CN106009637B - A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch - Google Patents
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch Download PDFInfo
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Abstract
The present invention relates to magnetic material preparing technical fields, more particularly to a kind of increase-volume preparation method of permanent-magnet ferrite nylon master batch, purpose is to solve existing soft magnetic materials using the modified magnetic powder such as bulking agent, coupling agent, ineffective, magnetic powder is easily reunited, make magnetic composite magnetic property reduce the problem of.Blending is stirred magnetic powder, then be blended with the nylon 6 containing branch unit and magnetic powder using dendritic macromole first, the compatibility of magnetic powder and nylon 6 is effectively improved by dendritic macromole molecule interchain physical reactions；Different nylon materials is finally added, through batch mixing, is granulated obtained increase-volume permanent-magnet ferrite nylon master batch.The present invention, using magnetic powder and nylon masterbatch mix as soft magnetic materials bulking agent, while magnetic material compatibility is improved, does not influence magnetic material self performance for improving the compatibility of ferrite and nylon；Master batch and soft magnetism each component compatibility are good, can effectively improve the availability of ferromagnetic oxide powder, improve soft magnet performance.
Description
Technical field
The present invention relates to the preparing technical fields of magnetic material, and in particular to a kind of increase-volume permanent-magnet ferrite nylon master batch
Preparation method.
Background technology
Ferrite permanent-magnet materials are a kind of permanent-magnet materials of current dosage maximum in the world, different according to technique and ingredient,
It can be divided into Hard Magnetic and soft magnetism.Soft magnetism does not need to high temperature and pressure control since its forming technology is simple, it is easily fabricated go out size essence
Degree is high, the magnet product without secondary operation, can prepare magnet that complicated shape multipole orientation magnetizes, can be with other components entirety
Injection molding is easy to large-scale production.Therefore, the market expansion is exceedingly fast in recent years, shows good development prospect.
The magnetic property of soft magnetism depends primarily on ferrite particle material filling content and filling quality.In general, iron oxygen
Body distribution of particles is more uniform, filling content is higher, and soft magnet performance is better.Therefore, in order to improve the magnetic property of injection molded magnets, it is necessary to
Increase the particle content in ferrite particle material, still, excessively high magnetic powder loading can make the viscous of magnetic powder/binder mixtures again
Degree becomes larger, and mobility is deteriorated, finally so that magnet difficult forming during injection molding, also because magnetic powder is unevenly distributed, causes soft
Magnetic material property is greatly lowered.
At present, it in order to which soft magnetism is made still to possess preferable mobility in high-content ferrite particle, often uses and fills out
Enter insoluble auxiliary agent, including bulking agent, coupling agent, plasticizer etc..Magnetic powder can be improved to a certain extent by adding this analog assistant
Dispersion degree in high molecular material, but this analog assistant tend not to add in it is excessively high；And when magnetic powder is filled up to more than 90%,
The addition of auxiliary agent further cannot promote magnetic powder to disperse, instead to a certain extent so that magnetic powder is reunited, so as to greatly drop
The low performance of magnetic material.Such as Unexamined Patent 9-106904A, CN1645526A, CN1645526A.
Dendritic macromole is that current one kind to flourish is three-dimensional, the novel synthesis macromolecule of high-sequential.
And one amine dendritic macromole of polyamide is one of relatively broad and ripe dendritic macromole, intramolecule and end contain
There are a large amount of highly polar phthalein amine key and active amino, its low algebraically (3.0 generation of PAMAM dendritic macromoles synthesized by divergent method
Below) to open wide and of a relatively loose structure.Using this unique texture and performance, it can make its processing in polymer material should
It is played a role with aspect.
Using PAMAM dendritic macromoles, its low algebraically (below 3.0 generations) is opened wide and of a relatively loose structure and molecule
The a large amount of highly polar phthalein amine keys and active amino that internal and end is contained carry out modification of nylon 6, have new structure to reach synthesis
The purpose of nylon 6.Research shows that the obtained nylon 6 containing branch unit has good mobile performance.
The present invention carries out blending and modifying using PAMAM and the nylon 6 containing branch unit and magnetic powder, is used so as to prepare increase-volume
Permanent-magnet ferrite nylon master batch, the master batch is since main body is nylon molecules and ferrite molecule, as compatilizer for soft
Magnetic body of material has natural compatibility, is filled using the nylon 6 containing branch unit compared with short molecular chain and preferable mobile performance
When lubricant effect, the rheological property of soft-magnetic composite material can be also greatlyd improve.
