CN109400144A - A method of high performance magnet is prepared with wet pressing permanent-magnet ferrite reclaimed materials - Google Patents
A method of high performance magnet is prepared with wet pressing permanent-magnet ferrite reclaimed materials Download PDFInfo
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- CN109400144A CN109400144A CN201811322226.8A CN201811322226A CN109400144A CN 109400144 A CN109400144 A CN 109400144A CN 201811322226 A CN201811322226 A CN 201811322226A CN 109400144 A CN109400144 A CN 109400144A
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- 239000000463 material Substances 0.000 title claims abstract description 81
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000003825 pressing Methods 0.000 title claims abstract description 15
- 239000004615 ingredient Substances 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 239000000159 acid neutralizing agent Substances 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- 230000001133 acceleration Effects 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical group OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- -1 hydroxyl isomaltulose Chemical compound 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- AYRXSINWFIIFAE-SCLMCMATSA-N Isomaltose Natural products OC[C@H]1O[C@H](OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O)[C@@H](O)[C@@H](O)[C@@H]1O AYRXSINWFIIFAE-SCLMCMATSA-N 0.000 description 1
- LKDRXBCSQODPBY-AMVSKUEXSA-N L-(-)-Sorbose Chemical compound OCC1(O)OC[C@H](O)[C@@H](O)[C@@H]1O LKDRXBCSQODPBY-AMVSKUEXSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- DLRVVLDZNNYCBX-RTPHMHGBSA-N isomaltose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)C(O)O1 DLRVVLDZNNYCBX-RTPHMHGBSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012913 prioritisation Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
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- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
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Abstract
The invention discloses a kind of method for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials, operating procedure includes: (1) reclaimed materials comminution pretreatment, and (2) weigh ingredient, and (3) are once ground, (4) pre-burning, (5) secondary grinding, (6) sintering.The present invention is to pass through retrofit to reclaimed materials and increase pre-burning program again, so that the utilization rate of reclaimed materials greatly improves, solve in the prior art that permanent-magnet ferrite reclaimed materials utility value is low, is difficult to the most technical problem with permanent-magnet ferrite reclaimed materials material production high-performance permanent-magnet ferrite, realize recycling for permanent-magnet ferrite reclaimed materials material, turn waste into wealth, reclaimed materials utilization rate is improved, material cost is reduced, improves the cost performance of material.
Description
Technical field:
The present invention relates to technical field of magnetic materials, relate generally to a kind of prepare high-performance magnetism with wet pressing permanent-magnet ferrite reclaimed materials
The method of body.
Background technique:
The reclaimed materials of permanent ferrite wet pressure magnetic tile manufacturer, the country accounts for 40% or more of raw material input amount at present, permanent magnet oxygen
Body reclaimed materials includes: magnet steel powder, grinding material, molded blank or unformed ball milling material (un-sintered).The general processing side of reclaimed materials
Formula is divided into: mode 1, individually grinds, and degradation does the use of low performance product；Mode 2 is arranged in pairs or groups with Preburning material and is used；Mode 3, does not make
With selling at a low price.Mode 1 does low performance product, and material performance performance does not come out, and waste is serious；2 blend proportion of mode cannot
More than 20%, needing to degrade more than 20% raw material is used, and has special want to the original performance, ingredient, contraction etc. of reclaimed materials
It asks；Mode 3 causes very big cost pressure, wastage of material and causes environmental pollution.
Patent of invention number: although certain applications that CN201210038488.8 solves reclaimed materials production high performance magnet are asked
Topic, but reclaimed materials is low as auxiliary material investment ratio, major ingredient performance requirement height and magnetic property and elemental composition because of reclaimed materials
Unstability, main phase molecular formula is unstable, it is difficult to realize mass large-scale production.
It is domestic that the mentality of designing of preheating and direction again are carried out to reclaimed materials not yet, then pre-burning is present invention original creation,
By reasonable ingredient and pre-burning, the magnetic property of material can be given full play to, reaches Br >=4500Gs, Hcb >=4150Oe, Hcj >=
5400Oe, (BH) max >=4.9MGOe, squareness ratio Hk/Hcj >=0.93 are equivalent to the FB12H performance of Japanese TDK, reach international
Top standard.
Summary of the invention:
The object of the invention is exactly to mention in order to which the reclaimed materials utilization rate for solving the problems, such as permanent ferrite wet pressure magnetic tile manufacturer is low
For a kind of method that wet pressing permanent-magnet ferrite reclaimed materials prepares high performance magnet, the circulation of permanent-magnet ferrite reclaimed materials is realized
It utilizes, turns waste into wealth, reduce the production cost of material, improve economic benefit.
