CN101364467A - Preparation of ferrite magnetic spliced magnet having great processability - Google Patents
Preparation of ferrite magnetic spliced magnet having great processability Download PDFInfo
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- CN101364467A CN101364467A CNA2008100166942A CN200810016694A CN101364467A CN 101364467 A CN101364467 A CN 101364467A CN A2008100166942 A CNA2008100166942 A CN A2008100166942A CN 200810016694 A CN200810016694 A CN 200810016694A CN 101364467 A CN101364467 A CN 101364467A
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 6
- 235000021317 phosphate Nutrition 0.000 claims description 6
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- 125000002723 alicyclic group Chemical group 0.000 claims description 4
- 150000001408 amides Chemical class 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
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- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 3
- 229940063655 aluminum stearate Drugs 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- HTDKEJXHILZNPP-UHFFFAOYSA-N dioctyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OCCCCCCCC HTDKEJXHILZNPP-UHFFFAOYSA-N 0.000 claims description 3
- QEWYKACRFQMRMB-UHFFFAOYSA-N monofluoroacetic acid Natural products OC(=O)CF QEWYKACRFQMRMB-UHFFFAOYSA-N 0.000 claims description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 3
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 3
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000571 Nylon 11 Polymers 0.000 claims description 2
- 229920000299 Nylon 12 Polymers 0.000 claims description 2
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 2
- 229920000572 Nylon 6/12 Polymers 0.000 claims description 2
- 235000010290 biphenyl Nutrition 0.000 claims description 2
- 239000004305 biphenyl Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- XCOASYLMDUQBHW-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)butan-1-amine Chemical compound CCCCNCCC[Si](OC)(OC)OC XCOASYLMDUQBHW-UHFFFAOYSA-N 0.000 claims description 2
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
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- 229910052712 strontium Inorganic materials 0.000 description 6
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- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
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- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 229920003189 Nylon 4,6 Polymers 0.000 description 1
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- IXSZQYVWNJNRAL-UHFFFAOYSA-N etoxazole Chemical compound CCOC1=CC(C(C)(C)C)=CC=C1C1N=C(C=2C(=CC=CC=2F)F)OC1 IXSZQYVWNJNRAL-UHFFFAOYSA-N 0.000 description 1
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- MOMGDEWWZBKDDR-UHFFFAOYSA-M sodium;3,4,5,6-tetrahydro-2h-azepin-7-olate Chemical compound [Na+].O=C1CCCCC[N-]1 MOMGDEWWZBKDDR-UHFFFAOYSA-M 0.000 description 1
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- Hard Magnetic Materials (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention relates to a ferrite bonded magnet with good processing characteristics, which can retain excellent high temperature fluidity without losing magnetic characteristics and mechanical strength. The ferrite bonded magnet is prepared by the steps as follows: adding isotropic strontian ferrite magnetic powder, thermoplastic resin (nylon) monomer, a sodium salt, a processing assistant and a magnetic powder modifier into a pretreatment kettle according to a certain proportion, and vacuuming; heating the pretreatment kettle while stirring the materials for a while, introducing a certain quantity of nitrogen gas under pressure, adding a certain quantity of an activator, and stirring for a while to obtain a compound pre-polymer; and delivering the pre-polymer into a double screw extrusion machine to conduct conveying, polymerization initiation, growth, termination and residual monomers removal, extruding the obtained polymer via a neck ring mold, cooling, drying, and granulating to obtain the finished ferrite bonded magnet granules.
Description
Technical field:
The present invention relates to a kind of ferrite bonded magnet material, with and preparation technology.
Background technology:
About the seventies in 20th century, bonded permanent magnet a kind of novel magnetic material appearred:.So-called bonded permanent magnet, be meant that with plastics or rubber be binding agent and the magnetic magnet by the required form be combined into, the magnetic material relative density that is obtained is light, and easily machine-shaping becomes the high and complex-shaped goods of dimensional accuracy, overcome hard and crisp, the poor in processability of former magnetic material, can't make the defective of complexity, precise shape goods.Usually by the permanent magnet of rubber bound because toughness is had a surplus, undercapacity generally is not used for substituting traditional permanent magnet.And with the permanent magnet of plastic bonding magnetic powders, can obtain the bonded permanent magnet of high strength, high-modulus, high magnetic, shown very excellent characteristic, since emerging development swift and violent, in the middle of magnetic material, occupied critical role at present.In China, the plastic bonding magnet still belongs to new things, except the small-scale production of a small amount of kind, and all the other basic dependence on import, except the plastic bonding magnet of some kind can reach the equal level of external similar commercial product in the laboratory, integral body is still backward relatively.