At present in the domestic technology prepared about soft magnetic materials, do not occurred the nylon 6 containing branch unit, PAMAM with containing
The nylon 6 of branch unit compounds prepared soft magnetism increase-volume master batch.
Invention content
For the deficiencies in the prior art, the purpose of the present invention is to provide a kind of increase-volume permanent-magnet ferrite nylon
The preparation method of master batch, master batch prepared by this method can improve the mobility of magnetic material for soft magnetic materials, improve magnetic powder with
The compatibility of nylon molecules.
The present invention is realized by following technical proposal：
The preparation method of a kind of increase-volume permanent-magnet ferrite nylon master batch, which is characterized in that the preparation method step is such as
Under：
(1) it is surface-treated：Dendritic macromole is used to be stirred blending for additive and ferromagnetic oxide powder；
The dendritic macromole is with the novel functional polymer compound of the one kind for repeating branching unit, it is one
Class is three-dimensional, high-sequential, there is the novel macromolecule of nanoscale.Dendritic macromole can be as needed in synthesis
Its bulk of molecule, shape, structure and function group are designed, strictly controlled on a molecular scale, product is general
Symmetry is high, monodispersity is good.Dendrimer is by initially causing core, causing the radially connected repetition branching unit of core with initial
It is formed with the terminal groups being connect with outermost layer repetition branching unit.Structural unit is often repeated once as primary in dendrimer
Procreation, the algebraically of obtained product are increased by 1, therefore the number of surface functional group forms exponential increase with the increase of algebraically, most
Lead to that space surface is crowded and generates Geometrical change eventually.Generally open point when Polyamidoamine Dendrimers algebraically is relatively low
Sub- configuration, increase and branched continuation with the number of plies, is formed more closing since forth generation dendrimer more
The spherical three-dimensional structure in hole, eighth generation are then surface almost seamless spheres.And the dendrimer formation surface of high algebraically is tight
Closely packed three-dimensional structure, inner space is larger, and property is similar to micelle.
Commodity purchased in market can be used in heretofore described dendritic macromole, can also be used divergent method synthesis (Tomalia DA,
Dewald J R.US4507466,1985.).In the synthesis process, cause core using ethylenediamine to be initial.First, initially cause core
Michael addition reactions are carried out with methyl acrylate in a solvent, obtain 0.5 generation dendritic macromole product.Products therefrom is again
Amidation process is carried out with ethylenediamine in a solvent to get 1.0 generation dendritic macromoles.Such Micheal overlapping successively
Addition and each reaction step of amidation process, you can obtain the dendritic macromole that algebraically successively increases, i.e. polyamide-amide tree
Dendrimer, English entitled Polyamidoamine, referred to as PAMAM.
The dendritic macromole is preferably 1-3 for PAMAM.
(2) batch mixing：First the nylon containing branch unit is added in into the ferromagnetic oxide powder after the completion of step (1) surface treatment
6 powder, are sufficiently stirred, and are uniformly mixed；Then nylon particles are added in into mixture again, continue to be uniformly mixed；Mixed is mixed
Material, which is placed in 80-100 DEG C of vacuum drying oven, dries；
6 powder of nylon containing branch unit is in situ in autoclave for dendritic macromole and caprolactam for 1-3
Polymerisation forms, and 1-3 is 200-800nm for dendritic macromole grain size；Caprolactam and dendritic macromole in-situ polymerization
Reaction method is：By 1-3 for dendritic macromole and caprolactam using mass ratio as 1:10 ratio is added in autoclave,
Then initiator 6-aminocaprolc acid (chemistry is pure, and dosage is the 1% of caprolactam quality) is added in, mixture is in N2Atmosphere, temperature
To be reacted 2-4 hours under environment in 130 DEG C and pressure 5Mpa reaction kettles, reactant is crushed through milling up to containing branch unit
6 powder of nylon.
(3) it is granulated：Batch mixing after step (2) is dried is placed in extruding pelletization in 210-250 DEG C of single screw extrusion machine, pelletizing
Increase-volume permanent-magnet ferrite nylon master batch is obtained afterwards.
