12.2KGS, Hcb:10.8-11.3KOe, Hcj:17.3-18.0KOe, (BH) max:34.2-36.5MGOe, according to
gB/T13560-2000 judges that its performance meets the performance requirement of the 35H trade mark, and this batch of powder may be used for batch production 35H trade mark product.
Embodiment six
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, re-use the powder that crushing material is become below 3mm particle diameter by intermediate crusher, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the praseodymium hydride neodymium of 4wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:12.5-12.8KGS, Hcb:11.7-12.3KOe, Hcj:13.4-13.9KOe, (BH) max:38.2-40.3MGOe, there are the order 40M trade mark and 40SH trade mark powder in existing enterprise, according to
gB/T13560-2000 judges, final products performance is made to meet the performance requirement of the 40M trade mark, in powder, adding the 40SH trade mark of 10wt%, (performance data is Br:12.6-12.8KGS, Hcb:11.5-12.3KOe, Hcj:21.0-22.5KOe, (BH) max:38.8-40.8MGOe) powder, stir 1-3 hour, 1wt ‰-5wt ‰ powder process additive is added before stirring, after powder fully mixes, be pressed mass, sintering, properties of product after testing, test data is Br:12.6-12.8KGS, Hcb:11.8-12.4KOe, Hcj:14.2-14.8KOe, (BH) max:38.8-40.4MGOe.
Embodiment seven
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, re-use the powder that crushing material is become below 3mm particle diameter by intermediate crusher, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the praseodymium hydride neodymium of 6wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:12.0-12.4KGS, Hcb:11.2-11.8KOe, Hcj:17.3-17.9KOe, (BH) max:35.8-37.2MGOe, there are the order 35SH trade mark and 30AH trade mark powder in existing enterprise, according to
gB/T13560-2000 judges, final products performance is made to meet the performance requirement of the 35SH trade mark, in powder, adding the 30AH trade mark of 20wt%, (performance data is Br:10.8-11.3KGS, Hcb:10.2-10.6KOe, Hcj:35.5-36.5KOe, (BH) max:28.9-30.7MGOe) powder, stir 1-3 hour, 1wt ‰-5wt ‰ powder process additive is added before stirring, after powder fully mixes, be pressed mass, sintering, properties of product after testing, test data is: Br:11.8-12.1KGS, Hcb:10.4-11.0KOe, Hcj:20.1-20.9KOe, (BH) max:33.8-35.4MGOe.
Embodiment eight
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, re-use the powder that crushing material is become below 3mm particle diameter by intermediate crusher, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the hydrogenation gadolinium iron of 5wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:11.8-12.1KGS, Hcb:11.1-11.3KOe, Hcj:13.5-14.7KOe, (BH) max:35.1-36.0MGOe, there are the order 35H trade mark and 35UH trade mark powder in existing enterprise, according to
gB/T13560-2000 judges, final products performance is made to meet the performance requirement of the 35H trade mark, in powder, adding the 35UH trade mark of 40wt%, (performance data is Br:11.8-12.0KGS, Hcb:11.2-11.5KOe, Hcj:25.8-26.8KOe, (BH) max:34.0-35.2MGOe) powder, stir 1-3 hour, 1wt ‰-5wt ‰ powder process additive is added before stirring, after powder fully mixes, be pressed mass, sintering, properties of product after testing, test data is: Br:11.8-12.0KGS, Hcb:11.3-11.8KOe, Hcj:18.3-19.0KOe, (BH) max:34.3-35.5MGOe, reach 35H trade mark performance standard.
Embodiment nine
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, re-use the powder that crushing material is become below 3mm particle diameter by intermediate crusher, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the hydrogenation gadolinium iron of 2wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:12.2-12.6KGS, Hcb:11.5-12.2KOe, Hcj:13.4-14.7KOe, (BH) max:36.7-38.4MGOe, there are the order 38M trade mark and 38H trade mark powder in existing enterprise, according to
gB/T13560-2000 judges, final products performance is made to meet the performance requirement of the 38M trade mark, in powder, adding the 38H trade mark of 50wt%, (performance data is Br:12.3-12.5KGS, Hcb:11.7-12.0KOe, Hcj:17.8-18.5KOe, (BH) max:37.0-38.2MGOe) powder, stir 1-3 hour, 1wt ‰-5wt ‰ powder process additive is added before stirring, after powder fully mixes, be pressed mass, sintering, properties of product after testing, test data is: Br:12.3-12.5KGS, Hcb:11.6-11.9KOe, Hcj:15.0-16.3KOe, (BH) max:36.9-38.0MGOe, reach the performance standard of the 38M trade mark.
