CN105397082B - A kind of magnetic material is molded particle masterbatch preparation process - Google Patents

A kind of magnetic material is molded particle masterbatch preparation process Download PDF

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CN105397082B
CN105397082B CN201510870090.4A CN201510870090A CN105397082B CN 105397082 B CN105397082 B CN 105397082B CN 201510870090 A CN201510870090 A CN 201510870090A CN 105397082 B CN105397082 B CN 105397082B
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nylon
magnetic
magnetic material
preparation process
particle masterbatch
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CN105397082A (en
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胡江平
金志洪
郭超阳
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

Particle masterbatch preparation process is molded the invention discloses a kind of magnetic material, is comprised the following steps:(1) nylon is added in nylon solvent, stirring to nylon is completely dissolved, obtain nylon solution, by 80~90% magnetics, 9~17% nylon solutions, 0.1~3% surface conditioning agent, the weight/mass percentage composition proportioning of 0.05~0.1% lubricant (each component mass percent sum is 100%) weighs each component, stand-by;(2) after 30~40min, 10~20min of nylon solution and mix lubricant is added;(3) mixed material is used after banbury banburying, producing magnetic material by jaw crushing crusher machine is molded particle masterbatch.Present invention process step is simple, and nylon is added in the form of nylon solution, nylon is fully combined with magnetic, therefore nylon is made to be combined with magnetic without carrying out granulation by high-temperature heating, energy consumption can be reduced, is avoided that magnetic is aoxidized because of high temperature again, while easily shaping.