Further, it is described preparation increase-volume be with each raw material proportioning of permanent-magnet ferrite nylon master batch：
Further, the ferrite is the mixture of di-iron trioxide, magnesia and zinc oxide, and wherein di-iron trioxide accounts for
Than >=80wt%, the ferrite each component average grain diameter is 1-4 μm.
The nylon particles are preferably nylon 6, nylon66 fiber and/or nylon 12.
Compared with prior art, the advantages of the present invention are：
Existing soft magnetic materials is solved using the modified magnetic powder such as bulking agent, coupling agent, ineffective, magnetic powder is easily reunited, made
The problem of magnetic composite magnetic property reduces.The present invention is for improving the compatibility of ferrite and nylon, using magnetic powder and Buddhist nun
Imperial masterbatch mix while magnetic material compatibility is improved, does not influence magnetic material itself property as soft magnetic materials bulking agent
Energy；Master batch and soft magnetism each component compatibility are good, effectively increase the availability of ferromagnetic oxide powder, improve soft magnetism
Energy.
Specific embodiment
Present patent application is described further with reference to specific embodiment, but the protection domain of present patent application is unlimited
In this.
Dendritic macromole is synthetically prepared using divergent method into (Tomalia described in the following embodiment of the present invention
DA, Dewald J R.US4507466,1985.).In the synthesis process, cause core using ethylenediamine to be initial.First, initially draw
It sends out core and carries out Michael addition reactions with methyl acrylate in a solvent, obtain 0.5 generation dendritic macromole product.Gained produces
Object carries out amidation process to get 1.0 generation dendritic macromoles with ethylenediamine in a solvent again.It is so overlapping successively
Micheal additions and each reaction step of amidation process, you can obtain the dendritic macromole that algebraically successively increases, i.e. polyamides
Amine-amine dendrimer, English entitled Polyamidoamine, referred to as PAMAM.
6 powder of nylon containing branch unit is in situ in autoclave for dendritic macromole and caprolactam for 1-3
Polymerisation forms, and 1-3 is 200-800nm for dendritic macromole grain size；Caprolactam and dendritic macromole in-situ polymerization
Reaction method is：By 1-3 for dendritic macromole and caprolactam using mass ratio as 1:10 ratio is added in autoclave,
Then initiator 6-aminocaprolc acid (chemistry is pure, and dosage is the 1% of caprolactam quality) is added in, mixture is in N2Atmosphere, temperature
To be reacted 2-4 hours under environment in 130 DEG C, pressure 5Mpa reaction kettles, reactant is crushed through milling up to the Buddhist nun containing branch unit
Imperial 6 powder.
Embodiment 1：
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch：
Taking 50Kg ferromagnetic oxide powders, (di-iron trioxide accounts for 85wt%, magnesia accounts for 10wt%, zinc oxide accounts for 5wt%, mixing
Object each component average grain diameter is 1-4 μm), it adds in 0.5Kg generation PAMAM and blending and modifying is stirred to ferromagnetic oxide powder surface
(concrete operations are：0.5Kg generation PAMAM and 50Kg ferromagnetic oxide powders are placed in stirring infiltration blending in high speed mixer), so
Adding in nylon 6 powder of the 13.5Kg containing branch unit afterwards, (dendritic macromole that the nylon 6 containing branch unit is added is one
For PAMAM) it is blended, it is sufficiently stirred, it is ensured that be uniformly mixed；Then 36Kg nylon 6 is added in into mixture, it is mixed to continue stirring
It closes uniformly, mixed batch mixing is placed in 80 DEG C of vacuum drying ovens, dry.
Batch mixing after drying is granulated in 210 DEG C of single screw extrusion machine, rate of feeding 2.0m/min, and screw speed is
80 turns/min, extrusion molding is carried out, after then being cooled down by conveyer belt, the particle of diameter 2mm, length 3mm are cut into pulverizer
Material, as prepared increase-volume permanent-magnet ferrite nylon master batch.
By prepared 3kg increase-volumes permanent-magnet ferrite nylon master batch, 90kg magnetic powders (ferromagnetic oxide powder, wherein three oxidations
Two iron account for 85wt%, magnesia accounts for 10wt%, zinc oxide accounts for 5wt%, and mixture each component average grain diameter is 1-4 μm) and 7kg Buddhist nun
Imperial 6 particles are placed in blended under agitation in homogenizer, and blend prepares magnetic material through single screw extrusion machine extrusion, and obtained is soft
Magnetic material granule is put into fusion index instrument, tests the melt index (MFI) of particle, and test condition is 250 DEG C, load 2.5kg.
