CN106637441A - Anti-bacterial wearproof chinlon 6 pre-oriented yarn - Google Patents
Anti-bacterial wearproof chinlon 6 pre-oriented yarn Download PDFInfo
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- CN106637441A CN106637441A CN201610779911.8A CN201610779911A CN106637441A CN 106637441 A CN106637441 A CN 106637441A CN 201610779911 A CN201610779911 A CN 201610779911A CN 106637441 A CN106637441 A CN 106637441A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6677—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- 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
-
- 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
- D01F1/103—Agents inhibiting growth of microorganisms
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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
- D01F6/90—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 polyamides
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/08—Interlacing constituent filaments without breakage thereof, e.g. by use of turbulent air streams
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
Abstract
The invention relates to the field of spinning, and discloses anti-bacterial wearproof chinlon 6 pre-oriented yarn. The preparing method includes the steps of (1) mixing, wherein polycaprolactam chips, anti-bacterial particles and wearproof functional master batch are mixed; (2) fusing, wherein the mixture is heated, fused and extruded in a screw extruder; (3) spinning, wherein the fused material is spun in a spinning assembly and is sprayed from a spinneret plate to form a flux trickle, and monofilaments are formed after blowing cooling; (4) oil applying and bundling, wherein oil applying and bundling are carried out on a nozzle to form tows; (5) pre-interlacing, wherein pre-interlacing is carried out on the tows through a pre-interlacing machine; (6) winding, wherein the tows are wound and formed on a winding head. On the basis of keeping original performance, the anti-bacterial wearproof chinlon 6 pre-oriented yarn has the advantages of excellent antibacterial property and wearproofness and can be applied to special fields with the requirement for high antibacterial property and wearproofness.
Description
Technical field
The present invention relates to spinning field, more particularly to a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6.
Background technology
Preoriented yarn refers to the degree of orientation of Jing high speed spinnings acquisition to be orientated not being completely stretched between silk and drawn yarn
Chemical-fibres filaments, compared with undrawn yarn, it has a certain degree of orientation, good stability, is usually used as draw false twisting deformation
Silk（DTY）Special silk.Polyamide fibre 6 is one of conventional textile fabric, with a series of premium properties, is widely used in clothes
Each domain is led in dress, home textile, decoration, agricultural, fishery etc..
The Chinese patent of Application No. 201110432639.3 discloses a kind of fine denier polyamide fiber 6 preoriented yarn of porous, system
Standby technique and its equipment.Add in screw rod melting extrusion step with the random of methacrylate, maleic anhydride and benzene alkene
Copolymer additives；The fracture strength of the preoriented yarn for obtaining is 3.45 ± 0.25cN/dex, and elongation at break is 80 ± 20%.
Present invention improves over the FDY equipment and the manufacturing condition of correlation of routine, have efficiently controlled spinneret draft forming process
Middle aggregated structure adjustment, high order orientation and the supramolecular structure for crystallizing, further improve melt mixed uniformity and pressure are steady
Qualitative, the winding tensile and bar of effectively adjustment and control strand do uneven rate, after improving porous micro Denier polyamide fibre 6POY
Tensile property.The product that the technical scheme is provided can reach the maximization of company interest.
Although in the production method of polyamide fibre 6 of above-mentioned patent, it is possible to increase melt mixed uniformity and pressure stability, having
The winding tensile and bar of effect adjustment and control strand does uneven rate, improves the after-drawing of the fine denier polyamide fiber 6 POY of porous
Energy.
But its product lacks the features such as antibiotic property, wearability, it is impossible to be applied to some high antibacterials requirements, high abrasion will
In the specific area asked.
The content of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6.Present invention system
The preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 for obtaining, on the basis of original performance is kept, also with outstanding antibiotic property, wearability
The features such as.In being applicable to some high antibacterials requirement, specific areas of high abrasion requirement.
The present invention concrete technical scheme be：A kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6, preparation method is as follows：
（1）Batch mixing：By polycaprolactam section, antibacterial granule, the mixing of wear-resisting functions master batch, wherein the antibacterial granule accounts for total matter
The 1.5-2.5% of amount, the wear-resisting functions master batch accounts for the 1-3% of gross mass.
（2）Melting：By mixed material in screw extruder plus hot-melt extrusion technology.
（3）Spinning：Material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream,
Then monofilament is formed after quenching.
（4）Oil boundling：The boundling that oils is carried out at nozzle, tow is formed.
（5）Pre- network：The tow carries out pre- network on pre- Network device.
