CN103578735A - Preparing method for soft rubber NdFeB (neodymium iron boron) magnet - Google Patents
Preparing method for soft rubber NdFeB (neodymium iron boron) magnet Download PDFInfo
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Abstract
The invention discloses a preparing method for a soft rubber NdFeB (neodymium iron boron) magnet and solves the problems that during the machining of the soft rubber NdFeB magnet in the prior art, the binding strength with rubber is lower, magnetic powder is easily stripped from the surface of a product, the tenacity is poor, cracking easily occurs, and the surface coating is easy to crack and strip. The method comprises the following steps of (1) surface modifying; (2) burdening; (3) open refining; (4) closed refining; (5) smashing; (6) tabletting; (7): laminating; (8) cutting; (9) spraying and (10) magnetizing. The raw materials of the NdFeB magnet and sprayed components of the coating are modified, before being subjected to the surface modifying, the rapid quenched NdFeB magnetic powder is preprocessed, and the drying process after the coating is sprayed is also optimally designed. The soft rubber NdFeB magnet manufactured by the preparing method has excellent strength and tenacity as well as excellent magnetic performance, and the binding strength of the coating at the surface of the soft rubber NdFeB magnet and the soft rubber NdFeB magnet is strong, so cracking difficultly occurs.
Description
Technical field
The present invention relates to a kind of neodymium iron boron magnetic body, especially relate to a kind of preparation method of flexible rubber neodymium iron boron magnetic body.
Background technology
NdFeB material belongs to high-performance metal magnetic material, and traditional neodymium iron boron is processed as sintering electroplating technology, and this technique is large to the dependence of mould, and the hardness of product high (rigidity neodymium iron boron composite material), and volume is large.NdFeB material also adopted the bonding agents such as epoxy resin to mix explained hereafter such as carrying out mold pressing, injection moulding with neodymium iron boron afterwards, and the hardness of product is also high, can not be crooked, cannot be made into thin thickness, and there is flexible product.
And along with the miniaturization precise treatment of various electric equipment productss changes, increasing product all needs to use thin thickness, performance is high, and flexible magnetic material that can free bend.For this reason, permanent-magnet ferrite rubber-plastic magnet arises at the historic moment, but the magnetic property of permanent-magnet ferrite material is low, cannot be applied in high-end market.NdFeB material can substitute permanent magnetic ferrite magnetic powder, improves the performance of product, but adopts the production technology of permanent magnetism rubber ferromagnetic to make two technical barriers of rubber and plastic neodymium iron boron magnetic body existence: the one, and toughness is bad, density is low, intensity is low, easily fracture; The 2nd, the processing of flexible rubber-plastic neodymium iron boron magnetic body is rear and rubber bound intensity is low, and magnetic easily comes off from the surface of product; The 3rd, the coating and the bond strength between flexible rubber-plastic neodymium iron boron magnetic body that are sprayed on flexible rubber-plastic neodymium-iron-boron surface are low, and poor toughness, when flexible rubber-plastic neodymium iron boron magnetic body is crooked, coating is easy to crack, peel off, easily cause the oxidation and rusting of flexible rubber-plastic neodymium iron boron magnetic body, reduce magnetic property, impact is used.
Chinese patent Granted publication number: CN101866733B, Granted publication day 2013.05.29, disclose a kind of elastic bonding type Nd-Fe-B magnetic material and manufacture method thereof, this neodymium-iron-boron magnetic material makes by following steps: batching: raw material is comprised of following component: the NdFeB magnetic powder of 10-95 weight portion; The ferromagnetic oxide powder of 1-50 weight portion, it is selected from strontium ferrite and/or barium ferrite; The binding agent of 2-20 weight portion, it is selected from CPE plastics, PE plastics, at least one in NBR rubber; The coupling agent of 0.1-3 weight portion; The plasticizer of 0.2-3 weight portion; And the adhesive of 0.1-3 weight portion, while wherein preparing burden, the first screening through 40 orders or larger order number by NdFeB magnetic powder, then by the NdFeB magnetic powder after described screening and coupling agent blend, make coupling agent thorough impregnation in metal magnetic, and then add other raw materials; And by the refining of powder process mixture, calendering, heat treatment, the moulding that prepare, obtain elastic bonding type Nd-Fe-B magnetic material.In this neodymium-iron-boron magnetic material, be added with ferromagnetic oxide powder, although cost, but magnetic property has also decreased simultaneously, simultaneously, for improving the intensity of neodymium iron boron magnetic body, add simultaneously and have binding agent and resinae adhesive, in addition, this neodymium iron boron magnetic body is by adding plasticizer to strengthen the toughness of neodymium iron boron magnetic body, and this has all increased cost to a certain extent.