The present invention is achieved by the following technical solutions:
A method of high performance magnet is prepared with wet pressing permanent-magnet ferrite reclaimed materials, it is characterised in that: concrete operations include such as
Lower step:
(1) reclaimed materials comminution pretreatment
Rewinding 500g is fetched, water for ball milling Crushing of Ultrafine, water removal, broken sieving are carried out；
(2) ingredient is weighed
Weigh appropriate ingredient, wherein Fe2O3Powder 60~80g, CaCO3Powder 3~7g, La2O3Powder 3~4g, Co2O3Powder
0~1.5g, acceleration of sintering 1~2g of cosolvent, 1.5~8g of dispersing agent, 3~5g of acid-base neutralization agent；
(3) primary grinding
Reclaimed materials and ingredient are put into sand mill, and steel ball 12kg, 3.8~4kg of water is added, and carry out water for ball milling, water polo time consuming
For 1.5~3h, it is ground to 0.8~0.95 μm of slurry average particle size；
(4) pre-burning
It is dried being put by the material once ground in an oven, drying temperature is set as 200 DEG C, is crushed after drying, then puts
Enter and carries out pre-burning in Muffle furnace；
(5) secondary grinding
It is 3 μm that Preburning material, which is crushed to average particle size, takes Preburning material 500g, adds water 1000g, and secondary additive is added, secondary to add
Adding agent is SiO2Powder 0.5-1.5g, Bi2O3Powder 3-5g, D-sorbite 1-4g, HCOOH powder 0.5-2g, NH4HCO3Powder
Last 1-2g several combinations is put into ball grinder, grinds 15h, until average particle size is 0.81~0.85 μm；
(6) it is sintered
It is 60~65% by ground slurry precipitating or Direct Dehydration to pulp density, in the high magnetic field intensity of 120KA/M
Under, being pressed into density is 3.1~3.4g/cm3Regular magnet, the density that regular magnet is formed be 5.0~5.2g/cm3Magnetic
Body.
The water for ball milling Crushing of Ultrafine is that reclaimed materials is milled to average particle size less than 2.0 μm；The temperature for removing water is
150~800 DEG C, the water content for removing water to reclaimed materials is 1.0~1.2%；The aperture of the broken sieving selection standard sub-sieve
Below 60 mesh.
The acceleration of sintering cosolvent is SiO2, the dispersing agent is H3BO3, in D-sorbite and hydroxyl isomaltulose one
Kind or more, the acid-base neutralization agent is CH3COOH or NH4HCO3。
The temperature of pre-burning is 1200~1320 DEG C in the installation steps (4), and pre-burning soaking time is 60 ~ 200min.
Sintering temperature in the step (6) is 1200~1280 DEG C.
The additive amount of the metal oxide is not higher than the 20% of total 1 amount of material.
The total amount of adding of the dispersing agent and acid-base neutralization agent is not higher than the 5% of material total amount.
The beneficial effect comprise that
1, the present invention is to pass through retrofit to reclaimed materials and increase pre-burning program again, so that the utilization rate of reclaimed materials substantially mentions
It is high.The present invention solves in the prior art that permanent-magnet ferrite reclaimed materials utility value is low, is difficult to most permanent-magnet ferrite reclaimed materials
Material produces the technical problem of high-performance permanent-magnet ferrite, realizes recycling for permanent-magnet ferrite reclaimed materials material, becomes useless
For treasured, reclaimed materials utilization rate is improved, material cost is reduced, improves the cost performance of material.
2, mentality of designing and the direction that the present invention has initiated again preheating can be abundant by reasonable ingredient and pre-burning
The magnetic property for playing material, reaches Br >=4500Gs, Hcb >=4150Oe, Hcj >=5400Oe, (BH) max >=4.9MGOe, rectangle
Than Hk/Hcj >=0.93, it is equivalent to the FB12H performance of Japanese TDK, is reached the international leading level.
3, ingredient total addition level is economical and practical less than 20%.
4, the dispersing agent in prioritization scheme and acid-base neutralization agent total amount of adding are lower than 5%, and slurry is viscous when can reduce grinding
Property, reach abundant mixing, and reduce milling time, lower calcined temperature, solid phase reaction can be obtained in a pre-burning
Sufficiently, high magnetic characteristics are obtained.
Specific embodiment:
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, the present invention is carried out
It is further described.It should be appreciated that the specific embodiments described herein are only used to explain the present invention, it is not used to limit
The fixed present invention.
