CN108301065A - The long-acting strong magnetic staple fiber and its small lot preparation method of rare earth permanent-magnetic material - Google Patents
The long-acting strong magnetic staple fiber and its small lot preparation method of rare earth permanent-magnetic material Download PDFInfo
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- CN108301065A CN108301065A CN201810089802.2A CN201810089802A CN108301065A CN 108301065 A CN108301065 A CN 108301065A CN 201810089802 A CN201810089802 A CN 201810089802A CN 108301065 A CN108301065 A CN 108301065A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to the long-acting strong magnetic staple fibers and its small lot preparation method of a kind of rare earth permanent-magnetic material.It is characterized in that preparing magnetic material not instead of single component used in the method for magnetic staple fiber, rare-earth magnetic composition, this method is suitable for small lot production in addition.First prepare rare-earth magnetic composition and magnetic master batch before spinning, magnetic master batch is added to by when spinning by a certain percentage can spin the magnetic staple fiber containing different particle contents in resin slicer.The rare-earth magnetic composition that the method uses can not only make magnetic material have better stability and magnetism; and any influence is not present to processing performance when being used to prepare magnetic master batch or spinning permanent magnetism staple fiber; so that the magnetic staple fiber magnetic induction intensity prepared is strong, it is at low cost.
Description
Technical field
The present invention relates to functional fibre fields, a kind of long-acting strong magnetic staple fiber more particularly to rare earth permanent-magnetic material and its
Preparation method.
Background technology
With the development of magnetic therapy technology and sanitary health career, the textile with magnetic therapy functions has been developed and throws
Enter to use.The mechanism of magnetic therapy is commonly considered as：Magnetic field promotes cycle, activation biological enzyme, control blood by reducing body fluid viscosity
The movement etc. of Lactoferrin offsets silt and subtracts swollen anti-inflammatory, reduce wound cicatrix, slow down pain, improve sleep, alleviation depression etc.
With reliable curative effect, and it is safe, noninvasive, nontoxic, for magnetostatic field, even if magnetic induction intensity reaches 2000G, to human body
It is still safe.In brief, magnetic therapy is exactly to be adjusted and restored in human body using this biomagnetic effect of inside of human body
Various uneven or abnormal functional states achieve the purpose that treatment.The indication of magnetic therapy generally has：Soft tissue strain and contusion,
Muscle fibre knits inflammation, external humeral epicondylitis, arthritis, the periarthritis of shoulderjoint, cervical spondylosis, soft tissue inflammation infection；Bronchitis, branch
San bronchial asthma, hypertension, gastrointestinal dysfunction, canker, cholelithiasis, enruesis, neuralgia, neurosis；Hyperplasia of mammary glands,
Essential uterine bleeding, dysmenorrhoea；Facial tic, temporomandibular arthritis, auricular perichondritis, capillary hemangioma etc..
Magnetic fibre is a kind of material having both textile fiber character and magnetism, wherein having magnetic object is called magnetic
Body can keep magnetic magnet to be called permanent magnet for a long time.
Permanent-magnet material is a kind of important basic function material.The basic function of permanent-magnet material, which is to provide, stablizes lasting magnetic
Flux need not consume electric energy, be one of the important means of energy saving.Current permanent-magnet material substantially may be used by the height of magnetic property
It is divided into two classes, one kind is Conventional permanent magnet material, and such as alnico, ferrite, the characteristics of this kind of material is that magnetic property is relatively low, but price
It is cheap；Another kind of is rare earth permanent-magnetic material, this kind of dilute such as samarium series magnet (such as SmCo5) and neodymium series magnet (such as MgMnNd)
The characteristics of native permanent-magnet material is that magnetic property is higher, but relative price is expensive.
The development experience of permanent-magnet material Al-Ni-Co series Permanent magnet metallics (14~44KJ/m of maximum magnetic energy product) (maximum magnetic flux
Energy product be reflect magnetism of material an overall target), ferrite (barium ferrite, strontium ferrite) permanent-magnet material (maximum magnetic energy
Product 8~30KJ/M), SmCo system rare earth permanent-magnetic material (1:5 SmCos：110~160KJ/m of maximum magnetic energy product；2:17 SmCos：It is maximum
180~240KJ/m of magnetic energy product), Nd-Fe-B rare earth permanent magnetic material (230~280KJ/m of maximum magnetic energy product), samarium iron nitrogen rare earth forever
The courses such as magnetic material (maximum magnetic energy product 100kJ/m) (Pan Shuming,《Kicker magnet-rare earth permanent-magnetic material original from, manufacture and application》,
Chemical Industry Press, in March, 2011).Wherein SmCo is second generation permanent-magnet material, is suitable for hot environment adaptation, because containing me
The shorter strategic element cobalt of state, therefore higher price.Neodymium iron boron is third generation permanent-magnet material, containing rear earth element nd, and I
State possesses abundant rare earth resources and ferro element and boron element relative moderate, although its temperature tolerance not as good as SmCo, as guarantor
Strong textile uses, temperature tolerance that need not be very high.Because its magnetic induction intensity reaches highest at present, it is known as " magnetic king ", therefore especially
It is suitable for making magnetic therapy product.The theoretical maximum magnetic energy product of forth generation permanent-magnet material samarium iron nitrogen will reach 600KJ/m, and without using war
Slightly element cobalt, production cost will be less than neodymium iron boron.But not yet break through mass production techniques at present.Song Houding,《Magnetic material and
Device》, it is loaded with following comparison number in April, 2007：Alnico maximum magnetic energy product is 8~88KJ/m, barium strontium ferrite maximum magnetic flux
Energy product is 8~36KJ/m, SmCo 1:5 type maximum magnetic energy products are 127~207 KJ/m, SmCo 2:17 type maximum magnetic energy products are 175
~255KJ/m, neodymium iron boron maximum magnetic energy product are 239~446KJ/m.Therefore, neodymium iron boron is that have most ferromagnetic permanent magnetism at present
Material.