Plastic bonding magnet (polymer bonded magnets) generally ranges permanent magnet.It is that processing characteristics is good.The plastics of lighter weight, for example PPS, nylon etc. mix with magnetic, become the permanent magnetic material of different shape according to the demand moulding.Wherein the ferrite bonded permanent magnet is the important component part in the bonded permanent magnet.Its general manufacture method is that ferromagnetic oxide powder, binding agent and processing aid are mixed, by extrude, method moulding such as injection or mold pressing obtain the bonded permanent magnet that different shape is different, the magnetic property requirement is different.Wherein utilize injection molding bonded permanent magnet to save the molding process of goods, and can moulding obtain different, baroque accurate magnetic device, for example strip, sheet, tubulose and thin-walled ring-type.The injection moulding production technology is simple, production efficiency is high, and the magnet size precision height of moulding, need not secondary operations meets the developing direction of modern magnetic device towards lightweight, precise treatment, miniaturization, high performance and low energy consumptionization.
In order to guarantee that bonded permanent magnet has enough mechanical performances, bonded permanent magnet generally selects for use high strength engineering plastics such as nylon, Merlon, polyphenylene sulfide and polyimides as binding agent, in order to obtain higher magnetic property, require to improve the load capacity of magnetic again, this can reduce the flowability of melt undoubtedly.But extrude, injection moulding has relatively high expectations for the bonded permanent magnet temperature flowing, so strengthen the temperature flowing of bonded permanent magnet when keeping higher magnetic loading, is the difficult problem that this patent important solution.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that prior art exists, a kind of novel bonding magnet with fine magnetic property, mechanical performance and processing characteristics (temperature flowing) is provided, when keeping magnetic property and machinery constant substantially, increase fluidity of molten, utilize the reaction extruding-out process, with the pellet of preparation magnetic material.
Another object of the present invention is to provide the manufacture method of above-mentioned ferrite bonded permanent magnet.
A kind of ferrite bonded permanent magnet provided by the invention, its composition and weight content are:
Isotropic ferrite magnetic: 80~92%
Thermoplastic resin: 15~20%
Various processing aids, magnetic modifier: 0~5%
The basis of ferromagnetic oxide powder of the present invention comprises with the iron oxide being principal phase, doped portion strontium oxide strontia.Main component is SrO6Fe
2O
3Ferrimagnet is compared with magnets such as SmFeN with the NdFeB magnet, the antioxidant anticorrosive better performances, and magnetic production is simple, and magnetic does not contain strategic materials, but the magnetic magnetic property is low, is applicable to the low side purposes.
The thermoplastic resin that the present invention selects for use is mainly nylon 11, nylon 12, NYLON610, nylon 612, nylon 1010, nylon 46, nylon 7, nylon 9, the resin material of system such as nylon 13 nylon such as grade, nylon material has very high mechanical strength, and the softening point height is heat-resisting, coefficient of friction is low, and is wear-resistant, self lubricity, shock absorption and noise reduction, oil resistant, weak acid resistant, alkaline-resisting and common solvent, electrical insulating property is good, and self-extinguishment is arranged, nontoxic, odorless, good weatherability, and be good with the ferromagnetic oxide powder compatibility, and temperature flowing is splendid, and can remain on 300 ℃ and do not degrade with interior, the employed resin of this patent is not a finished commercial prod for utilizing monomer reaction extruding polymerization gained.
The processing aid that the present invention selects for use comprises one or several in ethylene bis stearamide, aluminum stearate, 3-phenoxy group-4-fluorobenzaldehyde, oleamide, dibutyl ester dioctyl ester, the fatty diglycollic amide; Magnetic modifier comprises one or several in two (dioctyl phosphate) titanate esters of fluoroacetic acid ester, two (the two hot phosphates) titanate esters of tetra isopropyl, two (the two hot phosphates) titanate esters of tetra isopropyl, two-[r-(triethoxy is silica-based) propyl group] amine, N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan, N-(normal-butyl)-3-aminopropyl trimethoxysilane, the amino silane.