Data are shown in Table 1.
Embodiment 2：
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch：
Taking 30Kg ferromagnetic oxide powders, (di-iron trioxide accounts for 80wt%, magnesia accounts for 10wt%, zinc oxide accounts for 10wt%, mixes
It is 1-4 μm to close object each component average grain diameter), it adds in 1.0Kg bis- generations PAMAM and blending and modifying is stirred to ferromagnetic oxide powder surface
(concrete operations are：Bis- generations of 1.0Kg PAMAM and 30Kg ferromagnetic oxide powders are placed in stirring infiltration blending in high speed mixer), so
Adding in nylon 6 powder of the 9Kg containing branch unit afterwards, (dendritic macromole that the nylon 6 containing branch unit is added was two generations
PAMAM it) is blended, is sufficiently stirred, it is ensured that is uniformly mixed；Then 60Kg nylon66 fibers are added in into mixture, it is mixed to continue stirring
It closes uniformly, mixed batch mixing is placed in 85 DEG C of vacuum drying ovens, dry.
Batch mixing after drying is granulated in 220 DEG C of single screw extrusion machine, rate of feeding 2.0m/min, and screw speed is
80 turns/min, extrusion molding is carried out, after then being cooled down by conveyer belt, the particle of diameter 2mm, length 3mm are cut into pulverizer
Material, as prepared increase-volume permanent-magnet ferrite nylon master batch.
By prepared 3kg increase-volumes permanent-magnet ferrite nylon master batch, 90kg magnetic powders (ferromagnetic oxide powder, wherein three oxidations
Two iron account for 80wt%, magnesia accounts for 10wt%, zinc oxide accounts for 10wt%, and mixture each component average grain diameter is 1-4 μm) and 7kg
Nylon66 fiber particle is placed in blended under agitation in homogenizer, and blend prepares magnetic material through single screw extrusion machine extrusion, obtained
Soft magnetic materials particle be put into fusion index instrument, test the melt index (MFI) of particle, test condition is 250 DEG C, load
2.5kg.Data are shown in Table 1.
Embodiment 3：
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch：
Taking 60Kg ferromagnetic oxide powders, (di-iron trioxide accounts for 90wt%, magnesia accounts for 5wt%, zinc oxide accounts for 5wt%, mixing
Object each component average grain diameter is 1-4 μm), it adds in 2.0Kg three generations PAMAM and blending and modifying is stirred to ferromagnetic oxide powder surface
(concrete operations are：2.0Kg three generations's PAMAM and 60Kg ferromagnetic oxide powders are placed in stirring infiltration blending in high speed mixer), so
Adding in nylon 6 powder of the 18Kg containing branch unit afterwards, (dendritic macromole that the nylon 6 containing branch unit is added is three generations
PAMAM it) is blended, is sufficiently stirred, it is ensured that is uniformly mixed；Then 20Kg nylon 12 is added in into mixture, it is mixed to continue stirring
It closes uniformly, mixed batch mixing is placed in 90 DEG C of vacuum drying ovens, dry.
Batch mixing after drying is granulated in 235 DEG C of single screw extrusion machine, rate of feeding 2.0m/min, and screw speed is
80 turns/min, extrusion molding is carried out, after then being cooled down by conveyer belt, the particle of diameter 2mm, length 3mm are cut into pulverizer
Material, as prepared increase-volume permanent-magnet ferrite nylon master batch.
By prepared 3kg increase-volumes permanent-magnet ferrite nylon master batch, 90kg magnetic powders (ferromagnetic oxide powder, wherein three oxidations
Two iron account for 90wt%, magnesia accounts for 5wt%, zinc oxide accounts for 5wt%, and mixture each component average grain diameter is 1-4 μm) and 7kg Buddhist nun
Imperial 12 particles are placed in blended under agitation in homogenizer, and blend prepares magnetic material through single screw extrusion machine extrusion, obtained
Soft magnetic materials particle is put into fusion index instrument, tests the melt index (MFI) of particle, and test condition is 250 DEG C, load
2.5kg.Data are shown in Table 1.