（6）Winding：The tow of pre- network is wound shaping after seal wire, at winding head, and wherein winding speed is
4300-4500m/min。
The present invention carries out batch mixing before melting to polycaprolactam, and antibacterial granule can effectively improve the antibiotic property of fiber
Can so that fiber can be applied in the field that high antibacterial is required.Wear-resisting functions master batch can further improve the wear-resisting of polyamide fibre
Performance so that fiber can be applied in the field that high abrasion is required.
Preferably, the preparation method of the antibacterial granule is：Shitosan is added and is uniformly dispersed into water, preparation is obtained
Concentration is the chitosan solution of 1-3wt%, and silver nitrate of the quality for 0.5-0.7 times of shitosan, stirring are added in chitosan solution
After uniform, solution ph is controlled 4, solution is heated to into 40-50 DEG C under dark surrounds, be incubated 3-4h, be then centrifuged for point
From obtaining solid, after solid is cleaned, be dried, in being dissolved in sodium hydroxide solution, in sodium hydroxide solution solid masses is added
0.01-0.02 times of sodium borohydride, adjusts pH to neutrality, and successively through stirring, centrifugation is obtained antibacterial after dry, pulverize
Particle.
Material antibacterial granule obtained in said method has outstanding anti-microbial property, and wherein Nano Silver simple substance is in shitosan
Load capacity it is big, load fastness is high, and good dispersion of the antibacterial granule in batch mixing, in spinning solution.
Preferably, the antibacterial granule is micron order or nanoscale.
Preferably, the preparation method of the wear-resisting functions master batch is：Concentration is water-soluble for the graphene oxide of 8-12wt%
Liquid is heated to 50-60 DEG C, the water-soluble polyamic acid solution that concentration is 4-6wt% is added dropwise in graphene oxide water solution simultaneously same
When be stirred, wherein the dripping quantity of water-soluble polyamic acid solution is 2-3 times of graphene oxide water solution volume, after dropwise addition
It is uniformly dispersed to form colloidal sol, under normal temperature 10-16h is stood, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is shifted
Into inert gas environment, colloidal sol is warming up to into 350-400 DEG C with the heating rate of 5-7 DEG C/min, 2-3h is incubated, then with 7-
The heating rate of 9 DEG C/min is continuously heating to 500-550 DEG C, is incubated 4-5h, then takes out reactant, washes away miscellaneous in reactant
It is dried after matter, graphene aerogel dry powder is obtained after finally crushing；By PPG, many isocyanides of polymethylene polyphenyl
The mixing of acid esters, glycerine, triethylene diamine, graphene aerogel dry powder and water, the stirring foaming at a temperature of 50-60 DEG C, normal
Temperature is lower to stand aging 0.5-1h, finally crushes and obtains wear-resisting functions master batch；Wherein, in parts by mass, the PPG is
40-50 parts, poly methylene poly phenyl poly isocyanate 60-70 parts, glycerine 2-3 parts, triethylene diamine 0.2-0.4 parts, graphite
Alkene aeroge dry powder 30-40 parts, water 4-8 parts.
Wear-resisting functions master batch obtained in said method, due to the presence for having Graphene, with superpower anti-wear performance；And
In preparation process, first water-soluble polyamic acid solution is added drop-wise in graphene oxide water solution, carries out cross-linking reaction, formed
Colloidal sol shape, the colloidal sol has network pore structure because of the crosslinking of material.Then the ladder heating of two steps is carried out to colloidal sol, the
When one step is heated, heat Asia amidatioon and be converted into polyimides in the moisture evaporation in colloidal sol, water-soluble polyamic acid, now oxygen there is
Graphite alkene is further crosslinked with polyimides, and graphene oxide is also reduced to Graphene, generates a large amount of three-dimensional pore spaces.
During two-step heating, part skeletal substance is carbonized in colloidal sol, volatile substances volatilization, so as to its space originally occupied is formed
Space, becomes aeroge, the good stability of the graphene aerogel for now obtaining, and wearability is high.Then, by graphene aerogel
Dry powder and PPG, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene aerogel dry powder
With water mixing, and foamed, aging, the wear-resisting functions masterbatch that is dried and foam powdery is obtained after crushing, glycerine is used as friendship
Connection agent, triethylene diamine is carried on the surface of foam powder as catalyst, water as foaming agent, graphene aerogel dry powder.
The wear-resisting functions masterbatch has a wear-resisting functions, and while light weight, density is little, and porosity is high, moreover it is possible to play heat-insulation warm keeping effect,
And compatibility height, dispersion effect are good in spinning solution.