Currently used for the magnetic material of magnetic health-care textile, mostly ndfeb disk or ferrite magnetic fiber.The former is
Rigid block movement, Magnetic field inhomogeneity in use, the firm discomfort of sense of touch；The latter's magnetic induction intensity is very low, a maximum of about of 10Gs." magnetic king " neodymium
Iron boron has strongest magnetism, but violent oxidation reaction easily occurs after encountering micro oxygen and (or) water, fires
Burn phenomenon；Even if can generate heat, lose magnetism if burning.Especially small particle is being used in order to adapt to co-blended spinning requirement
When magnetic powder, the specific surface area bigger of magnetic powder is more easy to fail because of ingress of air and water, becomes and Nd-Fe-B series magnetic fibre is prevented to add
The bottleneck of work manufacture.Meanwhile the more ordinary ferrite-type magnetic material of price of " magnetic king " neodymium iron boron wants high.
Therefore, although currently on the market there are some magnetic function textiles, magnetic property often not high or comfort level
It is bad.It is not yet seen in and prepares strong magnetic staple fiber by magnetic material spinning of neodymium iron boron.
The information for being disclosed in the background of invention technology segment is merely intended to deepen the reason of the general background technology to the present invention
Solution, and it is known to those skilled in the art existing to be not construed as recognizing or imply that the information is constituted in any form
Technology.
Invention content
In the prior art, the existing staple fiber production equipment separate unit daily output is huge, and it is smaller to be not suitable with functional fiber
Demand；In addition, the magnetic textile with healthcare function needs the staple fiber that is magnetic, to be applied to cotton spinning, wool spinning etc. no
It is blended with short-staple or wool type fiber in system of processing, to adapt to inhomogeneous textile, and nimble adjusting textile
The magnetic induction intensity possessed, to adapt to different health care requirements.In view of the above shortcomings of the prior art with demand, and solve existing
The problems such as magnetic relatively low, feel is poor present in the staple fiber that is magnetic technology of preparing, the present invention provides a kind of rare earth permanent-magnetic material
Long-acting strong magnetic staple fiber and preparation method thereof.Magnetic staple fiber magnetic induction intensity prepared by this method is strong, at low cost, in addition should
Method is produced suitable for small lot.
To achieve the above object, the present invention relates to a kind of magnetic staple fibers, it is characterised in that used in magnetic staple fiber
Magnetic material is rare-earth magnetic composition.The magnetism staple fiber includes the fiber-forming polymer tree of 50~75 parts by weight by weight
The magnetic master batch of fat, 25~50 parts by weight.The fiber-forming polymer resin is selected from polyethylene terephthalate, is poly- to benzene two
Formic acid propylene glycol ester, polyamide 6, polyamide 56, polyamide 66, polyethylene, polypropylene, gathers polybutylene terephthalate (PBT)
Any one of lactic acid, poly- naphthalene.The magnetism master batch includes 35~70 parts by weight vector resins, 30~65 by weight
Parts by weight rare-earth magnetic composition and 0~5 parts by weight spin finish aid.The rare-earth magnetic composition includes by weight：80
~95 parts by weight rare earth permanent-magnetic material magnetic powders, 0~5 parts by weight auxiliary agent and 5~15 parts by weight coverings.The wherein described rare earth permanent magnet
Material magnetic powder is the mixture of rare earth permanent-magnetic material or rare earth permanent-magnetic material and ferrite-type magnetic powder, the mixing of the mixture
Ratio is 1:1~1:5, the grain size of mixture is 0.1~4.0 μm.The rare-earth magnetic composition can not only be such that magnetic material has more
Good stability and magnetism, and when being used to prepare magnetic master batch or spinning permanent magnetism staple fiber, to processing performance, there is no any
It influences.
In rare-earth magnetic composition, the rare earth permanent-magnetic material is samarium system, neodymium series permanent-magnet material, for example, SmCo
(SmCo) permanent magnet, Nd-Fe-B permanent magnet.In the present invention, rare earth permanent-magnetic material refers to that rare earth metal and magnesium-yttrium-transition metal are formed
Alloy through permanent-magnet material made of certain technique.Particularly, rare earth permanent-magnetic material is by samarium, neodymium mixed rare-earth metal and mistake
The alloy for crossing metal (such as cobalt, iron) composition is sintered with powder metallurgy process die mould, the magnetism material obtained after magnetic field is magnetized
Material.
When spinning the magnetic fibre, spinning system domestic demand blanketing with inert gas prevents rare-earth magnetic composition in high temperature
Oxygen and oxidation deactivation are contacted under spinning condition.First prepare rare-earth magnetic composition and magnetic master batch before spinning, when spinning presses one
Certainty ratio is added to the magnetic staple fiber that different particle contents can be spinned in resin slicer.The institute wherein in preparing magnetic master batch
Each component ratio is：35~70 parts of vector resin, 30~65 parts of rare-earth magnetic composition, 0~5 part of spin finish aid.
The vector resin of the present invention in magnetic master batch is sliced for fibre resin, is selected from poly terephthalic acid second
Diol ester, polybutylene terephthalate (PBT), polyamide 6, polyamide 56, polyamide 66, gathers at polypropylene terephthalate
Any one of ethylene, polypropylene, polylactic acid, poly- naphthalene.
In the magnetic master batch of magnetic staple fiber, the spin finish aid is for improving spinning state, according to actual
Master batch application demand is chosen；Such as can be anti-spider web auxiliary agent, occur around end when preventing winding filament to be molded
There is the case where line in face.