The employed equipment of patent of the present invention has prepolymerization kettle and double screw extruder.Be furnished with each cover of mechanical type mixing plant and inflated with nitrogen and pumped vacuum systems in the prepolymerization kettle, adopting biphenyl is the chuck heating of heating agent, and the bottom of still is controlled with ball valve, and links to each other by stainless steel pipe and double screw extruder are airtight.The draw ratio of double screw extruder is 36.
The preparation method of ferrite bonded permanent magnet of the present invention is: seal charge door after sodium salt, NaOH and the magnetic of a certain amount of thermoplastic resin alicyclic monomer and thermoplastic resin alicyclic monomer, various processing aid and magnetic modifier are added the preliminary treatment still jointly according to certain ratio, vacuumize then.The preliminary treatment still is warmed up to 100 ℃ stirs material simultaneously; this process continues 2 hours; be pressed into a certain amount of nitrogen (interior pressure-controlled is at 0.01MPa) then as protective atmosphere; continue to add a certain amount of activator (for example 2 then; the 4-2 toluene di-isocyanate(TDI)), continue to stir 10~15min and make compound performed polymer.Open ball valve, the performed polymer that obtains is sent into double screw extruder, conveying, the polymerization of finishing compound performed polymer cause, increase, stop and remove residual monomer, and polymer through port mould is extruded then, cooling and shaping in tank, forced air drying then, granulation.
Bonded permanent magnet of the present invention adopts reaction extrusion process to obtain the bonded permanent magnet pellet.The bonded permanent magnet that uses this moulding process to obtain, magnetic is uniformly dispersed in thermoplastic resin, and magnetic property is stable, temperature flowing is compared splendid with commercially available ferrite bonded permanent magnet, the bonded permanent magnet freedom shape that obtains is big, magnet rate of finished products height, and the waste product that obtains can also reuse.When selecting thermoplastic resin, the softening temperature of resin and temperature flowing are important reference factors, but and to consider the highest processing temperature of ferromagnetic oxide powder, but need seek a balance point in primary liquidity temperature and the highest processing temperature, and cut down the consumption of energy as much as possible.Relatively be fit to extruding and injection moulding of nylon based ferrite bonded permanent magnet at 230 ℃~270 ℃.
The present invention has following beneficial effect:
1. owing to adopted homemade isotropism strontium ferrite magnetic powder as raw material, cost of material is cheap, does not contain strategic metal, and extensively is easy to get.The price of the monomer that uses is usually also less than the price of commercially available corresponding monomer polymerization product.
2. when not reducing mechanical performance and magnetic property substantially, can not keep temperature flowing preferably, be easy to injection moulding.
3. in the bonded permanent magnet that obtains, thermoplastic resin coating magnetic surface is comparatively complete, and heat-resisting oxygen corrosion is better, thereby the temperature range and the application that are suitable for are wider.
4. magnet of the present invention can be widely used in the middle of the low side magnetic product scopes such as electrical micro-machine, automobile making, electronic instrument.
Specific embodiments:
Following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1
It is the strontium ferrite powder of 2~5 μ m that magnetic is selected average grain diameter for use, and its quality accounts for 79.21% of bonded permanent magnet gross mass.Magnetic modifier is selected two (dioctyl phosphate) titanate esters of fluoroacetic acid ester for use, and its quality accounts for 0.79% of bonded permanent magnet gross mass; Processing aid is selected ethylene bis stearamide for use, and its quality accounts for 1% of bonded permanent magnet gross mass; Seal charge door after this mixture and 19% the caprolactam that accounts for the bonded permanent magnet gross mass and caprolactam sodium salt and NaOH added the preliminary treatment still jointly, vacuumize then.The preliminary treatment still is warmed up to 100 ℃ stirs material simultaneously; this process continues 2 hours, is pressed into a certain amount of nitrogen (interior pressure-controlled is at 0.01MPa) then as protective atmosphere, continues then to add a certain amount of 2; the 4-2 toluene di-isocyanate(TDI)), continue to stir 10min and make compound performed polymer.Open ball valve, the performed polymer that obtains is sent into double screw extruder, conveying, the polymerization of finishing compound performed polymer cause, increase, stop and remove residual monomer, and polymer through port mould is extruded then, cooling and shaping in tank, forced air drying then, granulation.