Summary of the invention
To be flexible rubber neodymium iron boron magnetic body in order to solve prior art adding man-hour and rubber bound intensity is low in the present invention, magnetic easily comes off from the surface of product, poor toughness, easy fracture, and face coat is easy to crack, the problem of peeling off, provides a kind of preparation method of flexible rubber neodymium iron boron magnetic body, and this preparation method's step is simple, the flexible rubber neodymium iron boron magnetic body magnetic property and the toughness that obtain are good, and the coating on surface not easy to crack when flexible rubber-plastic neodymium iron boron magnetic body is crooked, peel off.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for flexible rubber neodymium iron boron magnetic body, comprises the following steps:
(1) surface modification: fast quenching NdFeB magnetic powder is added in surface modifier and soaks 10 ~ 12h after ultrasonic dispersion 10 ~ 30min, in vacuum, at 60 ~ 80 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:3 ~ 5, in described modifier, the mass percent of each component is: Silane coupling agent KH550 5 ~ 10%, pliability epoxy resin JEF-0240 or pliability epoxy resin JEF-0242 10 ~ 15%, modified amine curing agent JH-0111 3 ~ 5%, surplus is acetone.The present invention selects Silane coupling agent KH550, pliability epoxy resin JEF-0240 or pliability epoxy resin JEF-0242 and modified amine curing agent JH-0111 process the modifying surface of fast quenching NdFeB magnetic powder, on magnetic surface, form a high strength, the mobility of the coating film of high tenacity when improving dispersed homogeneous degree in haloflex of affinity between magnetic and haloflex and magnetic and banburying, make magnetic and haloflex form an organic crosslinked integral body, thereby greatly improve the bond strength of magnetic and haloflex, make magnetic be difficult for coming off from the surface of product, and effectively improve the intensity of flexible rubber neodymium iron boron magnetic body, in addition, coating film can also improve antioxygenic property and the corrosion resistance of magnetic, thereby improved to a certain extent the magnetic property of flexible rubber neodymium iron boron magnetic body.The model of the silane coupler in modifier of the present invention, epoxy resin and modifier and the selection of addition are all key points, this is that inventor constantly screens and optimization obtains, and the flexible rubber neodymium iron boron magnetic body that the fast quenching NdFeB magnetic powder of only being crossed by modifier treatment of the present invention makes just can have excellent intensity, toughness and magnetic property concurrently.
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 87.4 ~ 92.8% of surface modification, heat stabilizer 0.2 ~ 0.6%, haloflex 6 ~ 13%, each constituent content sum is 100%.Owing to adding in the present invention, there is haloflex (CPE), and haloflex can produce HCl gas because degraded occurs the physical actions such as friction, shearing in the process of banburying, HCl gas has autocatalysis, can impel CPE further to degrade, and the degraded of haloflex can impel the aging of flexible rubber neodymium iron boron magnetic body, reduce intensity and the toughness of flexible rubber neodymium iron boron magnetic body, also can affect its magnetic property, therefore, in the present invention, add and have heat stabilizer to suppress the degraded of haloflex.
(3) open refining: the roll spacing of mill is adjusted to 0.5 ~ 1.5mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 5 ~ 15min.
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 0.1 ~ 1Mpa, 40 ~ 100 ℃ of banburying temperature, the banburying time is 5 ~ 15min.
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 2 ~ 6min, and grinding screen screen distance is ∮ 2 ~ ∮ 10mm.
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, 20 ~ 80 ℃ of slice temperature, the THICKNESS CONTROL of slice is at 0.6 ~ 2mm.