In the magnetic master batch of magnetic staple fiber, it is preferable that the rare-earth magnetic composition is by weight by 80~95
Parts by weight rare earth permanent-magnetic material magnetic powder, 5~15 parts by weight coverings and 0~5 parts by weight auxiliary agent composition.
In a preferred embodiment of the invention, in rare-earth magnetic composition, kinematic viscosity of the covering at 40 DEG C
For 30~200m2/ s, the covering are selected from one or more of polyalphaolefin, silicone oil, vegetable oil, atoleine.Here,
In rare-earth magnetic composition, the fusing point of auxiliary agent not above resin processing temperature, generally between 100~250 DEG C, auxiliary agent
For improving the oil as covering to the wellability of magnetic powder, the oil to realize as covering is to the quick cladding of magnetic powder, institute
It states auxiliary agent and is selected from silicone auxiliary agent, ethylene bis stearic acid amide, ethylene acrylic acid co polymer, amide waxe, polyethylene wax, polypropylene wax
One or more of.
In another preferred embodiment of the present invention, in rare-earth magnetic composition, the range of viscosities of covering is
1000~10000mPas (25 DEG C), the covering are silane coupling agent, such as model KH550, KH560, KH570
(G570) silane coupling agent；Or it is titanate coupling agent, such as the titanate esters of model NDZ-201, NDZ-101, HY-311
Coupling agent.The molecular weight of covering be not easy it is excessively high, preferably between 500 to 5000, the molecular weight of covering it is excessive or it is too small all
Covered effect can be caused poor.Here, in rare-earth magnetic composition, the range of viscosities of auxiliary agent is 0.3~1.0mPas (25
DEG C), the boiling point of auxiliary agent is more much lower than the boiling point of covering, prevents the covering in distillation process from being steamed with auxiliary agent；It helps
The compatibility of agent and covering will be got well, and be conducive to covering and disperseed in auxiliary agent, to equably coat magnetic powder in auxiliary agent；Auxiliary agent
For molecular weight generally 50 to 500, boiling point is 80 to 150 DEG C；The auxiliary agent is selected from organic solvent-benzene, dimethylbenzene, acetone.Also exist
This, it is further preferred that in rare-earth magnetic composition, the volume of auxiliary agent is about the 1.5 to 2.0 of rare earth permanent-magnetic material magnetic powder
Times；Preferably, auxiliary agent weight is the 0~5% of rare earth permanent-magnetic material magnetic powder weight；Preferably, the weight of covering be rare earth forever
The 5~15% of magnetic material magnetic powder weight, covering too high levels can influence subsequently to use, and extra covering may be heated or press
The effect of power and leach, so that the yield of magnetic master batch is reduced；Content is too low, then leads to the cladding effect to rare earth permanent-magnetic material magnetic powder
Fruit is undesirable, and coating incomplete part can contact with oxygen and/or water, and fail.
The preparation method of the magnetic staple fiber of the present invention carries out according to the following steps：
I) the preparation of rare-earth magnetic composition comprising：
1) under the protection of inert gas, keep air pressure lower 0.5~1.0kPa than ambient pressure and oxygen content is less than 0.05%
In the environment of, rare earth permanent-magnetic material magnetic powder is injected into excessive covering, wherein the rare earth permanent-magnetic material magnetic powder is dilute
The mixture of native permanent-magnet material or rare earth permanent-magnetic material and ferrite-type magnetic powder, mixed proportion 1:1~1:5, the grain of mixture
Diameter is 0.1~4.0 μm；
2) auxiliary agent is added in the liquid composition obtained by step 1), is dispersed with stirring；
3) liquid composition obtained by step 2) is transferred in ball mill or sand mill, is ground, 300~999 turns/
It grinds 5~45 minutes under the speed divided, is optionally protected using inert gas in process of lapping；
4) liquid after grinding is filtered using Suction filtration device, filters out extra covering, obtain rare-earth magnetic combination
Object；
II) the preparation of magnetic master batch：
35~70 parts by weight vector resins, 30~65 parts by weight rare-earth magnetic compositions and 0~5 parts by weight spinning are helped
Agent uniformly mixes in blend ingredients system, and through double screw extruder extruding pelletization at 180~280 DEG C, magnetism master batch is made,
Whole system must carry out under inert gas protection；Particularly preferably, the preparation of magnetic master batch carries out as follows：
1) to being dried as the vector resin of master batch carrier, make vector resin is aqueous to be less than 20 ppm；
2) under the protection of inert gas, 35~70 parts by weight vector resins, 30~65 parts by weight rare-earth magnetics are combined
Object, 0~5 parts by weight spin finish aid put into blender, are blended uniform；
3) blend obtained by step 2) is put into double screw extruder under the protection of inert gas, at 180~280 DEG C
Through double screw extruder extruding pelletization；
4) inert gas shielding, gained master batch is used to vacuumize packaging using aluminium foil bag and preserve during pelletizing；
III magnetic fibre long filament) is prepared：
By step II) magnetic master batch be added to mixing in fiber-forming polymer resin slicer in 25~50% ratios, through lazy
The spinning system of property gas shield, melting, spinning, winding, drawing-off obtain magnetic fibre long filament；
IV magnetic staple fiber) is spinned：
Under the protection of inert gas, by step III) magnetic fibre long filament through boundling, oil, heat, it is primary more than
Drawing-off, curling, cut-out, obtain magnetic staple fiber.
Preferably, the inert gas is argon gas or nitrogen.
Preferably, in the step of preparing rare-earth magnetic composition, ball mill described in step 3) is vertical or horizontal ball
Grinding machine.