Preferably, the particle diameter of the wear-resisting functions master batch is 0.4-10 microns.
Preferably, step（2）Middle hot-melt extrusion technology is divided into 4 processes, and its melt temperature is respectively：245-250℃、
250-255℃、255-260℃、250-255℃。
Preferably, step（3）Middle quenching temperature is 18-22 DEG C, and cold air blast velocity is 0.5-0.6m/s.
Preferably, step（4）During oiling, epoxy resin, the epoxy resin are contained in the spinning oil for oiling
Consumption for preoriented yarn quality 0.2-0.4%.
Add epoxy resin in spinning oil, epoxy resin is attached to fiber surface after oiling, in follow-up seal wire mistake
Cheng Zhong, by certain stretching action, with the slight stretching of fiber, epoxy resin can gradually penetrate into fibrous inside.
Epoxy resin can react at a higher temperature with polyamide, can improve molecular weight as the chain extender of polyamide.
Because the resistance to ag(e)ing of polyamide fibre is poor, easily it is subject to be degraded after high temperature and long-time illumination, causes fibre property to decline.
The addition of epoxy resin, is capable of the degraded of impedance macromole polyamide, and can be attached the polyamide molecule of degraded,
Molecular weight is improved, so as to prevent fiber aging, fibre property is kept.But if the mixing process by epoxy resin before melting
Middle addition, because follow-up spinning process temperature is higher, epoxy resin can shift to an earlier date and be reacted with spinning solution, so as to be unable to reach
Effect.And the addition of excessive functional additive, the spinnability of spinning solution can be affected.The present invention is in fatliquoring stage by asphalt mixtures modified by epoxy resin
Fat is attached to fiber surface, then penetrates into fibrous inside by stretching, not only will not react with spinning solution, and not
The spinnability of spinning solution can be affected.
Preferably, the pressure of the pre- Network device is 0.8-1.0bar.
The present invention combines the raw material of the present invention, the technological parameter in spinning process is set accordingly so that antibacterial
Particle, wear-resisting functions master batch, epoxy resin etc. are uniformly distributed in the fibre, good dispersion.Oozing especially for epoxy resin
Thoroughly, specific aim is needed to set the technique after spinning, so as to improve its permeability.
It is compared with the prior art, the invention has the beneficial effects as follows：The obtained preorientation of anti-bacterial wear-resisting polyamide fibre 6 of the invention
Silk, on the basis of original performance is kept, also with outstanding antibiotic property, wearability the features such as.It is applicable to some height anti-
In the specific area that bacterium requirement, high abrasion are required.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6, preparation method is as follows：
（1）Batch mixing：Polycaprolactam section, nano level antibacterial granule, wear-resisting functions master batch are mixed, wherein the antibacterial
Grain accounts for the 2% of gross mass, and the wear-resisting functions master batch accounts for the 2% of gross mass.
Wherein, the preparation method of the antibacterial granule is：Shitosan is added and is uniformly dispersed into water, preparation obtains concentration
For the chitosan solution of 2wt%, silver nitrate of the quality for 0.6 times of shitosan is added in chitosan solution, after stirring, will
Solution ph is controlled 4, and solution is heated to into 45 DEG C under dark surrounds, is incubated 3.5h, is then centrifuged for isolated solid, will
Solid clean, be dried after, in being dissolved in sodium hydroxide solution, in sodium hydroxide solution add 0.015 times of solid masses boron hydrogen
Change sodium, adjust pH to neutrality, successively through stirring, centrifugation is obtained antibacterial granule after dry, pulverize.
The preparation method of the wear-resisting functions master batch is：Graphene oxide water solution of the concentration for 10wt% is heated to into 55
DEG C, concentration is added dropwise in graphene oxide water solution for the water-soluble polyamic acid solution of 5wt% and is stirred simultaneously, wherein
The dripping quantity of water-soluble polyamic acid solution is 2.5 times of graphene oxide water solution volume, is uniformly dispersed to form molten after dropwise addition
13h is stood under glue, normal temperature, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is transferred in inert gas environment,
Colloidal sol is warming up to into 375 DEG C with the heating rate of 6 DEG C/min, 2.5h is incubated, then continues to heat up with the heating rate of 8 DEG C/min
To 525 DEG C, 4.5h is incubated, then takes out reactant, washed away and be dried after the impurity in reactant, stone is obtained after finally crushing
Black alkene aeroge dry powder；By PPG, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, Graphene
Aeroge dry powder and water mix, and stirring foaming, stands at normal temperatures aging 45min at a temperature of 55 DEG C, finally crush and obtain grain
Footpath is the wear-resisting functions master batch of 0.4-1 microns.