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 3 ~ 10 layers, minute 3 ~ 4 sections of calenderings, every section press down rate≤40%.
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product.
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, the coating of spraying is comprised of the component of following mass percent: PU328-12KS waterborne polyurethane resin 80 ~ 83%, the stain resistant aqueous polyurethane resin 15 ~ 18% of PU8280, PUS-100 curing agent 1 ~ 2%, each constituent content sum is 100%.In flexible rubber neodymium-iron-boron surface, carry out spray treatment to improve the anti-oxidant of product, anti-corrosion capability, coating paintability of the present invention is splendid, excellent to the adhesive force of base material, the coating forming after dry has softness, resistance to xanthochromia, the feature that warping strength, wear-resisting and hot strength is high, when flexible rubber-plastic neodymium iron boron magnetic body is crooked, can not ftracture.
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2000 ~ 2500V.
As preferably, fast quenching NdFeB magnetic powder in step (1) carries out carrying out preliminary treatment before surface modification, pretreated concrete steps are: first use the NaOH solution of concentration 0.1 ~ 0.3mol/L to carry out alkali cleaning 10 ~ 15min to fast quenching NdFeB magnetic powder, use again 50 ~ 80 ℃ go dried up fast quenching NdFeB magnetic powder is washed, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 5 ~ 10min, finally dry 1 ~ 2h at 80 ~ 90 ℃ in being placed on ethanol at 40 ~ 50 ℃.Preliminary treatment is mainly to remove the grease adhering on fast quenching NdFeB magnetic powder, fast quenching NdFeB magnetic powder is carried out to surface active simultaneously, fast quenching NdFeB magnetic powder is placed in to the ultrasonic dispersion 5 ~ 10min of ethanol, finally at 80 ~ 90 ℃, dry 1 ~ 2h can thoroughly remove the impurity that is hidden between fast quenching NdFeB magnetic powder (as hydrogen, oxygen, moisture etc.), can not only make modifier evenly be coated on magnetic surface and form uniform coating film, improve oxidation-protective effect, can also effectively improve the bond strength between modifier and fast quenching NdFeB magnetic powder, can dry time and temperature extremely crucial for effectively removing impurity, excess Temperature, overlong time easily forms oxide-film meeting on magnetic surface, affect the covered effect of modifier and magnetic, temperature is too low, time is too short, impurity is difficult for removing completely, and efficiency is low.
As preferably, in step (2), described heat stabilizer is stearate.
As preferably, described stearate is calcium stearate or zinc stearate.
As preferably, in step (3), to open while refining, the roll spacing of mill is adjusted to 0.8 ~ 1mm, and mixing time is 8 ~ 12min.
As preferably, in step (4), during banburying, banburying pressure is 0.2 ~ 0.5Mpa, 50 ~ 80 ℃ of banburying temperature, and the banburying time is 6 ~ 10min.
As preferably, while pulverizing in step (5), grinding time is 3 ~ 4 minutes, and grinding screen screen distance is ∮ 2 ~ ∮ 4mm.
As preferably, in step (6) during slice, 30 ~ 60 ℃ of the temperature of slice, the THICKNESS CONTROL of slice is at 0.8 ~ 1.2mm.
As preferably, in step (9), the coating layer thickness of spraying is 50 ~ 70 μ m.Coating layer thickness is 50 ~ 70 μ m, there is special consideration: coating is too thin, wear-resisting effect is poor, and coating is too thick, when flexible rubber neodymium iron boron magnetic body is crooked, coating is easy to crack, and the time that blocked up coating need to be longer when solidifying and larger energy consumption, so the thickness of coating is advisable to be controlled at 50 ~ 70.