Preferably, in the step of preparing rare-earth magnetic composition, sand mill described in step 3) is horizontal sand mill.
Preferably, in the step of preparing rare-earth magnetic composition, Suction filtration device described in step 4) is preferably vacuum pump.
Vector resin of the present invention is sliced for fibre resin.Polyethylene terephthalate, poly- terephthaldehyde
One in acid propylene glycol ester, polybutylene terephthalate (PBT), polyamide 6, polyamide 56, polyamide 66, polyethylene, polypropylene
Kind.
In the step of preparing rare-earth magnetic composition, preferably under inert gas protection, first make NdFeB magnetic powder and packet
Agent mixing is covered, auxiliary agent is then added, to make NdFeB magnetic powder be uniformly dispersed, and is sufficiently mixed with covering.Preferably, it coats
Agent is selected from one or more of polyalphaolefin, silicone oil, vegetable oil, atoleine；It is double stearic that auxiliary agent is selected from silicone auxiliary agent, ethylene
One or more of sour amide, ethylene acrylic acid co polymer, amide waxe, polyethylene wax, polypropylene wax.
In addition, the present invention also provides another method for preparing magnetic staple fiber, the method includes：
I) the preparation of rare-earth magnetic composition comprising：
1) under the protection of inert gas, rare earth permanent-magnetic material magnetic powder is injected into auxiliary agent, wherein the rare earth permanent magnet
Material magnetic powder is the mixture of rare earth permanent-magnetic material or rare earth permanent-magnetic material and ferrite-type magnetic powder, mixed proportion 1:1~1:
5, the grain size of mixture is 0.1~4.0 μm；
2) in the state of stirring, the weight that covering is added dropwise to covering into the mixture obtained in step 1) is dilute
The 5~15% of native magnetic powder permanent-magnet material weight；
3) it stirs 5~30 minutes, so that the composition obtained in step 2) is sufficiently mixed, in rare earth permanent-magnetic material magnetic powder
Surface forms coating film；
4) so that the composition obtained in step 3) is filtered, filter out extra auxiliary agent, then carry out pneumatic conveying drying or shaking
Ebullated bed under dynamic state is dried, alternatively, distilled, condensed to the composition obtained in step 3), make auxiliary agent with it is dilute
Native permanent-magnet material magnetic powder is separated and recovered from auxiliary agent, obtains rare-earth magnetic composition；
II) the preparation of magnetic master batch：
35~70 parts by weight vector resins, 30~65 parts by weight rare-earth magnetic compositions and 0~5 parts by weight spinning are helped
Agent uniformly mixes in homemade blend ingredients system, and through double screw extruder extruding pelletization at 180~280 DEG C, magnetic is made
Sexupara grain, whole system must carry out under inert gas protection；Particularly preferably, the preparation of magnetic master batch as follows into
Row：
1) to being dried as the vector resin of master batch carrier, make vector resin is aqueous to be less than 20 ppm；
2) under the protection of inert gas, by 35~70 parts by weight vector resins, the rare earth of 30~65 parts by weight steps 1)
Magnetic powder composition, 0~5 parts by weight spin finish aid put into blender, are blended uniform；
3) blend obtained by step 2) is put into double screw extruder under the protection of inert gas, at 180~280 DEG C
Through double screw extruder extruding pelletization；
4) inert gas shielding, gained master batch is used to vacuumize packaging using aluminium foil bag and preserve during pelletizing；
III magnetic fibre long filament) is prepared：
By step II) magnetic master batch be added to mixing in fiber-forming polymer resin slicer in 25~50% ratios, through lazy
The spinning system of property gas shield, melting, spinning, winding, drawing-off obtain magnetic fibre long filament；
IV magnetic staple fiber) is spinned：
Under the protection of inert gas, by step III) magnetic fibre long filament through boundling, oil, heat, it is primary more than
Drawing-off, curling, cut-out, obtain magnetic staple fiber.
Preferably, it is to need to carry out spinning according to the application of magnetic master batch during above-mentioned preparation magnetism master batch
Fiber type selects suitable covering.The selection of covering is to be risen with the active part of rare earth permanent-magnetic material magnetic powder first
Reaction, the possibility that closing activity group is combined with moisture and oxygen；In addition, having as possible with vector resin preferable compatible
Property, to be stabilized in magnetic master batch.Preferably, covering is selected from silane coupling agent or titanate coupling agent；Auxiliary agent
Selected from organic solvent-benzene, dimethylbenzene or acetone.
Preferably, the inert gas is argon gas or nitrogen.
Preferably, in the step of preparing rare-earth magnetic composition, filter device described in step 4) is preferably vacuum pump.
In the step of preparing rare-earth magnetic composition, the rare-earth magnetic composition obtained is measured by TGA,
It can determine the content of coupling agent, and infer that it directly affects the degree of covered effect.