Wherein, in parts by mass, the PPG be 45 parts, 65 parts of poly methylene poly phenyl poly isocyanate, third
2.5 parts of triol, 0.3 part of triethylene diamine, 35 parts of graphene aerogel dry powder, 6 parts of water.
（2）Melting：By mixed material in screw extruder plus hot-melt extrusion technology.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melt temperature is respectively：248℃、253℃、258℃、253℃.
（3）Spinning：Material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream,
Then monofilament is formed after quenching.Wherein, quenching temperature is 20 DEG C, and cold air blast velocity is 0.55m/s.
（4）Oil boundling：The boundling that oils is carried out at nozzle, tow is formed.（5）Pre- network：The tow is in pre- network
Pre- network is carried out on device.The pressure of the pre- Network device is 0.8bar.
（6）Winding：The tow of pre- network is wound shaping after seal wire, at winding head, and wherein winding speed is
4300m/min。
Embodiment 2
A kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6, preparation method is as follows：
（1）Batch mixing：Polycaprolactam section, nano level antibacterial granule, wear-resisting functions master batch are mixed, wherein the antibacterial
Grain accounts for the 1.5% of gross mass, and the wear-resisting functions master batch accounts for the 1% of gross mass.
Wherein, the preparation method of the antibacterial granule is：Shitosan is added and is uniformly dispersed into water, preparation obtains concentration
For the chitosan solution of 1wt%, silver nitrate of the quality for 0.5 times of shitosan is added in chitosan solution, after stirring, will
Solution ph is controlled 4, and solution is heated to into 40 DEG C under dark surrounds, is incubated 4h, is then centrifuged for isolated solid, will be solid
Body clean, be dried after, in being dissolved in sodium hydroxide solution, in sodium hydroxide solution add 0.01 times of solid masses hydroboration
Sodium, adjusts pH to neutrality, and successively through stirring, centrifugation is obtained antibacterial granule after dry, pulverize.
The preparation method of the wear-resisting functions master batch is：Graphene oxide water solution of the concentration for 8wt% is heated to into 50
DEG C, concentration is added dropwise in graphene oxide water solution for the water-soluble polyamic acid solution of 4wt% and is stirred simultaneously, wherein
The dripping quantity of water-soluble polyamic acid solution is 2 times of graphene oxide water solution volume, is uniformly dispersed to form colloidal sol after dropwise addition,
10h is stood under normal temperature, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is transferred in inert gas environment, with 5
DEG C/colloidal sol is warming up to 350 DEG C by the heating rate of min, is incubated 3h, is then continuously heating to 500 with the heating rate of 7 DEG C/min
DEG C, 5h is incubated, reactant is then taken out, wash away and be dried after the impurity in reactant, Graphene gas is obtained after finally crushing
Gel dry powder；By PPG, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene aerogel
Dry powder and water mix, and stirring foaming, stands at normal temperatures aging 1h at a temperature of 50 DEG C, and it is that 5-10 is micro- finally to crush and obtain particle diameter
The wear-resisting functions master batch of rice.
Wherein, in parts by mass, the PPG be 40 parts, 60 parts of poly methylene poly phenyl poly isocyanate, third
2 parts of triol, 0.2 part of triethylene diamine, 30 parts of graphene aerogel dry powder, 4 parts of water.
（2）Melting：By mixed material in screw extruder plus hot-melt extrusion technology.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melt temperature is respectively：245℃、250℃、255℃、250℃.
（3）Spinning：Material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream,
Then monofilament is formed after quenching.Wherein, quenching temperature is 18 DEG C, and cold air blast velocity is 0.5m/s.
（4）Oil boundling：The boundling that oils is carried out at nozzle, tow is formed.During oiling, the spinning oil for oiling
In contain epoxy resin, the consumption of the epoxy resin is the 0.2% of preoriented yarn quality.
（5）Pre- network：The tow carries out pre- network on pre- Network device.The pressure of the pre- Network device is 0.9bar.
（6）Winding：The tow of pre- network is wound shaping after seal wire, at winding head, and wherein winding speed is
4400m/min。
Embodiment 3
A kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6, preparation method is as follows：
（1）Batch mixing：Polycaprolactam section, micron-sized antibacterial granule, wear-resisting functions master batch are mixed, wherein the antibacterial
Grain accounts for the 2.5% of gross mass, and the wear-resisting functions master batch accounts for the 3% of gross mass.