Embodiment 2
It is the strontium ferrite powder of 2~5 μ m that magnetic is selected average grain diameter for use, and its quality accounts for 79.21% of bonded permanent magnet gross mass.Magnetic modifier is selected two (the two hot phosphates) titanate esters of tetra isopropyl for use, and its quality accounts for 0.79% of bonded permanent magnet gross mass; Processing aid is selected aluminum stearate for use, and its quality accounts for 1% of bonded permanent magnet gross mass; Seal charge door after this mixture and 19% the ring lauramide that accounts for the bonded permanent magnet gross mass and ring lauramide sodium salt and NaOH added the preliminary treatment still jointly, vacuumize then.The preliminary treatment still is warmed up to 100 ℃ stirs material simultaneously; this process continues 2 hours, is pressed into a certain amount of nitrogen (interior pressure-controlled is at 0.01MPa) then as protective atmosphere, continues then to add a certain amount of 2; the 4-2 toluene di-isocyanate(TDI)), continue to stir 10min and make compound performed polymer.Open ball valve, the performed polymer that obtains is sent into double screw extruder, conveying, the polymerization of finishing compound performed polymer cause, increase, stop and remove residual monomer, and polymer through port mould is extruded then, cooling and shaping in tank, forced air drying then, granulation.
Embodiment 3
It is the strontium ferrite powder of 2~5 μ m that magnetic is selected average grain diameter for use, and its quality accounts for 79.21% of bonded permanent magnet gross mass.Magnetic modifier is selected two (the two hot phosphates) titanate esters of tetra isopropyl for use, and its quality accounts for 0.79% of bonded permanent magnet gross mass; Processing aid is selected 3-phenoxy group-4-fluorobenzaldehyde for use, and its quality accounts for 1% of bonded permanent magnet gross mass; Seal charge door after this mixture and 19% ring nine acid amides that account for the bonded permanent magnet gross mass and ring nine chlorseptols and NaOH added the preliminary treatment still jointly, vacuumize then.The preliminary treatment still is warmed up to 100 ℃ stirs material simultaneously; this process continues 2 hours, is pressed into a certain amount of nitrogen (interior pressure-controlled is at 0.01MPa) then as protective atmosphere, continues then to add a certain amount of 2; the 4-2 toluene di-isocyanate(TDI)), continue to stir 10min and make compound performed polymer.Open ball valve, the performed polymer that obtains is sent into double screw extruder, conveying, the polymerization of finishing compound performed polymer cause, increase, stop and remove residual monomer, and polymer through port mould is extruded then, cooling and shaping in tank, forced air drying then, granulation.
Embodiment 4
It is the strontium ferrite powder of 2~5 μ m that magnetic is selected average grain diameter for use, and its quality accounts for 79.21% of bonded permanent magnet gross mass.Magnetic modifier is selected two-[r-(triethoxy is silica-based) propyl group] amine for use, and its quality accounts for 0.79% of bonded permanent magnet gross mass; Processing aid is selected oleamide for use, and its quality accounts for 1% of bonded permanent magnet gross mass; Seal charge door after this mixture and 19% the ring undecanoic amide that accounts for the bonded permanent magnet gross mass, ring undecanoic amide sodium salt and NaOH added the preliminary treatment still jointly, vacuumize then.The preliminary treatment still is warmed up to 100 ℃ stirs material simultaneously; this process continues 2 hours, is pressed into a certain amount of nitrogen (interior pressure-controlled is at 0.01MPa) then as protective atmosphere, continues then to add a certain amount of 2; the 4-2 toluene di-isocyanate(TDI)), continue to stir 10min and make compound performed polymer.Open ball valve, the performed polymer that obtains is sent into double screw extruder, conveying, the polymerization of finishing compound performed polymer cause, increase, stop and remove residual monomer, and polymer through port mould is extruded then, cooling and shaping in tank, forced air drying then, granulation.