Description

A kind of magnetic material is molded particle masterbatch preparation process
Technical field
The present invention relates to magnetic materials production technical field, it is molded particle masterbatch more particularly, to a kind of magnetic material and prepares Method.
Background technology
Magnetic, high polymer binder, auxiliary agent are kneaded according to a certain percentage, granulated, pellet is then passed through into note again Penetrate the machine magnet that injection molding method is prepared at a proper temperature and be referred to as injection molded magnets.Such magnet is used as bonding magnetic One important branch of body, due to dimensional accuracy height, good mechanical property, the magnetic that complicated shape multipole orientation magnetizes can be prepared Body, can with the shaping of other part integral molded plastics, be easy to large-scale production the advantages of, be widely used in household electrical appliance, automobile, logical Believe the fields such as equipment, instrumentation, computer, office equipment.In recent years, as Chinese industrial is automated and the modernization of information Develop rapidly, injection moulding magnet as electronics industry and information industry a kind of important functional material, with wide hair Open up space.
The development of injection molded magnets device starts from 1980s, so far the history of more than 20 years, but be due to injection The complexity and particularity of magnet generation technique, it is desirable to grasp magnetic material, macromolecular material, machinery, electronics etc. many Technology, only the U.S., Japan and European a small number of advanced industrial countries just possess the industrialization that high-performance is molded magnetic device at present Production capacity.The development of more than 20 years is passed through by domestic injection magnetic device producer, although also achieve larger progress, but it is noted The integrated production capacity for moulding magnetic, kneading machine, mould magnetic Circuit Design, resin and auxiliary agent still differs greatly with Foreign Advanced Lerel.
Compared with ferrite and shirt cobalt permanent magnet, third generation rare-earth Nd-Fe-B permanent magnet has more excellent magnetic property, Show as high saturated pole intensity, high-coercive force, high energy product.With development in science and technology, client will to injecting magnetic device performance The continuous improvement asked, causes the demand of the injection particulate material masterbatch produced with neodymium iron boron increasing, but such injection magnetic device The production technology of the masterbatch of production is all monopolized by external manufacturing enterprise substantially, and injection magnetic device producer of the country is required for passing through substantially External import particulate material masterbatch could carry out the production of such high-end product.
Existing domestic production injection neodymium iron boron particles material is primarily present problem:1st, particle need to be granulated by high temperature and is made, Prilling temperature is 220 DEG C, neodymium iron boron particles material easy high-temperature oxydation in itself, and in particulate material granulation process, NdFeB magnetic powder is easy High-temperature oxydation influences the magnetic property of particulate material;2nd, binding agent dispersing uniformity is poor, and the associativity of NdFeB magnetic powder and binding agent is poor, The particulate material stability and mobility of production is not good.
The content of the invention
The present invention is to be molded the easy high-temperature oxydation of particle masterbatch, the particulate material of production to solve the magnetic material of prior art The problem of stability and poor fluidity, is simple there is provided a kind of processing step, can reduce energy consumption, it is to avoid magnetic is aoxidized, and is more easy into The magnetic material injection particle masterbatch preparation process of type.
To achieve these goals, the present invention uses following technical scheme:
A kind of magnetic material is molded particle masterbatch preparation process, comprises the following steps:
(1) 80~90% magnetics are pressed, 9~17% nylon, 0.1~3% surface conditioning agent, 0.05~0.1% lubricant is (each Constituent mass percentage sum weighs each component for weight/mass percentage composition proportioning 100%), stand-by.
The amount of nylon solvent is not particularly limited, and is completely dissolved with nylon.
(2) nylon is added in nylon solvent, stirring is completely dissolved to nylon, obtains nylon solution.The amount of nylon solvent with Nylon is completely dissolved.
(3) surface conditioning agent is added in magnetic to mix after 30~40min, add nylon solution and mix lubricant 10~ 20min.Add surface conditioning agent in magnetic to be surface-treated, to avoid magnetic from reuniting;Nylon uses nylon in the present invention The form of solution is added, and nylon is fully combined with magnetic, therefore makes nylon and magnetic without carrying out granulation by high-temperature heating Powder is combined, and can reduce energy consumption, moreover it is possible to avoid magnetic from being aoxidized because of high temperature.
(4) mixed material is used after banbury banburying, producing magnetic material by jaw crushing crusher machine is molded Particle masterbatch.The present invention has abandoned traditional high temperature granulation step, not only processing step is more simple using banburying mixing, and And energy consumption can be reduced, it is to avoid magnetic is aoxidized, more easy-formation.
Preferably, in step (1), the nylon is the powder of nylon 6 and/or the powder of nylon 12.
Preferably, in step (2), the nylon solvent is formic acid, metacresol, trifluoroethanol, phenol and HFC-134a Mixed solvent, dimethylformamide, the one or more in the mixed solvent of cyclohexanone and dimethyl n butanol.
Preferably, the mass ratio of phenol and HFC-134a is 1 in the mixed solvent of the phenol and HFC-134a:1, ring Ketone is 7 with the mass ratio of dimethyl n butanol with cyclohexanone in the mixed solvent of dimethyl n butanol:3.
Preferably, in step (1), the magnetic is NdFeB magnetic powder or ferromagnetic oxide powder.
Preferably, in step (1), the surface conditioning agent is phosphate coupling agent, titanate coupling agent, silane coupled One or more in agent, aluminate coupling agent.