Embodiment ten
Adopt jaw crusher the nickel plating sintered NdFeB waste material coarse crushing of collection to be become the particle of below 25mm, re-use the powder that crushing material is become below 3mm particle diameter by intermediate crusher, nickel coating is peeled off from sheet neodymium iron boron matrix;
Then in the nitrogen glove box of sealing, use 30-60 mesh sieve to sieve powder, remove most of nickel coating tablet;
Add the hydrogenation gadolinium iron of 6wt% in powder after sizing, stir 1-3 hour, make uniform composition, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, again stir 1-3 hour, before each stirring, add 1wt ‰-5wt ‰ powder process additive;
Powder is after stirring fully mixing, get appropriate powder to be pressed, to sinter, make 5-20 block 52 × 52 × 27 size Nd-Fe-B magnets sample, carry out Performance Detection, test data is: Br:11.8-12.1KGS, Hcb:11.1-11.3KOe, Hcj:13.4-14.5KOe, (BH) max:35.1-36.0MGOe, there are the order N42 trade mark and N48 trade mark powder in existing enterprise, according to
gB/T13560-2000 judges, final products performance is made to meet the performance requirement of the N42 trade mark, through designing the N48 trade mark adding 60wt% in powder, (performance data is Br:13.8-13.9KGS, Hcb:12.5-12.6KOe, Hcj:12.8-13.5KOe, (BH) max:47.1-47.9MGOe) powder, stir 1-3 hour, 1wt ‰-5wt ‰ powder process additive is added before stirring, after powder fully mixes, be pressed mass, sintering, properties of product after testing, test data is: Br:12.9-13.1KGS, Hcb:12.2-12.6KOe, Hcj:12.9-13.6KOe, (BH) max:41.2-42.6MGOe, reach the performance standard of the N42 trade mark.
Claims (5)
1. a kind of reuse method of nickel plating sintered NdFeB waste material, its feature comprises the following steps:
A, first adopt jaw crusher coarse crushing to become the particle of below 25mm in nickel plating sintered NdFeB waste material, then with intermediate crusher, crushing material is become the powder of below 3mm particle diameter;
B, by powder sealing nitrogen glove box in use 30-60 mesh sieve sieve, remove most of nickel coating tablet;
Praseodymium hydride neodymium or the hydrogenation gadolinium iron rare earth hydride of 2wt%-10wt% is added in c, powder after sieving through b step, stir 1-3 hours, then adopt airflow milling preparation to be become the fine powder of 3-5 μm, then add 1wt ‰-5wt ‰ powder process additive, then stir 1-3 hour;
D, get and walk through c the powder pressing forming and sintering made in right amount, neodymium iron boron magnetic body sample will be made and carry out Performance Detection;
E, walk the performance requirement of properties of sample testing result and product according to d, add the relevant trade mark powder of 0-60wt%, then add 1wt ‰-5wt ‰ powder process additive, stirring 1-3 hour, makes uniform composition;
F, by walk through e the powder pressing made shaping, sintering, make neodymium iron boron magnetic body.
2. a kind of reuse method of nickel plating sintered NdFeB waste material according to claim 1, is characterized in that described praseodymium hydride neodymium addition is 2-6wt%.
3. a kind of reuse method of nickel plating sintered NdFeB waste material according to claim 1, is characterized in that described hydrogenation gadolinium iron addition is 2-6wt%.
4. a kind of reuse method of nickel plating sintered NdFeB waste material according to claim 1, it is characterized in that powder process additive comprises gasoline and protection against oxidation agent, the mass ratio of described gasoline and protection against oxidation agent is 5:2.
5. a kind of reuse method of nickel plating sintered NdFeB waste material according to claim 4, is characterized in that described protection against oxidation agent is poly(ethylene oxide) allyl ether or poly(ethylene oxide) allyl glycidyl ether.
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| CN114686746A (en) * | 2022-04-27 | 2022-07-01 | 江苏晨朗电子集团有限公司 | Recycling method of nickel-plated sintered neodymium iron boron waste material |
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