Embodiment 4：
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch：
Taking 55Kg ferromagnetic oxide powders, (di-iron trioxide accounts for 95wt%, magnesia accounts for 2wt%, zinc oxide accounts for 3wt%, mixing
Object each component average grain diameter is 1-4 μm), it adds in 1.5Kg bis- generations PAMAM and blending and modifying is stirred to ferromagnetic oxide powder surface
(concrete operations are：Bis- generations of 1.5Kg PAMAM and 55Kg ferromagnetic oxide powders are placed in stirring infiltration blending in high speed mixer), so
Adding in nylon 6 powder of the 13.5Kg containing branch unit afterwards, (dendritic macromole that the nylon 6 containing branch unit is added is two
For PAMAM) it is blended, it is sufficiently stirred, it is ensured that be uniformly mixed；Then 30Kg nylon 12 and nylon 6 are added in into mixture
Mixture (nylon 12：Nylon 6=1:1, mass ratio), continue to be uniformly mixed, mixed batch mixing is placed in 95 DEG C of vacuum dries
In case, drying.
Batch mixing after drying is granulated in 240 DEG C of single screw extrusion machine, rate of feeding 2.0m/min, and screw speed is
80 turns/min, extrusion molding is carried out, after then being cooled down by conveyer belt, the particle of diameter 2mm, length 3mm are cut into pulverizer
Material, as prepared increase-volume permanent-magnet ferrite nylon master batch.
By prepared 3kg increase-volumes permanent-magnet ferrite nylon master batch, 90kg magnetic powders (ferromagnetic oxide powder, wherein three oxidations
Two iron account for 95wt%, magnesia accounts for 2wt%, zinc oxide accounts for 3wt%, and mixture each component average grain diameter is 1-4 μm) and 7kg Buddhist nun
Imperial 12 particles are placed in blended under agitation in homogenizer, and blend prepares magnetic material through single screw extrusion machine extrusion, obtained
Soft magnetic materials particle is put into fusion index instrument, tests the melt index (MFI) of particle, and test condition is 250 DEG C, load
2.5kg.Data are shown in Table 1.
Embodiment 5：
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch：
Taking 40Kg ferromagnetic oxide powders, (di-iron trioxide accounts for 85wt%, magnesia accounts for 5wt%, zinc oxide accounts for 10wt%, mixing
Object each component average grain diameter is 1-4 μm), it adds in 1.8Kg three generations PAMAM and blending and modifying is stirred to ferromagnetic oxide powder surface
(concrete operations are：1.8Kg three generations's PAMAM and 40Kg ferromagnetic oxide powders are placed in stirring infiltration blending in high speed mixer), so
Adding in nylon 6 powder of the 10.2Kg containing branch unit afterwards, (dendritic macromole that the nylon 6 containing branch unit is added is three
For PAMAM) it is blended, it is sufficiently stirred, it is ensured that be uniformly mixed；Then 48Kg nylon66 fibers and nylon 6 are added in into mixture
Mixture (nylon66 fiber：Nylon 6=2:1, mass ratio), continue to be uniformly mixed, mixed batch mixing is placed in 100 DEG C of vacuum dries
In case, drying.
Batch mixing after drying is granulated in 245 DEG C of single screw extrusion machine, rate of feeding 2.0m/min, and screw speed is
80 turns/min, extrusion molding is carried out, after then being cooled down by conveyer belt, the particle of diameter 2mm, length 3mm are cut into pulverizer
Material, as prepared increase-volume permanent-magnet ferrite nylon master batch.
By prepared 3kg increase-volumes permanent-magnet ferrite nylon master batch, 90kg magnetic powders (ferromagnetic oxide powder, wherein three oxidations
Two iron account for 85wt%, magnesia accounts for 5wt%, zinc oxide accounts for 10wt%, and mixture each component average grain diameter is 1-4 μm) and 7kg Buddhist nun
Imperial 66 particles are placed in blended under agitation in homogenizer, and blend prepares magnetic material through single screw extrusion machine extrusion, obtained
Soft magnetic materials particle is put into fusion index instrument, tests the melt index (MFI) of particle, and test condition is 250 DEG C, load
2.5kg.Data are shown in Table 1.