Preferably, in step (1), the lubricant is ethylene bis stearic acid amide, paraffin, calcium stearate, stearic acid One or more in magnesium.
Preferably, in step (3), the surface conditioning agent is mixed to form after mixed solution with absolute ethyl alcohol or isopropanol Use, absolute ethyl alcohol or the percent by volume shared by isopropanol are 65~85% in mixed solution.Surface conditioning agent and anhydrous second Alcohol or isopropanol are used in mixed way, to improve its dispersing uniformity, while absolute ethyl alcohol or isopropanol are volatile, are easily removed, ethanol Or the amount of isopropanol is so that surface conditioning agent is completely dissolved is advisable.
Preferably, in step (3), the temperature that addition surface conditioning agent is mixed in magnetic is 80~110 DEG C.Temperature Control is at 80~110 DEG C, so that solvent volatilizees completely.
Preferably, in step (4), mixing temperature is 95~100 DEG C.Mixing temperature controls 95~100 DEG C, both can guarantee that Shaping, is avoided that magnetic is aoxidized again.
Therefore, the present invention has the advantages that:Nylon is added in the form of nylon solution, enables nylon and magnetic Fully combine, therefore nylon is combined with magnetic without carrying out granulation by high-temperature heating, processing step is simple, can reduce energy Consumption, is avoided that magnetic is aoxidized because of high temperature again, while easily shaping.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
(1) 80% magnetic (ferromagnetic oxide powder), 16.9% nylon (powder of nylon 12), 3% surface conditioning agent (phosphate are pressed Coupling agent), the weight/mass percentage composition proportioning of 0.1% lubricant (ethylene bis stearic acid amide) weighs each component, stand-by;
(2) nylon is added in nylon solvent (formic acid), stirring is completely dissolved to nylon, obtains nylon solution;
(3) surface conditioning agent and absolute ethyl alcohol are mixed to form into mixed solution to add in magnetic, mixed at 80 DEG C of temperature After 40min, adding the percent by volume in nylon solution and mix lubricant 20min, mixed solution shared by absolute ethyl alcohol is 65%.
(4) use banbury in after 95 DEG C of banburyings mixed material, magnetic material is produced by jaw crushing crusher machine Material injection particle masterbatch.
Embodiment 2
(1) 90% magnetic (NdFeB magnetic powder), 9% nylon (powder of nylon 6), 0.95% surface conditioning agent (phosphate are pressed Coupling agent and silane coupler mass ratio 1:3), (ethylene bis stearic acid amide is 1 with Quality of Paraffin Waxes ratio to 0.05% lubricant:1) Weight/mass percentage composition proportioning weigh each component, it is stand-by;
(2) nylon is added into nylon solvent (mixed solvent of phenol and HFC-134a, phenol is with HFC-134a mass ratio 1:1) in, stirring is completely dissolved to nylon, obtains nylon solution;
(3) surface conditioning agent and isopropanol are mixed to form into mixed solution to add in magnetic, mixed at 110 DEG C of temperature After 30min, it is 65% to add the percent by volume in nylon solution and mix lubricant 10min, mixed solution shared by isopropanol.
(4) use banbury in after 100 DEG C of banburyings mixed material, magnetic material is produced by jaw crushing crusher machine Material injection particle masterbatch.
Embodiment 3
(1) 82.81% magnetic (NdFeB magnetic powder) is pressed, (powder of nylon 6 and the powder of nylon 12, mass ratio is 17% nylon 1:1), (titanate coupling agent and aluminate coupling agent, mass ratio are 1 to 0.1% surface conditioning agent:1), 0.09% lubricant is (hard Resin acid calcium and magnesium stearate, mass ratio 1:3) weight/mass percentage composition proportioning weighs each component, stand-by;
(2) nylon is added into nylon solvent (trifluoroethanol, dimethylformamide and cyclohexanone, mass ratio 1:3:1) in, stirring It is completely dissolved to nylon, obtains nylon solution;
(3) surface conditioning agent and absolute ethyl alcohol are mixed to form into mixed solution to add in magnetic, mixed at 100 DEG C of temperature After 35min, adding the percent by volume in nylon solution and mix lubricant 15min, mixed solution shared by absolute ethyl alcohol is 70%.
(4) use banbury in after 98 DEG C of banburyings mixed material, magnetic material is produced by jaw crushing crusher machine Material injection particle masterbatch.
Embodiment 4
(1) 85% magnetic (ferromagnetic oxide powder), 12% nylon (powder of nylon 12), 2.93% surface conditioning agent (phosphoric acid are pressed Ester coupling agent), the weight/mass percentage composition proportioning of 0.07% lubricant (ethylene bis stearic acid amide) weighs each component, stand-by;
(2) nylon is added into nylon solvent (mixed solvent of cyclohexanone and dimethyl n butanol, cyclohexanone and dimethyl n The mass ratio of butanol is 7:3) in, stirring is completely dissolved to nylon, obtains nylon solution;
(3) surface conditioning agent and absolute ethyl alcohol are mixed to form into mixed solution to add in magnetic, mixed at 110 DEG C of temperature After 30min, it is 65 to add the percent by volume in nylon solution and mix lubricant 15min, mixed solution shared by absolute ethyl alcohol ~85%.
(4) use banbury in after 100 DEG C of banburyings mixed material, magnetic material is produced by jaw crushing crusher machine Material injection particle masterbatch.
Particle masterbatch made from the various embodiments described above is put into injection machine, 275 DEG C of injection temperature, injection pressure 75kg/ cm2, the dwell time be 5.0S, be injected into external diameter 3.2cm, internal diameter 1.2cm, high 1cm cylinder ring carry out compressive strength determination;And By injection machine molded samples, molded samples size is diameter 3cm, high 1cm standard sample post, 315 DEG C of forming temperature, during shaping All plus 10000Oe alignment magnetic field;Its melt and dissolved index measurement temperature is 270 DEG C, is incubated under 10min, pressure 10kg and measures.Data It is shown in Table 1.
The magnetic property for the molded samples that each embodiment of table 1 is made, compression strength, melt and dissolved index contrast data
Embodiment described above is a kind of preferably scheme of the present invention, not makees any formal to the present invention Limitation, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.