In addition, in a preferred embodiment of the invention, also providing a kind of method preparing magnetic staple fiber, the method
Including：
I) the preparation of rare-earth magnetic composition comprising：
1) inert gas is persistently filled in control box, air therein is discharged, the air pressure in control box is made to be less than environment
0.5~1.0KPa of air pressure makes oxygen content be less than 0.05%, covering is added in control box；
2) then, sequentially rare earth permanent-magnetic material magnetic powder and auxiliary agent are added in control box, using heating stirring machine, 50~
20~30min is stirred at 80 DEG C, covering, auxiliary agent and rare earth permanent-magnetic material magnetic powder is dispersed with stirring uniformly, wherein the rare earth
Permanent-magnet material magnetic powder is the mixture of rare earth permanent-magnetic material and ferrite-type magnetic powder, mixed proportion 1:1~1:5, mixture
Grain size is 0.1~4.0 μm；
3) optionally under air or inert gas atmosphere, the composition obtained by step 2) is filtered using vacuum pump, is filtered out
Extra covering obtains rare-earth magnetic composition；
II) the preparation of magnetic master batch：
By 35~70 amount part vector resins, 30~65 parts by weight rare-earth magnetic compositions and 0~5 parts by weight spin finish aid
It is uniformly mixed in homemade blend ingredients system, through double screw extruder extruding pelletization at 180~280 DEG C, magnetism is made
Master batch, whole system must carry out under inert gas protection；Particularly preferably, the preparation of magnetic master batch carries out as follows：
1) to being dried as the vector resin of master batch carrier, make vector resin is aqueous to be less than 20 ppm；
2) under the protection of inert gas, by 35~70 parts by weight vector resins, the rare earth of 30~65 parts by weight steps 1)
Magnetic powder composition, 0~5 parts by weight spin finish aid put into blender, are blended uniform；
3) blend obtained by step 2) is put into double screw extruder under the protection of inert gas, at 180~280 DEG C
Through double screw extruder extruding pelletization；
4) inert gas shielding, gained master batch is used to vacuumize packaging using aluminium foil bag and preserve during pelletizing；
III magnetic fibre long filament) is prepared：
By step II) magnetic master batch be added to mixing in fiber-forming polymer resin slicer in 25~50% ratios, through lazy
The spinning system of property gas shield, melting, spinning, winding, drawing-off obtain magnetic fibre long filament；
IV magnetic staple fiber) is spinned：
Under the protection of inert gas, by step III) magnetic fibre long filament through boundling, oil, heat, it is primary more than
Drawing-off, curling, cut-out, obtain magnetic staple fiber.
In the step of preparing rare-earth magnetic composition, the babinet of the control box may be used on fluid mechanical design
The inert gas of various different densities effectively excludes air, does not stay the dead angle of air pocket；The control box is connected with negative simultaneously
Pumping equipment is pressed, in favor of extracting air or being pumped into inert gas；Optionally, different working positions is provided with vacuum degree inspection
Measurement equipment, humidity and temperature testing equipment；Also optionally, setting remote control arm, can be fed, be stirred outside control box,
The operations such as discharging, to keep each component dispersion mixing in rare-earth magnetic composition uniform.
Preferably, in the step of preparing rare-earth magnetic composition, covering is selected from silane coupling agent or titanate esters are coupled
Agent；Auxiliary agent is selected from organic solvent-benzene, dimethylbenzene or acetone.It is further preferred that in the step of preparing rare-earth magnetic composition, cladding
Agent is selected from one or more of polyalphaolefin, silicone oil, vegetable oil, atoleine；It is double stearic that auxiliary agent is selected from silicone auxiliary agent, ethylene
One or more of sour amide, ethylene acrylic acid co polymer, amide waxe, polyethylene wax, polypropylene wax.
The magnetic staple fiber of the present invention is spinned using the mixture of rare earth permanent-magnetic material and ferrite-type magnetic powder as magnetic material
Magnetic staple fiber can reduce the cost using rare earth permanent-magnetic material magnetic material, on the other hand can integrally improve magnetic staple fiber and knit
At the magnetic induction intensity to magnetize after fabric.In addition, in the method that the present invention prepares magnetic staple fiber, carry out more than primary
Stretching will not generate and largely break so that Ke Yijie accordingly even when containing a large amount of additive or on the basis of impurity
About cost and improve production efficiency and product quality.The magnetic staple fiber of the present invention is convenient for mixed with short-staple or wool type fiber
It spins, is adapted to inhomogeneous textile.The method that the present invention prepares magnetic staple fiber is produced suitable for small lot, so it is completely
It is adapted to the smaller demand of functional fiber, and can neatly adjust the magnetic induction intensity that textile is possessed, with
Adapt to different health care requirements.The daily output that the present invention prepares the method for magnetic staple fiber can be about 1~12.
Specific implementation mode
A kind of magnetic staple fiber that the present invention designs, it is characterised in that magnetic material used in magnetic staple fiber be not it is single at
Point, it is rare-earth magnetic composition.When spinning the magnetic fibre, spinning system domestic demand blanketing with inert gas prevents rare earth permanent magnet
Material contacts oxygen and oxidation deactivation under high temperature spinning condition.Rare-earth magnetic composition and magnetic master batch are first prepared before spinning,
It is added in resin slicer the magnetic staple fiber containing different particle contents that can weave when spinning in proportion.
It is an advantage of the invention that：The magnetic material added in fiber is the mixture of rare earth permanent-magnetic material and ferrite-type magnetic powder,
It can effectively reduce cost.Rare-earth magnetic composition can not only make magnetic material have better stability and magnetism, and with
Any influence is not present to processing performance when preparing magnetic master batch or spinning permanent magnetism fiber.
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more
Add and clearly demonstrate technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
Specific embodiments of the present invention are as follows：
Embodiment 1
It is prepared as needed for poly- to the magnetic master batch in benzene first naphthalate (PET) fiber, wherein selection is planted
Object oil is as covering.
Argon gas is persistently filled in control box, air therein is discharged, the air pressure in control box, which is maintained at, compares ambient pressure
Low 1.0kPa, oxygen content 0.05%.90 parts of NdFeB magnetic powders are injected into 20 parts of vegetable oil, 1.5 parts of silicone are then added
Auxiliary agent is simultaneously transferred in vertical ball mill, under 500 revs/min of speed and is ground 30 minutes under nitrogen protection, is obtained neodymium iron boron
Magnetic powder composition.Then vacuum pump suction filtration is carried out to magnetic powder composition, filters out extra 11.5 parts of coverings.In the protection of nitrogen
Under, 40 parts by weight magnetic powder compositions are added to poly- be sliced in powder to benzene first naphthalate of 60 parts by weight and mix mixing,
By double screw extruder extruding pelletization, magnetic master batch is obtained.