Embodiment 1:
A method of high performance magnet being prepared with wet pressing permanent-magnet ferrite reclaimed materials, specific steps are as follows:
(1) reclaimed materials comminution pretreatment
It fetches rewinding 500g and carries out water for ball milling Crushing of Ultrafine, it is 1.0% that moisture content is dried at 800 DEG C, and sieving is crushed after drying, is broken
The aperture for the standard sub-sieve that broken sieving is selected is 60 mesh.
(2) ingredient is weighed
Weigh appropriate ingredient, wherein Fe2O3Powder 80g, CaCO3Powder 3g, La2O3Powder 4g, Co2O3Powder 1.5g, SiO2
Powder 1g, D-sorbite 1.5g, NH4HCO3Powder 5g.
(3) primary grinding
It weighs up reclaimed materials 500g and appropriate ingredient is put into sand mill, steel ball 12kg, water 3.8kg is added, carry out water for ball milling, water
Ball-milling Time is 3h, 0.8 μm of mill base slurry average particle size.
(4) pre-burning
It will put by an abrasive and dry in an oven, drying temperature is set as 200 DEG C, is crushed after drying, is then placed in horse
Not furnace is pre-sintered, and calcined temperature sets 1200 DEG C, keeps the temperature 200min.
(5) secondary grinding
Preburning material is 3 μm by shaking pulverizer to be crushed to average particle size, takes Preburning material 500g, adds water 1000g, secondary add is added
Add agent: SiO2Powder 1g, D-sorbite 1.5g, HCOOH powder 0.5g are put into ball grinder, 15h are ground, until average particle size is
0.85μm；
(6) it is sintered
It is 60% by ground slurry precipitating or Direct Dehydration to pulp density, under the high magnetic field intensity of 120KA/M, pressure
It is 3.1g/cm that density, which is made,3Regular magnet, the density that regular magnet is burnt at a temperature of 1280 DEG C be 5.0g/cm3Magnetic
Body.
The high-performance permanent-magnet ferrite that the present embodiment obtains, Br:4500Gs, Hcb:4150Oe, Hcj:5400Oe, (BH)
Max:4.9MGOe, squareness ratio Hk/Hcj:0.93.
Embodiment 2:
A method of high performance magnet being prepared with wet pressing permanent-magnet ferrite reclaimed materials, specific steps are as follows:
(1) reclaimed materials comminution pretreatment
It fetches rewinding 500g and carries out water for ball milling Crushing of Ultrafine, it is 1.2% that moisture content is dried at 150 DEG C, and sieving is crushed after drying；
(2) ingredient is weighed
Weigh appropriate ingredient, wherein Fe2O3Powder 60g, CaCO3Powder 7g, La2O3Powder 3g, SiO2Powder 2g, isomaltose
Alcohol 6g, H3BO3Powder 2g, CH3COOH3g.
(3) primary grinding
Reclaimed materials 500g and appropriate ingredient after sieving, which are put into sand mill, to carry out, and steel ball 12kg, water 4kg is added, and carries out water
Ball milling, water polo time consuming be 1.5h, 0.95 μm of mill base slurry average particle size.
(4) pre-burning
Blended stock after once grinding is subjected to pre-burning, calcined temperature sets 1320 DEG C, keeps the temperature 60min.
(5) secondary grinding
It is 3 μm that Preburning material, which is crushed to average particle size, takes Preburning material 500g, adds water 1000g, Bi is added2O3Powder 4g, sorbose
Alcohol 3g, NH4HCO3Powder 1g, is incorporated in ball grinder, grinds 15h, until average particle size is 0.81 μm；
(6) it is sintered
It is 65% by ground powder precipitation or Direct Dehydration to pulp density, in the high magnetic field intensity for being greater than 120KA/M
Under, being pressed into density is 3.4g/cm3Regular magnet, the density that regular magnet is burnt at a temperature of 1200 DEG C be 5.2g/cm3
Magnet.