Claims (7)

1. a kind of magnetic material is molded particle masterbatch preparation process, it is characterised in that comprise the following steps:
(1) by 80~90% magnetics, 9~17% nylon solutions, 0.1~3% surface conditioning agent, 0.05~0.1% lubricant Weight/mass percentage composition proportioning weighs each component, and each component mass percent sum is 100%, stand-by;
(2) nylon is added in nylon solvent, stirring is completely dissolved to nylon, obtains nylon solution;
(3) surface conditioning agent and absolute ethyl alcohol or isopropanol are mixed to form after mixed solution and added in magnetic, at 80~110 DEG C After 30~40min of lower mixing, absolute ethyl alcohol or isopropyl in 10~20min of nylon solution and mix lubricant, mixed solution are added Percent by volume shared by alcohol is 65~85%;
(4) mixed material is used after banbury banburying, producing magnetic material by jaw crushing crusher machine is molded particle Masterbatch, mixing temperature is 95~100 DEG C.
2. a kind of magnetic material injection particle masterbatch preparation process according to claim 1, it is characterised in that step (1) In, the nylon is the powder of nylon 6 and/or the powder of nylon 12.
3. a kind of magnetic material injection particle masterbatch preparation process according to claim 1, it is characterised in that step (1) In, the nylon solvent is the mixed solvent, dimethylformamide, ring of formic acid, metacresol, trifluoroethanol, phenol and HFC-134a One or more in the mixed solvent of ketone and dimethyl n butanol.
4. a kind of magnetic material injection particle masterbatch preparation process according to claim 3, it is characterised in that the phenol Mass ratio with phenol and HFC-134a in the mixed solvent of HFC-134a is 1:1, the mixing of cyclohexanone and dimethyl n butanol Cyclohexanone and the mass ratio of dimethyl n butanol are 7 in solvent:3.
5. a kind of magnetic material injection particle masterbatch preparation process according to claim 1, it is characterised in that step (1) In, the magnetic is NdFeB magnetic powder or ferromagnetic oxide powder.
6. a kind of magnetic material injection particle masterbatch preparation process according to claim 1, it is characterised in that step (1) In, the surface conditioning agent is one kind in phosphate coupling agent, titanate coupling agent, silane coupler, aluminate coupling agent Or it is a variety of.
7. a kind of magnetic material injection particle masterbatch preparation process according to claim 1, it is characterised in that step (1) In, the lubricant is the one or more in ethylene bis stearic acid amide, paraffin, calcium stearate, magnesium stearate.
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CN106009637B (en) * 2016-05-27 2018-06-19 湖北工程学院 A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch
CN106205940A (en) * 2016-07-07 2016-12-07 金华九禾磁电科技有限公司 A kind of plastic magnetic rotor and preparation method thereof
CN106384641A (en) * 2016-11-29 2017-02-08 杭州千石科技有限公司 Polymer/cerium-neodymium-iron-boron magnetic composite material and preparation method thereof
CN106890995A (en) * 2017-02-23 2017-06-27 深圳市卡德姆科技有限公司 A kind of metal injection molded forming and sintering preparation method of catalysis degreasing type feeding
CN109433391B (en) * 2018-11-05 2021-04-16 中国科学院宁波材料技术与工程研究所 Preparation method of magnetic composite powder

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JPH0837106A (en) * 1994-05-19 1996-02-06 Bridgestone Corp Magnetic powder for bonded magnet, composition for bonded magnet and manufacture thereof
JPH11340021A (en) * 1998-05-21 1999-12-10 Sumitomo Metal Mining Co Ltd Bonded magnet material and molded bonded magnet
CN100461306C (en) * 2005-10-18 2009-02-11 四川大学 Bonding type compound permanent-magnet material comprising Sm-Fe-N and Nd-Fe-N and preparation method thereof
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