Embodiment 5
It is the strontium ferrite powder of 2~5 μ m that magnetic is selected average grain diameter for use, and its quality accounts for 79.21% of bonded permanent magnet gross mass.Magnetic modifier is selected N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan for use, and its quality accounts for 0.79% of bonded permanent magnet gross mass; Processing aid selected fatty acid diglycollic amide, its quality accounts for 1% of bonded permanent magnet gross mass; Seal charge door after this mixture and 19% the ring tridecanoyl amine that accounts for the bonded permanent magnet gross mass, ring tridecanoyl amine sodium salt and NaOH added the preliminary treatment still jointly, vacuumize then.The preliminary treatment still is warmed up to 100 ℃ stirs material simultaneously; this process continues 2 hours, is pressed into a certain amount of nitrogen (interior pressure-controlled is at 0.01MPa) then as protective atmosphere, continues then to add a certain amount of 2; the 4-2 toluene di-isocyanate(TDI)), continue to stir 10min and make compound performed polymer.Open ball valve, the performed polymer that obtains is sent into double screw extruder, conveying, the polymerization of finishing compound performed polymer cause, increase, stop and remove residual monomer, and polymer through port mould is extruded then, cooling and shaping in tank, forced air drying then, granulation.
Claims (8)
1. ferrite bonded permanent magnet with excellent machinability, its composition and mass content are:
Isotropic ferrite magnetic: 80~92%
Thermoplastic resin: 15~20%
Various processing aids, magnetic modifier: 0~5%
2. ferrite bonded permanent magnet according to claim 1 is characterized in that: the basis of described ferrimagnet comprises with the iron oxide being principal phase, doped portion strontium oxide strontia.Main component is SrO6Fe
2O
3
3. ferrite bonded permanent magnet according to claim 1, it is characterized in that: described thermoplastic resin, can select nylon 11 for use, nylon 12, NYLON610, nylon 612, nylon 1010, nylon 9, one or several in the nylon 13 utilize reaction to extrude polycondensation reaction when extruding bonded permanent magnet and obtain.
4. ferrite bonded permanent magnet according to claim 1 is characterized in that: described processing aid and magnetic modifier comprise: 1. processing aid: one or several in ethylene bis stearamide, aluminum stearate, 3-phenoxy group-4-fluorobenzaldehyde, oleamide, dibutyl ester dioctyl ester, the fatty diglycollic amide.2. magnetic modifier: one or several in two (dioctyl phosphate) titanate esters of fluoroacetic acid ester, two (the two hot phosphates) titanate esters of tetra isopropyl, two (the two hot phosphates) titanate esters of tetra isopropyl, two-[r-(triethoxy is silica-based) propyl group] amine, N-β-(aminoethyl)-γ-An Bingjisanjiayangjiguiwan, N-(normal-butyl)-3-aminopropyl trimethoxysilane, the amino silane.
5. ferrite bonded permanent magnet according to claim 1 is characterized in that: the fair of processing aid is 5~10% of thermoplastic resin, and the fair of magnetic modifier is 1%~3% of magnetic.
6. ferrite bonded permanent magnet according to claim 1 is characterized in that: employed equipment has prepolymerization kettle and double screw extruder.Be furnished with each cover of mechanical type mixing plant and inflated with nitrogen and pumped vacuum systems in the prepolymerization kettle, adopting with biphenyl is the chuck heating of heating agent, and the bottom of still is controlled with ball valve, and links to each other by stainless steel pipe and double screw extruder are airtight.The draw ratio of double screw extruder is 36.
7. ferrite bonded permanent magnet according to claim 1, it is characterized in that, its preparation method is: seal charge door after then the sodium salt of a certain amount of thermoplastic resin alicyclic monomer and thermoplastic resin alicyclic monomer and NaOH and magnetic, various processing aid and magnetic modifier being added the preliminary treatment still jointly according to certain ratio, vacuumize then.The preliminary treatment still is warmed up to 100 ℃ stirs material simultaneously; this process continues 2 hours; be pressed into a certain amount of nitrogen (interior pressure-controlled is at 0.01MPa) then as protective atmosphere; continue to add a certain amount of activator (for example 2 then; the 4-2 toluene di-isocyanate(TDI)), continue to stir 10~15min and make compound performed polymer.Open ball valve, the performed polymer that obtains is sent into double screw extruder, conveying, the polymerization of finishing compound performed polymer cause, increase, stop and remove residual monomer, and polymer through port mould is extruded then, cooling and shaping in tank, forced air drying then, granulation.
8. the preparation process of ferrite bonded permanent magnet according to claim 7 is characterized in that: in extrusion, each section of double screw extruder temperature is respectively: 250 ℃, 240 ℃, 230 ℃, 220 ℃, 210 ℃, 200 ℃.
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