The high-performance permanent-magnet ferrite that the present embodiment obtains, Br:4550Gs, Hcb:4210Oe, Hcj:5400Oe, (BH)
Max:4.95MGOe, squareness ratio Hk/Hcj:0.94.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (7)
1. a kind of method for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials, it is characterised in that: concrete operations include
Following steps:
(1) reclaimed materials comminution pretreatment
Rewinding 500g is fetched, water for ball milling Crushing of Ultrafine, water removal, broken sieving are carried out；
(2) ingredient is weighed
Weigh appropriate ingredient, wherein Fe2O3Powder 60~80g, CaCO3Powder 3~7g, La2O3Powder 3~4g, Co2O3Powder 0
~1.5g, acceleration of sintering 1~2g of cosolvent, 1.5~8g of dispersing agent, 3~5g of acid-base neutralization agent；
(3) primary grinding
Reclaimed materials and ingredient are put into sand mill, and steel ball 12kg, 3.8~4kg of water is added, and carry out water for ball milling, water polo time consuming
For 1.5~3h, it is ground to 0.8~0.95 μm of slurry average particle size；
(4) pre-burning
It is dried being put by the material once ground in an oven, drying temperature is set as 200 DEG C, is crushed after drying, then puts
Enter and carries out pre-burning in Muffle furnace；
(5) secondary grinding
It is 3 μm that Preburning material, which is crushed to average particle size, takes Preburning material 500g, adds water 1000g, and secondary additive is added, secondary to add
Adding agent is SiO2Powder 0.5-1.5g, Bi2O3Powder 3-5g, D-sorbite 1-4g, HCOOH powder 0.5-2g, NH4HCO3Powder
Last 1-2g several combinations is put into ball grinder, grinds 15h, until average particle size is 0.81~0.85 μm；
(6) it is sintered
It is 60~65% by ground slurry precipitating or Direct Dehydration to pulp density, in the high magnetic field intensity of 120KA/M
Under, being pressed into density is 3.1~3.4g/cm3Regular magnet, the density that regular magnet is formed be 5.0~5.2g/cm3Magnetic
Body.
2. the method for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials stated according to claim 1, it is characterised in that:
The water for ball milling Crushing of Ultrafine is that reclaimed materials is milled to average particle size less than 2.0 μm；The temperature for removing water is 150~800
DEG C, the water content for removing water to reclaimed materials is 1.0~1.2%；The aperture of the broken sieving selection standard sub-sieve be 60 mesh with
Under.
3. the method according to claim 1 for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials, feature exist
In: the acceleration of sintering cosolvent is SiO2, the dispersing agent is H3BO3, one of D-sorbite and hydroxyl isomaltulose with
On, the acid-base neutralization agent is CH3COOH or NH4HCO3。
4. the method according to claim 1 for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials, feature exist
In: the temperature of pre-burning is 1200~1320 DEG C in the installation steps (4), and pre-burning soaking time is 60 ~ 200min.
5. the method according to claim 1 for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials, feature exist
In: the sintering temperature in the step (6) is 1200~1280 DEG C.
6. -5 any method for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials according to claim 1,
Be characterized in that: the additive amount of the metal oxide is not higher than the 20% of total 1 amount of material.
7. the method according to claim 6 for preparing high performance magnet with wet pressing permanent-magnet ferrite reclaimed materials, feature exist
In: the total amount of adding of the dispersing agent and acid-base neutralization agent is not higher than the 5% of material total amount.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661502A (en) * | 2020-12-25 | 2021-04-16 | 横店集团东磁股份有限公司 | High-frequency high-magnetic-field low-loss manganese-zinc ferrite material and preparation method thereof |
| CN112974472A (en) * | 2021-02-06 | 2021-06-18 | 中钢天源股份有限公司 | Method for recovering magnetic powder from injection-molded ferrite crushed aggregates |
Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2719280A1 (en) * | 1976-05-05 | 1977-11-10 | Lignes Telegraph Telephon | METHOD FOR MANUFACTURING FERRITE MAGNETIC CORE |
| JP2000211966A (en) * | 1999-01-20 | 2000-08-02 | Kagawa Prefecture | Production of soft ferrite or porcelain material supporting the same |
| EP1209135A1 (en) * | 2000-11-28 | 2002-05-29 | Minebea Co., Ltd. | Production process of recycled Mn-Zn ferrite |