As preferably, the concrete steps of drying in step (9) are: by the first constant temperature baking 30 ~ 40min at 70 ~ 80 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product after spraying, be then down to drying at room temperature 1 ~ 2h, finally constant temperature baking 1 ~ 2h at 50 ~ 60 ℃.Because spray painting is more liquid behind flexible rubber neodymium iron boron magnetic body crude product surface, it is inhomogeneous that under constant temperature, direct baking easily causes coating layer thickness, therefore the present invention first toasts 30 ~ 40min by coating at 70 ~ 80 ℃, make coating solidify rapidly the effect of playing sizing, thereby effectively avoid the inhomogeneous of coating layer thickness, baking temperature is difficult for too high, too high words coating outer surface can ftracture, the too low effect that can not play sizing, be down to again drying at room temperature 1 ~ 2h so that coating is thoroughly solidified, finally at 50 ~ 60 ℃, constant temperature toasts 1 ~ 2h, with further solidified coating, thereby further improve the bond strength between coating and flexible rubber neodymium iron boron magnetic body crude product.
Therefore, the present invention has following beneficial effect:
(1) the flexible rubber neodymium iron boron magnetic body making has excellent intensity, toughness and magnetic property concurrently;
(2) before fast quenching NdFeB magnetic powder carries out surface modification, carry out preliminary treatment, make modifier evenly be coated on magnetic surface and form uniform coating film, improve oxidation-protective effect, can also effectively improve the bond strength between modifier and fast quenching NdFeB magnetic powder;
(3) in the present invention, add and have heat stabilizer, to suppress the degraded of haloflex;
(4) coating of spraying is improved, paintability is splendid, excellent to the adhesive force of base material, and the coating forming after dry has softness, resistance to xanthochromia, the feature that warping strength, wear-resisting and hot strength is high, when flexible rubber-plastic neodymium iron boron magnetic body is crooked, can not ftracture;
(5) by the constant temperature baking 30 ~ 40min at 70 ~ 80 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product elder generation after spraying, then be down to drying at room temperature 1 ~ 2h, finally at 50 ~ 60 ℃, constant temperature toasts 1 ~ 2h, curing of coatings is thorough, even thickness, and and flexible rubber neodymium iron boron magnetic body crude product between bond strength high.
Embodiment
Below by embodiment, the present invention will be further described.
In the present invention, if not refer in particular to, all percentage is unit of weight, all devices and raw material all can be buied from market or the industry is conventional, wherein, Silane coupling agent KH550 blocks Chemical Co., Ltd. purchased from Hangzhou Jesse, pliability epoxy resin JEF-0240, pliability epoxy resin JEF-0242 and modified amine curing agent JH-0111 3 ~ 5% are all purchased from Changshu Jia Fa Chemical Co., Ltd., PU328-12KS waterborne polyurethane resin, the stain resistant aqueous polyurethane resin of PU8280 and PUS-100 curing agent are all purchased from Zhong Fang auxiliary reagent factory, Taixing, method in following embodiment, if no special instructions, be this area conventional method.
Embodiment 1
(1) surface modification: first with the NaOH solution of concentration 0.1mol/L, fast quenching NdFeB magnetic powder is carried out to alkali cleaning 15min, with 50 ℃ go is dried up, fast quenching NdFeB magnetic powder is washed again, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 5min in being placed on ethanol at 40 ℃, afterwards by fast quenching NdFeB magnetic powder dry 1h at 90 ℃, then add in surface modifier and soak 12h after ultrasonic dispersion 10min, finally in vacuum, at 60 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:3, in modifier, the quality percentage composition of each component is: Silane coupling agent KH550 10%, pliability epoxy resin JEF-0240 10%, modified amine curing agent JH-0111 3%, surplus is acetone.
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 92.8% of surface modification, heat stabilizer 0.6%, haloflex 6.6%, wherein heat stabilizer is calcium stearate.
(3) open refining: the roll spacing of mill is adjusted to 0.5mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 5min.
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 1Mpa, 100 ℃ of banburying temperature, the banburying time is 5min.
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 6min, and grinding screen screen distance is ∮ 10mm.
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, 80 ℃ of slice temperature, the THICKNESS CONTROL of slice is at 0.6mm.
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 3 layers, minute 3 sections of calenderings, every section press down rate≤40%.
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product.
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, the coating layer thickness of spraying is 50 ~ 70 μ m, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, in the coating of spraying, the quality percentage composition of each component is: PU328-12KS waterborne polyurethane resin 83%, the stain resistant aqueous polyurethane resin 16% of PU8280, PUS-100 curing agent 1%, the concrete steps of drying in this step are: by the constant temperature baking 30min at 80 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product elder generation after spraying, then be down to drying at room temperature 1h, finally at 50 ℃, constant temperature toasts 2h.