Prepared magnetic master batch is added in 30% ratio and is sliced through being dried to PET of the moisture content less than 30ppm
Middle mixing is obtained using the melt spinning machine by inert gas shielding through spinning screw extrusion molten, spinning, drawing-off and winding
Magnetic PET long filaments.
120 490dt/216f magnetism long filament silk cylinders are placed on guide frame, by filar guide boundling on after 5880tex
Oil enters Sheng silk cylinder through six roller drafting machine drawing-offs 10% after becoming the tow of 5346tex.Into contain silk cylinder process velocity be
360m/min.The tow of 4 Sheng silk cylinders is become to the big tow of 21382tex through creel boundling, then is led through guiding machine → the first
Stretch machine (75m/min) → water-bath drawing-off slot (65 DEG C of steam heating) → second drafting machine (130m/min) → steam traction case
(86 DEG C) → third drafting machine (129m/min), after carrying out drawing-off three times, fibre fineness reaches 1.5dtex, then through the (TSC- that oils
The short silk oiling agent of 202 synthetic fibers, 6% concentration) → curling steam chest → crimping machine (186m/min) → pendulum wire conveyer → relaxation
Heat setting machine (steam heats, 110 DEG C of area's temperature, two 125 DEG C of area's temperature, three 105 DEG C of area's temperature) → traction machine → tensioner
→ cutting machine (shearing length 38mm) → packing.Thus the magnetic PET cotton-type short fibers of 1.5dtex × 38mm are obtained.It presses
21382tex, 75m/min are calculated, 0.615 ton of split run yield, 1.85 tons of daily output.
It is magnetized 30s using 10000Gs high-intensity magnetic fields to magnetism PET cotton-type short fibers obtained, magnetic induction intensity reaches
108.9Gs。
Embodiment 2
It prepares as needed for the magnetic master batch in polypropylene fibre, selects polypropylene as covering.
Argon gas is persistently filled in control box, air therein is discharged, the air pressure in control box keeps lower than environment firm
1.0kPa, oxygen content 0.05%.85 parts of NdFeB magnetic powders are injected into 25 parts of polyolefin, it is double that 3.0 parts of ethylenes are then added
Stearic amide is simultaneously transferred in horizontal ball mill, under 800 revs/min of speed and is ground 30 minutes, is obtained under nitrogen protection
Neodymium-iron-boron compound powder.Then vacuum pump suction filtration is carried out to magnetic powder composition, filters out extra 13 parts of coverings.In nitrogen
Under protection, 35 parts by weight magnetic powder compositions are added in 65 parts by weight of polypropylene slice powder and mix mixing, pass through twin-screw
Machine extruding pelletization obtains polypropylene magnetism master batch.
Prepared magnetic master batch is added to the polypropylene for being less than 30ppm through being dried to moisture content in 50% ratio
Mixing in slice, using the melt spinning machine by inert gas shielding, through spinning screw extrusion molten, spinning, drawing-off and winding,
Obtain magnetic polypropylene filament.
240 830dt/196f magnetism long filament silk cylinders are placed on guide frame, by filar guide boundling on after 19920tex
Oil enters Sheng silk cylinder through six roller drafting machine drawing-offs 10% after becoming the tow of 18109tex.Into contain silk cylinder process velocity be
340m/min.The tow of 8 Sheng silk cylinders is become to the big tow of 144873tex through creel boundling, then through guiding machine → the first
Drafting machine (70m/min) → water-bath drawing-off slot (70 DEG C of steam heating) → second drafting machine (112m/min) → steam traction case
(90 DEG C) → third drafting machine (110m/min), after carrying out drawing-off three times, fibre fineness reaches 3.0dtex, then through the (TSC- that oils
The short silk oiling agent of 202 synthetic fibers, 6% concentration) → curling steam chest → crimping machine (185m/min) → pendulum wire conveyer → relaxation
Heat setting machine (steam heats, 112 DEG C of area's temperature, two 130 DEG C of area's temperature, three 105 DEG C of area's temperature) → traction machine → tensioner
→ cutting machine (shearing length 76mm) → packing.Thus the magnetic polypropylene wool type staple fiber of 3.0dtex × 76mm is obtained.It presses
18109tex, 70m/min are calculated, and class produces 3.89 tons, 11.86 tons of daily output.
It is magnetized 30s using 10000Gs high-intensity magnetic fields to magnetic polypropylene wool type staple fiber obtained, magnetic induction intensity reaches
167.8Gs。
Embodiment 3
It is prepared as needed for the magnetic master batch in polypropylene fibre, wherein selecting NDZ-101 as covering.
Argon gas is persistently filled in control box, air therein is discharged, the air pressure in control box, which is maintained at, compares ambient pressure
Low 1.0kPa, oxygen content 0.05%.80 parts of NdFeB magnetic powders are injected separately into 1.5 parts of acetone, 4 parts of covering NDZ-
It is stirred evenly in 101 (comparative examples 1) and 1.5 parts of acetone, 6 parts of covering NDZ-101 (embodiment 3) and is transferred to vertical ball
It in grinding machine, under 500 revs/min of speed and is ground 30 minutes under nitrogen protection, obtains two NDZ-101 and coat agent content
Then neodymium-iron-boron compound powder carries out condensation distillation to magnetic powder composition, recycle auxiliary agent, obtain two NDZ-101 coverings
The magnetic powder composition of content cladding.Under the protection of nitrogen, magnetic powder composition is added to polypropylene by 50% adding proportion
It is sliced in powder and is uniformly mixed, through double screw extruder extruding pelletization, obtain two kinds of magnetic master batches.