| CN101157548A (en) * | 2007-09-26 | 2008-04-09 | 中南大学 | A kind of preparation method of high performance manganese zinc ferrite material |
| CN101202138A (en) * | 2007-09-30 | 2008-06-18 | 常州迪迩磁性材料有限公司 | Permanent ferrite magnetic tile and preparation method thereof |
| CN101412623A (en) * | 2008-11-13 | 2009-04-22 | 中南大学 | Method for producing manganese-zinc ferrite particle from manganese-zinc ferrite waste material |
| CN101492288A (en) * | 2009-02-17 | 2009-07-29 | 四川川西磁业有限责任公司 | Method for producing permanent ferrite and permanent ferrite |
| CN102674824A (en) * | 2012-05-29 | 2012-09-19 | 江门安磁电子有限公司 | Method for manufacturing MnZn ferrite by using MnZn ferrite core grinding waste |
| CN103102150A (en) * | 2013-02-28 | 2013-05-15 | 中国计量学院 | Preparation method for recycling of permanent magnetic ferrite waste |
| CN103117143A (en) * | 2013-01-25 | 2013-05-22 | 宁波同创强磁材料有限公司 | Neodymium iron boron magnet made of neodymium iron boron nickel-plating waste materials in sintered mode |
| CN103496961A (en) * | 2013-09-24 | 2014-01-08 | 南通万宝磁石制造有限公司 | Modifying method of nanometer permanent magnetic ferrite |
| CN104045332A (en) * | 2014-05-21 | 2014-09-17 | 肇庆冠磁科技有限公司 | Recycling method of solid waste |
| CN104575904A (en) * | 2014-11-26 | 2015-04-29 | 宁波宏垒磁业有限公司 | NdFeB magnet formed by sintering NdFeB recycling waste and preparation method of NdFeB magnet |
| CN105439550A (en) * | 2014-09-03 | 2016-03-30 | 自贡市江阳磁材有限责任公司 | Method for recycling permanently magnetic ferrite wastes |
| CN106363775A (en) * | 2016-08-29 | 2017-02-01 | 虔东稀土集团股份有限公司 | Ceramic body forming method and device thereof |
-
2018
- 2018-11-08 CN CN201811322226.8A patent/CN109400144A/en active Pending
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2719280A1 (en) * | 1976-05-05 | 1977-11-10 | Lignes Telegraph Telephon | METHOD FOR MANUFACTURING FERRITE MAGNETIC CORE |
| JP2000211966A (en) * | 1999-01-20 | 2000-08-02 | Kagawa Prefecture | Production of soft ferrite or porcelain material supporting the same |
| EP1209135A1 (en) * | 2000-11-28 | 2002-05-29 | Minebea Co., Ltd. | Production process of recycled Mn-Zn ferrite |
| CN101157548A (en) * | 2007-09-26 | 2008-04-09 | 中南大学 | A kind of preparation method of high performance manganese zinc ferrite material |
| CN101202138A (en) * | 2007-09-30 | 2008-06-18 | 常州迪迩磁性材料有限公司 | Permanent ferrite magnetic tile and preparation method thereof |
| CN101412623A (en) * | 2008-11-13 | 2009-04-22 | 中南大学 | Method for producing manganese-zinc ferrite particle from manganese-zinc ferrite waste material |
| CN101492288A (en) * | 2009-02-17 | 2009-07-29 | 四川川西磁业有限责任公司 | Method for producing permanent ferrite and permanent ferrite |
| CN102674824A (en) * | 2012-05-29 | 2012-09-19 | 江门安磁电子有限公司 | Method for manufacturing MnZn ferrite by using MnZn ferrite core grinding waste |
| CN103117143A (en) * | 2013-01-25 | 2013-05-22 | 宁波同创强磁材料有限公司 | Neodymium iron boron magnet made of neodymium iron boron nickel-plating waste materials in sintered mode |
| CN103102150A (en) * | 2013-02-28 | 2013-05-15 | 中国计量学院 | Preparation method for recycling of permanent magnetic ferrite waste |
| CN103496961A (en) * | 2013-09-24 | 2014-01-08 | 南通万宝磁石制造有限公司 | Modifying method of nanometer permanent magnetic ferrite |
| CN104045332A (en) * | 2014-05-21 | 2014-09-17 | 肇庆冠磁科技有限公司 | Recycling method of solid waste |
| CN105439550A (en) * | 2014-09-03 | 2016-03-30 | 自贡市江阳磁材有限责任公司 | Method for recycling permanently magnetic ferrite wastes |
| CN104575904A (en) * | 2014-11-26 | 2015-04-29 | 宁波宏垒磁业有限公司 | NdFeB magnet formed by sintering NdFeB recycling waste and preparation method of NdFeB magnet |
| CN106363775A (en) * | 2016-08-29 | 2017-02-01 | 虔东稀土集团股份有限公司 | Ceramic body forming method and device thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘晓杰等: "钕铁硼磁性材料生产工艺及其废料综合利用的研究进展", 《稀有金属与硬质合金》 * |
| 陈带军等: "铁氧体废料制备宽频高导锰锌铁氧体球磨工艺研究", 《功能材料》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661502A (en) * | 2020-12-25 | 2021-04-16 | 横店集团东磁股份有限公司 | High-frequency high-magnetic-field low-loss manganese-zinc ferrite material and preparation method thereof |
| CN112661502B (en) * | 2020-12-25 | 2022-03-25 | 横店集团东磁股份有限公司 | High-frequency high-magnetic-field low-loss manganese-zinc ferrite material and preparation method thereof |
| CN112974472A (en) * | 2021-02-06 | 2021-06-18 | 中钢天源股份有限公司 | Method for recovering magnetic powder from injection-molded ferrite crushed aggregates |
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