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2000V.
Embodiment 2
(1) surface modification: first with the NaOH solution of concentration 0.3mol/L, fast quenching NdFeB magnetic powder is carried out to alkali cleaning 10min, with 80 ℃ go is dried up, fast quenching NdFeB magnetic powder is washed again, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 10min in being placed on ethanol at 50 ℃, afterwards by fast quenching NdFeB magnetic powder dry 2h at 80 ℃, then add in surface modifier and soak 10h after ultrasonic dispersion 30min, finally in vacuum, at 80 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:5, in modifier, the quality percentage composition of each component is: Silane coupling agent KH550 5%, pliability epoxy resin JEF-0242 15%, modified amine curing agent JH-0111 5%, surplus is acetone.
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 87.4% of surface modification, heat stabilizer 0.2%, haloflex 12.4%, wherein heat stabilizer is zinc stearate.
(3) open refining: the roll spacing of mill is adjusted to 1.5mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 15min.
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 0.1Mpa, 40 ℃ of banburying temperature, the banburying time is 15min.
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 2min, and grinding screen screen distance is ∮ 2mm.
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, 20 ℃ of slice temperature, the THICKNESS CONTROL of slice is at 2mm.
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 10 layers, minute 4 sections of calenderings, every section press down rate≤40%.
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product.
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, the coating layer thickness of spraying is 50 ~ 70 μ m, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, in the coating of spraying, the quality percentage composition of each component is: PU328-12KS waterborne polyurethane resin 80%, the stain resistant aqueous polyurethane resin 18% of PU8280, PUS-100 curing agent 2%, the concrete steps of drying in this step are: by the constant temperature baking 40min at 70 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product elder generation after spraying, then be down to drying at room temperature 2h, finally at 60 ℃, constant temperature toasts 1h.
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2500V.
Embodiment 3
(1) surface modification: first with the NaOH solution of concentration 0.2mol/L, fast quenching NdFeB magnetic powder is carried out to alkali cleaning 12min, with 60 ℃ go is dried up, fast quenching NdFeB magnetic powder is washed again, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 6min in being placed on ethanol at 45 ℃, afterwards by fast quenching NdFeB magnetic powder dry 1.5h at 85 ℃, then add in surface modifier and soak 11h after ultrasonic dispersion 15min, finally in vacuum, at 70 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:3 ~ 5, in modifier, the quality percentage composition of each component is: Silane coupling agent KH550 6%, pliability epoxy resin JEF-0242 11%, modified amine curing agent JH-0111 4%, surplus is acetone.
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 86.7% of surface modification, heat stabilizer 0.3%, haloflex 13%, wherein heat stabilizer is zinc stearate.
(3) open refining: the roll spacing of mill is adjusted to 0.6mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 7min.
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 0.6Mpa, banburying temperature 45 C, the banburying time is 11min.
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 5min, and grinding screen screen distance is ∮ 5mm.
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, 25 ℃ of slice temperature, the THICKNESS CONTROL of slice is at 0.7mm.
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 6 layers, minute 3 sections of calenderings, every section press down rate≤40%.
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product.
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, the coating layer thickness of spraying is 60 μ m, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, in the coating of spraying, the quality percentage composition of each component is: PU328-12KS waterborne polyurethane resin 81.5%, the stain resistant aqueous polyurethane resin 17% of PU8280, PUS-100 curing agent 1.5%, the concrete steps of drying in this step are: by the constant temperature baking 32min at 75 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product elder generation after spraying, then be down to drying at room temperature 1.5h, finally at 55 ℃, constant temperature toasts 1.5h.
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2300V.