Prepared magnetic master batch is added to the polypropylene for being less than 30ppm through being dried to moisture content in 40% ratio
Mixing in slice, using the melt spinning machine by inert gas shielding, through spinning screw extrusion molten, spinning, drawing-off and winding,
Obtain two kinds of magnetic polypropylene filaments.
240 540dt/196f magnetism long filament silk cylinders are placed on guide frame, by filar guide boundling on after 12960tex
Oil enters Sheng silk cylinder through six roller drafting machine drawing-offs 10% after becoming the tow of 11780tex.Into contain silk cylinder process velocity be
350m/min.The tow of 6 Sheng silk cylinders is become to the big tow of 70690tex through creel boundling, then is led through guiding machine → the first
Stretch machine (70m/min) → water-bath drawing-off slot (68 DEG C of steam heating) → second drafting machine (112m/min) → steam traction case
(88 DEG C) → third drafting machine (110m/min), after carrying out drawing-off three times, fibre fineness reaches 2.0dtex, then through the (TSC- that oils
The short silk oiling agent of 202 synthetic fibers, 6% concentration) → curling steam chest → crimping machine (185m/min) → pendulum wire conveyer → relaxation
Heat setting machine (steam heats, 112 DEG C of area's temperature, two 128 DEG C of area's temperature, three 105 DEG C of area's temperature) → traction machine → tensioner
→ cutting machine (shearing length 51mm) → packing.Thus the magnetic polypropylene medium-length staple fiber of 2.0dtex × 51mm is obtained.
It is calculated by 70690tex, 70m/min, class produces 1.9 tons, 5.7 tons of daily output.
10000Gs high-intensity magnetic fields are all made of to two kinds obtained magnetic polypropylene medium-length staple fibers to magnetize 30s, using 4 parts
The magnetic induction intensity of the magnetic polypropene staple of covering is 47.5Gs, using the short fibre of magnetic polypropylene of 6 parts of coverings
The magnetic induction intensity of dimension is 76.8Gs.
Embodiment 4
It is prepared as needed for poly- to the magnetic master batch in benzene first naphthalate (PET) fiber, wherein selecting
KH560 is as covering.
Argon gas is persistently filled in control box, air therein is discharged, the air pressure in control box, which is maintained at, compares ambient pressure
Low 1.2kPa, oxygen content 0.02%.85 parts of NdFeB magnetic powders are injected into 2.25 parts of dimethylbenzene auxiliary agent, are then added
It stirs evenly, and is transferred in horizontal ball mill in the covering for the KH560 that 12.75 parts of boiling points are 290 DEG C, at 800 revs/min
Speed under and nitrogen protection under grind 30 minutes, obtain neodymium-iron-boron compound powder.Then magnetic powder composition is distilled
Auxiliary agent is recycled in condensation, obtains the magnetic powder composition of coated dose of cladding.And by magnetic powder composition obtained and ferromagnetic oxide powder with
1：Magnetic powder composition and ferromagnetic oxide powder are added to PET by 40% and are sliced powder by 1.5 ratio mixing under the protection of nitrogen
It is uniformly mixed in body, through double screw extruder extruding pelletization, obtains composite magnetic master batch.
Prepared composite magnetic master batch is added to the PET for being less than 30ppm through being dried to moisture content in 40% ratio
Mixing in slice, using the melt spinning machine by inert gas shielding, through spinning screw extrusion molten, spinning, drawing-off and winding,
Obtain magnetic PET long filaments.
240 490dt/216f magnetism long filament silk cylinders are placed on guide frame, by filar guide boundling on after 11760tex
Oil enters Sheng silk cylinder through six roller drafting machine drawing-offs 10% after becoming the tow of 10690tex.Into contain silk cylinder process velocity be
360m/min.The tow of 7 Sheng silk cylinders is become to the big tow of 74836tex through creel boundling, then is led through guiding machine → the first
Stretch machine (75m/min) → water-bath drawing-off slot (65 DEG C of steam heating) → second drafting machine (130m/min) → steam traction case
(86 DEG C) → third drafting machine (129m/min), after carrying out drawing-off three times, fibre fineness reaches 1.5dtex, then through the (TSC- that oils
The short silk oiling agent of 202 synthetic fibers, 6% concentration) → curling steam chest → crimping machine (186m/min) → pendulum wire conveyer → relaxation
Heat setting machine (steam heats, 110 DEG C of area's temperature, two 125 DEG C of area's temperature, three 105 DEG C of area's temperature) → traction machine → tensioner
→ cutting machine (shearing length 38mm) → packing.Thus the magnetic PET cotton-type short fibers of 1.5dtex × 38mm are obtained.It presses
74836tex, 75m/min are calculated, 2.15 tons of split run yield, 6.47 tons of daily output.
It is magnetized 30s using 10000Gs high-intensity magnetic fields to magnetism PET cotton-type short fibers obtained, magnetic induction intensity reaches
76.3Gs。
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. it is a kind of magnetism staple fiber, which is characterized in that it is described magnetism staple fiber by weight include 50~75 parts by weight at
The magnetic master batch of fine polymeric resin, 25~50 parts by weight,
The magnetism master batch includes 35~70 parts by weight vector resins, 30~65 parts by weight rare-earth magnetic compositions by weight
With 0~5 parts by weight spin finish aid,
The rare-earth magnetic composition includes by weight：80~95 parts by weight rare earth permanent-magnetic material magnetic powders, 5~15 parts by weight
Covering and 0~5 parts by weight auxiliary agent.