Embodiment 6：
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch：
Taking 45Kg ferromagnetic oxide powders, (di-iron trioxide accounts for 85wt%, magnesia accounts for 7wt%, zinc oxide accounts for 8wt%, mixing
Object each component average grain diameter is 1-4 μm), it adds in 1.2Kg generation PAMAM and blending and modifying is stirred to ferromagnetic oxide powder surface
(concrete operations are：1.2Kg generation PAMAM and 45Kg ferromagnetic oxide powders are placed in stirring infiltration blending in high speed mixer), so
Adding in nylon 6 powder of the 13.8Kg containing branch unit afterwards, (dendritic macromole that the nylon 6 containing branch unit is added is one
For PAMAM) it is blended, it is sufficiently stirred, it is ensured that be uniformly mixed；Then 40Kg nylon66 fibers and nylon 12 are added in into mixture
Mixture (nylon66 fiber：Nylon 12=3:2, mass ratio), continue to be uniformly mixed, mixed batch mixing is placed in 80 DEG C of vacuum dries
In case, drying.
Batch mixing after drying is granulated in 250 DEG C of single screw extrusion machine, rate of feeding 2.0m/min, and screw speed is
80 turns/min, extrusion molding is carried out, after then being cooled down by conveyer belt, the particle of diameter 2mm, length 3mm are cut into pulverizer
Material, as prepared increase-volume permanent-magnet ferrite nylon master batch.
By prepared 3kg increase-volumes permanent-magnet ferrite nylon master batch, 90kg magnetic powders (ferromagnetic oxide powder, wherein three oxidations
Two iron account for 85wt%, magnesia accounts for 7wt%, zinc oxide accounts for 8wt%, and mixture each component average grain diameter is 1-4 μm) and 7kg Buddhist nun
Imperial 12 particles are placed in blended under agitation in homogenizer, and blend prepares magnetic material through single screw extrusion machine extrusion, obtained
Soft magnetic materials particle is put into fusion index instrument, tests the melt index (MFI) of particle, and test condition is 250 DEG C, load
2.5kg.Data are shown in Table 1.
Comparative example：
A kind of preparation method of increase-volume permanent-magnet ferrite nylon master batch：
Taking 50Kg ferromagnetic oxide powders, (di-iron trioxide accounts for 88wt%, magnesia accounts for 6wt%, zinc oxide accounts for 6wt%, mixing
Object each component average grain diameter is 1-4 μm), it adds in 2.0Kg bis- generations PAMAM and blending and modifying is stirred to ferromagnetic oxide powder surface
(concrete operations are：Bis- generations of 2.0Kg PAMAM and 50Kg ferromagnetic oxide powders are placed in stirring infiltration blending in high speed mixer), so
6 powder of 18Kg nylon is added in afterwards to be blended, and is sufficiently stirred, it is ensured that be uniformly mixed；Then 30Kg nylon is added in into mixture
66, continue to be uniformly mixed, mixed batch mixing is placed in 80 DEG C of vacuum drying ovens, dry.
Batch mixing after drying is granulated in 230 DEG C of single screw extrusion machine, rate of feeding 2.0m/min, and screw speed is
80 turns/min, extrusion molding is carried out, after then being cooled down by conveyer belt, the particle of diameter 2mm, length 3mm are cut into pulverizer
Material, as prepared increase-volume permanent-magnet ferrite nylon master batch.
By prepared 3kg increase-volumes permanent-magnet ferrite nylon master batch, 90kg magnetic powders (ferromagnetic oxide powder, wherein three oxidations
Two iron account for 88wt%, magnesia accounts for 6wt%, zinc oxide accounts for 6wt%, and mixture each component average grain diameter is 1-4 μm) and 7kg Buddhist nun
Imperial 66 particles are placed in blended under agitation in homogenizer, and blend prepares magnetic material through single screw extrusion machine extrusion, obtained
Soft magnetic materials particle is put into fusion index instrument, tests the melt index (MFI) of particle, and test condition is 250 DEG C, load
2.5kg.Data are shown in Table 1.
Above-described embodiment 1-6 and comparative example the soft magnetic materials particle prepared are put into injection molding machine, 245 DEG C of injection temperature,
Injection pressure 50kg/cm2, dwell time 10.0s, molding when add the alignment magnetic field of 100000e, be injected into outer diameter 3m, high 1cm
Standard sample, to test its magnetic property.Data are shown in Table 1.