Embodiment 4
(1) surface modification: first with the NaOH solution of concentration 0.1mol/L, fast quenching NdFeB magnetic powder is carried out to alkali cleaning 15min, with 80 ℃ go is dried up, fast quenching NdFeB magnetic powder is washed again, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 10min in being placed on ethanol at 40 ℃, afterwards by fast quenching NdFeB magnetic powder dry 2h at 80 ℃, then add in surface modifier and soak 10h after ultrasonic dispersion 30min, finally in vacuum, at 80 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:5, in modifier, the quality percentage composition of each component is: Silane coupling agent KH550 10%, pliability epoxy resin JEF-0240 15%, modified amine curing agent JH-0111 5%, surplus is acetone.
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 92.8% of surface modification, heat stabilizer 1.2%, haloflex 6%, wherein heat stabilizer is calcium stearate.
(3) open refining: the roll spacing of mill is adjusted to 0.8mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 12min.
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 0.5Mpa, banburying temperature 50 C, the banburying time is 10min.
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 4min, and grinding screen screen distance is ∮ 4mm.
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, 30 ℃ of slice temperature, the THICKNESS CONTROL of slice is at 0.8mm.
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 10 layers, minute 4 sections of calenderings, every section press down rate≤40%.
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product.
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, the coating layer thickness of spraying is 50 μ m, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, in the coating of spraying, the quality percentage composition of each component is: PU328-12KS waterborne polyurethane resin 83%, the stain resistant aqueous polyurethane resin 15% of PU8280, PUS-100 curing agent 2%, the concrete steps of drying in this step are: by the constant temperature baking 40min at 70 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product elder generation after spraying, then be down to drying at room temperature 2h, finally at 50 ℃, constant temperature toasts 2h.
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2000V.
Embodiment 5
(1) surface modification: first with the NaOH solution of concentration 0.3mol/L, fast quenching NdFeB magnetic powder is carried out to alkali cleaning 10min, with 50 ℃ go is dried up, fast quenching NdFeB magnetic powder is washed again, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 5min in being placed on ethanol at 50 ℃, afterwards by fast quenching NdFeB magnetic powder dry 1h at 90 ℃, then add in surface modifier and soak 12h after ultrasonic dispersion 10min, finally in vacuum, at 80 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:3, in modifier, the quality percentage composition of each component is: Silane coupling agent KH550 5%, pliability epoxy resin JEF-0242 10%, modified amine curing agent JH-0111 4%, surplus is acetone.
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 92.8% of surface modification, heat stabilizer 0.7%, haloflex 6.5%.
(3) open refining: the roll spacing of mill is adjusted to 1mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 8min.
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 0.2Mpa, 80 ℃ of banburying temperature, the banburying time is 6min.
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 3min, and grinding screen screen distance is ∮ 2mm.
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, slice temperature 60 C, the THICKNESS CONTROL of slice is at 1.2mm.
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 3 layers, minute 3 sections of calenderings, every section press down rate≤40%.
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product.
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, the coating layer thickness of spraying is 70 μ m, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, in the coating of spraying, the quality percentage composition of each component is: PU328-12KS waterborne polyurethane resin 81%, the stain resistant aqueous polyurethane resin 18% of PU8280, PUS-100 curing agent 1%, the concrete steps of drying in this step are: by the constant temperature baking 30min at 80 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product elder generation after spraying, then be down to drying at room temperature 1h, finally at 50 ℃, constant temperature toasts 1h.
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2500V.
Embodiment 6
(1) surface modification: first with the NaOH solution of concentration 0.2mol/L, fast quenching NdFeB magnetic powder is carried out to alkali cleaning 12min, with 65 ℃ go is dried up, fast quenching NdFeB magnetic powder is washed again, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 7min in being placed on ethanol at 45 ℃, afterwards by fast quenching NdFeB magnetic powder dry 1.5h at 85 ℃, then add in surface modifier and soak 11h after ultrasonic dispersion 15min, finally in vacuum, at 75 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:4, in described modifier, the quality percentage composition of each component is: Silane coupling agent KH550 10%, pliability epoxy resin JEF-0240 15%, modified amine curing agent JH-0111 3%, surplus is acetone.
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 88.5% of surface modification, heat stabilizer 0.5%, haloflex 11%.
(3) open refining: the roll spacing of mill is adjusted to 0.9mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 9min.
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 0.3Mpa, banburying temperature 60 C, the banburying time is 9min.