2. magnetism staple fiber according to claim 1, which is characterized in that the rare earth permanent-magnetic material magnetic powder is rare earth permanent magnet
The mixture of material or rare earth permanent-magnetic material and ferrite-type magnetic powder, mixed proportion 1:1~1:5, the grain size of mixture is 0.1
~4.0 μm.
3. magnetism staple fiber according to claim 1, which is characterized in that the covering choosing in the rare-earth magnetic composition
From one or more of polyalphaolefin, silicone oil, vegetable oil, atoleine；Auxiliary agent in the rare-earth magnetic composition is selected from silicon
One kind or several in ketone auxiliary agent, ethylene bis stearic acid amide, ethylene acrylic acid co polymer, amide waxe, polyethylene wax, polypropylene wax
Kind.
4. magnetism staple fiber according to claim 1, which is characterized in that the covering choosing in the rare-earth magnetic composition
From silane coupling agent or titanate coupling agent；Auxiliary agent in the rare-earth magnetic composition be selected from organic solvent-benzene, dimethylbenzene or
Acetone.
5. it is according to claim 1 magnetism staple fiber, which is characterized in that the rare-earth magnetic composition by weight by
80~95 parts by weight rare earth permanent-magnetic material magnetic powders, 5~15 parts by weight coverings and 0~5 parts by weight auxiliary agent composition.
6. a kind of method preparing magnetic staple fiber according to any one of claim 1 to 5, which is characterized in that described
Method includes：
I) the preparation of rare-earth magnetic composition；
II) the preparation of magnetic master batch：
By 35~70 parts by weight vector resins, 30~65 parts by weight rare-earth magnetic compositions and 0~5 parts by weight spin finish aid mixed
It is uniformly mixed in material feed proportioning system, through double screw extruder extruding pelletization at 180~280 DEG C, magnetism master batch is made, it is entire to be
System must carry out under inert gas protection；
III magnetic fibre long filament) is prepared：
By step II) magnetic master batch be added to mixing in fiber-forming polymer resin slicer in 25~50% ratios, through indifferent gas
The spinning system of body protection, melting, spinning, winding, drawing-off obtain magnetic fibre long filament；
IV magnetic staple fiber) is spinned：
Under the protection of inert gas, by step III) magnetic fibre long filament through boundling, oil, heat, primary above lead
It stretches, crimp, cut off, obtain magnetic staple fiber.
7. according to the method described in claim 6, it is characterized in that, step I) include：
1) under the protection of inert gas, keep air pressure lower 0.5~1.0kPa than ambient pressure and ring of the oxygen content less than 0.05%
Under border, rare earth permanent-magnetic material magnetic powder is injected into excessive covering, wherein the rare earth permanent-magnetic material magnetic powder be rare earth forever
The mixture of magnetic material or rare earth permanent-magnetic material and ferrite-type magnetic powder, mixed proportion 1:1~1:5, the grain size of mixture is
0.1~4.0 μm；
2) auxiliary agent is added in the liquid composition obtained by step 1), is dispersed with stirring,
3) liquid composition obtained by step 2) is transferred in ball mill or sand mill, is ground, at 300~999 revs/min
It grinds 5~45 minutes under speed, is optionally protected using inert gas in process of lapping,
4) liquid after grinding is filtered using Suction filtration device, filters out extra covering, obtain rare-earth magnetic composition.
8. the method according to the description of claim 7 is characterized in that step I) used in covering be selected from polyalphaolefin, silicon
One or more of oil, vegetable oil, atoleine, auxiliary agent are selected from silicone auxiliary agent, ethylene bis stearic acid amide, ethylene acrylic
One or more of copolymer, amide waxe, polyethylene wax, polypropylene wax.
9. according to the method described in claim 6, it is characterized in that, step I) include：
1) under the protection of inert gas, rare earth permanent-magnetic material magnetic powder is injected into auxiliary agent, wherein the rare earth permanent-magnetic material
Magnetic powder is the mixture of rare earth permanent-magnetic material and ferrite-type magnetic powder, mixed proportion 1:1~1:5, the grain size of mixture is 0.1
~4.0 μm；
2) in the state of stirring, the weight that covering is added dropwise to covering into the mixture obtained in step 1) is Rare-Earth Magnetic
The 5~15% of powder permanent-magnet material weight,
3) it stirs 5~30 minutes, so that the composition obtained in step 2) is sufficiently mixed, on the surface of rare earth permanent-magnetic material magnetic powder
Coating film is formed,
4) so that the composition obtained in step 3) is filtered, filter out extra auxiliary agent, then carry out pneumatic conveying drying or in vibration shape
Ebullated bed under state is dried, alternatively, being distilled, being condensed to the composition obtained in step 3), makes auxiliary agent and rare earth forever
Magnetic material magnetic powder is separated and recovered from auxiliary agent, obtains rare-earth magnetic composition.
10. according to the method described in claim 9, it is characterized in that, step I) used in covering be selected from silane coupling agent
Or titanate coupling agent, auxiliary agent are selected from organic solvent-benzene, dimethylbenzene or acetone.
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Address after: 316200 Dong Hai Road, Gao Ting Town, Daishan County, Zhoushan, Zhejiang, 171 Applicant after: Zhoushan Xinxin Fiber Co., Ltd. Applicant after: Suzhou Baoli Di material Polytron Technologies Inc Address before: 316200 Dong Hai Road, Gao Ting Town, Daishan County, Zhoushan, Zhejiang, 171 Applicant before: Zhoushan Xinxin Fiber Co., Ltd. Applicant before: POLY PLASTIC MASTERBATCH (SUZHOU) CO., LTD. |
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