1 comparative example of table and each embodiment magnetic property, melt index correction data
More than test result shows：It is added to increase-volume permanent-magnet ferrite by the use of the nylon containing branch unit as lubricant
Nylon master batch and soft-magnetic composite material, melt index (MFI) reach more than 33g/10min, are added with pure nylon as lubricant
It is compared to increase-volume with the melt index of permanent-magnet ferrite nylon master batch and soft-magnetic composite material (MFI) 21.1g/10min, soft magnetism is multiple
Condensation material rheological characteristic significantly improves.In addition, it is also indicated that from 1 magnetism testing of table, the soft magnetism composite wood of the nylon containing branch unit
The every magnetic property of material is also significantly better than the soft-magnetic composite material of pure nylon；The soft magnetism composite wood of this nylon of the explanation containing branch unit
Also the soft-magnetic composite material of purer nylon will be got well for the magnetic powder distribution of material.Increase-volume permanent magnetism prepared by nylon containing branch unit
Ferrite nylon master batch is added to soft-magnetic composite material so that soft magnetic materials also ensures that soft while high magnetic powder loading
The performances such as there is magnetic material good mobility, magnetic powder to be evenly distributed, excellent magnetic property.
Claims (4)
1. a kind of increase-volume preparation method of permanent-magnet ferrite nylon master batch, which is characterized in that the preparation method step is as follows：
（1）Surface treatment：Dendritic macromole is used to be stirred blending for additive and ferromagnetic oxide powder；
（2）Batch mixing：First to step（1）6 powder of nylon containing branch unit is added in ferromagnetic oxide powder after the completion of surface treatment
End is sufficiently stirred, and is uniformly mixed；Then nylon particles are added in into mixture again, continue to be uniformly mixed；Mixed batch mixing is put
It is dried in 80-100 DEG C of vacuum drying oven；
6 powder of nylon containing branch unit is 1-3 for dendritic macromole and caprolactam in-situ polymerization in autoclave
It reacts；
（3）It is granulated：By step（2）Batch mixing after drying is placed in extruding pelletization in 210-250 DEG C of single screw extrusion machine, after pelletizing
Increase-volume permanent-magnet ferrite nylon master batch；
It is described preparation increase-volume be with each raw material proportioning of permanent-magnet ferrite nylon master batch：
Material quality percentage
Ferromagnetic oxide powder 30wt%-60wt%,
Dendritic macromole 0.5wt%-2.0wt%,
6 powder 9wt%-20wt% of nylon containing branch unit,
Nylon particles 20wt%-55wt%；
The dendritic macromole is polyamide-amide dendrimer PAMAM；
The caprolactam and dendritic macromole home position polymerization reaction method are：By 1-3 for dendritic macromole and interior acyl
Amine is using mass ratio as 1:10 ratio is added in autoclave, then adds in initiator 6-aminocaprolc acid, mixture is in N2Atmosphere
Enclose, temperature is react 2-4 hour under environment in 130 DEG C and pressure 5Mpa reaction kettles, reactant crushes to set up to containing through milling
6 powder of nylon of branch unit.
2. preparation method according to claim 1, it is characterised in that：The step（1）The dendritic macromole used for
1-3 is for PAMAM.
3. preparation method according to claim 1 or 2, it is characterised in that：The ferrite is di-iron trioxide, magnesia
With the mixture of zinc oxide, wherein di-iron trioxide accounting >=80wt%, the ferrite each component average grain diameter is 1-4 μm.
4. preparation method according to claim 1 or 2, it is characterised in that：The nylon particles for nylon 6, nylon66 fiber and/
Or nylon 12.
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| CN101148506A (en) * | 2007-11-02 | 2008-03-26 | 湖南大学 | Method for producing high-fluidity nylon 6 |
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| CN101148506A (en) * | 2007-11-02 | 2008-03-26 | 湖南大学 | Method for producing high-fluidity nylon 6 |
| CN101864167A (en) * | 2007-11-13 | 2010-10-20 | 中国科学院金属研究所 | Magnetic iron oxide-dendritic polyamide core-shell nano complex and preparation thereof |
| CN104194325A (en) * | 2014-09-17 | 2014-12-10 | 中山大学 | Preparing method of heat-conductive and injection-molded magnetic composite |
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