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 3.5min, and grinding screen screen distance is ∮ 3mm.
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, slice temperature 45 C, the THICKNESS CONTROL of slice is at 0.9mm.
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 4 layers, minute 4 sections of calenderings, every section press down rate≤40%.
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product.
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, the coating layer thickness of spraying is 60 μ m, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, in the coating of spraying, the quality percentage composition of each component is: PU328-12KS waterborne polyurethane resin 82%, the stain resistant aqueous polyurethane resin 16% of PU8280, PUS-100 curing agent 2%, the concrete steps of drying in this step are: by the constant temperature baking 32min at 75 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product elder generation after spraying, then be down to drying at room temperature 1.5h, finally at 55 ℃, constant temperature toasts 1.5h.
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2400V.
The flexible rubber neodymium iron boron magnetic body finished product that the various embodiments described above are obtained detects, and the magnetic property obtaining is as shown in table 1:
The flexible rubber neodymium iron boron magnetic body finished product magnetic property of each embodiment of table 1
| Group | Br(T) | Hcj(kA/m) | Hcb(kA/m) | BH(kJ/m 3) |
| Embodiment 1 | 0.48 | 561.61 | 254.46 | 33.32 |
| Embodiment 2 | 0.43 | 573.23 | 258.68 | 32.31 |
| Embodiment 3 | 0.42 | 582.68 | 252.71 | 30.86 |
| Embodiment 4 | 0.49 | 565.61 | 261.56 | 36.75 |
| Embodiment 5 | 0.49 | 555.78 | 258.46 | 35.88 |
| Embodiment 6 | 0.45 | 572.25 | 259.65 | 32.43 |
From table 1, can obviously find out, flexible rubber neodymium iron boron magnetic body finished product of the present invention has good magnetic property.
Adopt rubber tensile testing machine to test hot strength and the elongation of the flexible rubber neodymium iron boron magnetic body finished product of each embodiment, the mechanical property obtaining is as shown in table 2:
The mechanical property of the flexible rubber neodymium iron boron magnetic body finished product of each embodiment of table 2
| Group | Hot strength (Mpa) | Elongation (%) | Density (g/cm 3) | Hardness (A) |
| Embodiment 1 | 3.01 | 52.2% | 4.53 | 97 |
| Embodiment 2 | 2.98 | 62.8% | 4.52 | 96 |
| Embodiment 3 | 3.06 | 63.3% | 4.58 | 95 |
| Embodiment 4 | 3.46 | 50.5% | 4.67 | 98 |
| Embodiment 5 | 3.41 | 51.2% | 4.68 | 98 |
| Embodiment 6 | 3.52 | 60.1% | 4.62 | 96 |
As can be seen from Table 2, flexible rubber neodymium iron boron magnetic body finished product of the present invention has excellent mechanical property.
Above-described embodiment is a kind of preferably scheme of the present invention, not the present invention is done to any pro forma restriction, also has other variant and remodeling under the prerequisite that does not exceed the technical scheme that claim records.
Claims (10)
1. a preparation method for flexible rubber neodymium iron boron magnetic body, is characterized in that, comprises the following steps:
(1) surface modification: fast quenching NdFeB magnetic powder is added in surface modifier and soaks 10 ~ 12h after ultrasonic dispersion 10 ~ 30min, in vacuum, at 60 ~ 80 ℃, dry, obtain the fast quenching NdFeB magnetic powder of surface modification, wherein, the mass ratio of fast quenching NdFeB magnetic powder and surface modifier is 1:3 ~ 5, in described modifier, the mass percent of each component is: Silane coupling agent KH550 5 ~ 10%, pliability epoxy resin JEF-0240 or pliability epoxy resin JEF-0242 10 ~ 15%, modified amine curing agent JH-0111 3 ~ 5%, surplus is acetone;
(2) batching: obtain compound after fast quenching NdFeB magnetic powder and heat stabilizer, the haloflex of surface modification are mixed, in compound, the quality percentage composition of each component is: the fast quenching NdFeB magnetic powder 87.4 ~ 92.8% of surface modification, heat stabilizer 0.2 ~ 0.6%, haloflex 6 ~ 13%, each constituent content sum is 100%;
(3) open refining: the roll spacing of mill is adjusted to 0.5 ~ 1.5mm, the compound that obtains is dropped into mill carry out mixingly in step (2), mixing time is 5 ~ 15min;
(4) banburying: the material of opening after refining is dropped into banburying in banbury, and banburying pressure is 0.1 ~ 1Mpa, 40 ~ 100 ℃ of banburying temperature, the banburying time is 5 ~ 15min;
(5) pulverize: the material after banburying is dropped into pulverizer and pulverize, grinding time is 2 ~ 6min, and grinding screen screen distance is ∮ 2 ~ ∮ 10mm;
(6) slice: the material after pulverizing is dropped into slice in film-discharging machine, 20 ~ 80 ℃ of slice temperature, the THICKNESS CONTROL of slice is at 0.6 ~ 2mm;
(7) laminate: to the calendering that superposes of the magnetic sheet after slice, the number of plies laminating is 3 ~ 10 layers, minute 3 ~ 4 sections of calenderings, every section press down rate≤40%;
(8) cutting: the magnetic sheet of calendering is cut, obtain flexible rubber neodymium iron boron magnetic body crude product;
(9) spraying: flexible rubber neodymium iron boron magnetic body crude product is carried out to spray treatment, dry, obtain flexible rubber neodymium iron boron magnetic body semi-finished product, the coating of spraying is comprised of the component of following mass percent: PU328-12KS waterborne polyurethane resin 80 ~ 83%, the stain resistant aqueous polyurethane resin 15 ~ 18% of PU8280, PUS-100 curing agent 1 ~ 2%, each constituent content sum is 100%;
(10) magnetize: the flexible rubber neodymium iron boron magnetic body semi-finished product that obtain in step (9) are magnetized, obtain flexible rubber neodymium iron boron magnetic body finished product, the voltage that magnetizes is 2000 ~ 2500V.
2. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, it is characterized in that, fast quenching NdFeB magnetic powder in step (1) carries out carrying out preliminary treatment before surface modification, pretreated concrete steps are: first use the NaOH solution of concentration 0.1 ~ 0.3mol/L to carry out alkali cleaning 10 ~ 15min to fast quenching NdFeB magnetic powder, use again 50 ~ 80 ℃ go dried up fast quenching NdFeB magnetic powder is washed, until fast quenching NdFeB magnetic powder pH is neutral, then by fast quenching NdFeB magnetic powder constant temperature drying ultrasonic dispersion 5 ~ 10min in being placed on ethanol at 40 ~ 50 ℃, finally at 80 ~ 90 ℃, be dried 1 ~ 2h.
3. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, is characterized in that, in step (2), described heat stabilizer is stearate.
4. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 3, is characterized in that, described stearate is calcium stearate or zinc stearate.
5. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, is characterized in that, while opening refining in step (3), the roll spacing of mill is adjusted to 0.8 ~ 1mm, and mixing time is 8 ~ 12min.
6. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, is characterized in that, during the middle banburying of step (4), banburying pressure is 0.2 ~ 0.5Mpa, 50 ~ 80 ℃ of banburying temperature, and the banburying time is 6 ~ 10min.
7. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, is characterized in that, while pulverizing in step (5), grinding time is 3 ~ 4 minutes, and grinding screen screen distance is ∮ 2 ~ ∮ 4mm.
8. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, is characterized in that, during the middle slice of step (6), and 30 ~ 60 ℃ of the temperature of slice, the THICKNESS CONTROL of slice is at 0.8 ~ 1.2mm.
9. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, is characterized in that, in step (9), the coating layer thickness of spraying is 50 ~ 70 μ m.
10. the preparation method of a kind of flexible rubber neodymium iron boron magnetic body according to claim 1, it is characterized in that, the concrete steps of drying in step (9) are: by the first constant temperature baking 30 ~ 40min at 70 ~ 80 ℃ of temperature of the flexible rubber neodymium iron boron magnetic body crude product after spraying, then be down to drying at room temperature 1 ~ 2h, finally constant temperature baking 1 ~ 2h at 50 ~ 60 ℃.
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