Wherein, the preparation method of the antibacterial granule is：Shitosan is added and is uniformly dispersed into water, preparation obtains concentration
For the chitosan solution of 3wt%, silver nitrate of the quality for 0.7 times of shitosan is added in chitosan solution, after stirring, will
Solution ph is controlled 4, and solution is heated to into 50 DEG C under dark surrounds, is incubated 3h, is then centrifuged for isolated solid, will be solid
Body clean, be dried after, in being dissolved in sodium hydroxide solution, in sodium hydroxide solution add 0.02 times of solid masses hydroboration
Sodium, adjusts pH to neutrality, and successively through stirring, centrifugation is obtained antibacterial granule after dry, pulverize.
The preparation method of the wear-resisting functions master batch is：Graphene oxide water solution of the concentration for 12wt% is heated to into 60
DEG C, concentration is added dropwise in graphene oxide water solution for the water-soluble polyamic acid solution of 6wt% and is stirred simultaneously, wherein
The dripping quantity of water-soluble polyamic acid solution is 3 times of graphene oxide water solution volume, is uniformly dispersed to form colloidal sol after dropwise addition,
16h is stood under normal temperature, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is transferred in inert gas environment, with 7
DEG C/colloidal sol is warming up to 400 DEG C by the heating rate of min, is incubated 2h, is then continuously heating to 550 with the heating rate of 9 DEG C/min
DEG C, 4h is incubated, reactant is then taken out, wash away and be dried after the impurity in reactant, Graphene gas is obtained after finally crushing
Gel dry powder；By PPG, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene aerogel
Dry powder and water mix, and stirring foaming, stands at normal temperatures aging 0.5h at a temperature of 60 DEG C, finally crush and obtain particle diameter for 1-5
The wear-resisting functions master batch of micron.
Wherein, in parts by mass, the PPG be 40-50 parts, 70 parts of poly methylene poly phenyl poly isocyanate,
3 parts of glycerine, 0.4 part of triethylene diamine, 40 parts of graphene aerogel dry powder, 8 parts of water.
（2）Melting：By mixed material in screw extruder plus hot-melt extrusion technology.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melt temperature is respectively： 250℃、255℃、260℃、255℃.
（3）Spinning：Material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream,
Then monofilament is formed after quenching.Wherein, quenching temperature is 22 DEG C, and cold air blast velocity is 0.6m/s.
（4）Oil boundling：The boundling that oils is carried out at nozzle, tow is formed.During oiling, the spinning oil for oiling
In contain epoxy resin, the consumption of the epoxy resin is the 0.4% of preoriented yarn quality.
（5）Pre- network：The tow carries out pre- network on pre- Network device.The pressure of the pre- Network device is 1.0bar.
（6）Winding：The tow of pre- network is wound shaping after seal wire, at winding head, and wherein winding speed is
4500m/min。
Embodiment 4
A kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6, preparation method is as follows：
（1）Batch mixing：Polycaprolactam section, nano level antibacterial granule, wear-resisting functions master batch are mixed, wherein the antibacterial
Grain accounts for the 1.5% of gross mass, and the wear-resisting functions master batch accounts for the 2.5% of gross mass.
Wherein, the preparation method of the antibacterial granule is：Shitosan is added and is uniformly dispersed into water, preparation obtains concentration
For the chitosan solution of 1.5wt%, silver nitrate of the quality for 0.5 times of shitosan is added in chitosan solution, after stirring,
Solution ph is controlled 4, solution is heated to into 45 DEG C under dark surrounds, be incubated 3h, be then centrifuged for isolated solid, will
Solid clean, be dried after, in being dissolved in sodium hydroxide solution, in sodium hydroxide solution add 0.01 times of solid masses hydroboration
Sodium, adjusts pH to neutrality, and successively through stirring, centrifugation is obtained antibacterial granule after dry, pulverize.
The preparation method of the wear-resisting functions master batch is：Graphene oxide water solution of the concentration for 9wt% is heated to into 58
DEG C, concentration is added dropwise in graphene oxide water solution for the water-soluble polyamic acid solution of 4.5wt% and is stirred simultaneously, its
The dripping quantity of middle water-soluble polyamic acid solution is 2.5 times of graphene oxide water solution volume, is uniformly dispersed to be formed after dropwise addition
14h is stood under colloidal sol, normal temperature, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is transferred to into inert gas environment
In, colloidal sol is warming up to into 380 DEG C with the heating rate of 6 DEG C/min, 3h is incubated, then continue to rise with the heating rate of 8 DEG C/min
Temperature is incubated 5h to 520 DEG C, then takes out reactant, washes away and is dried after the impurity in reactant, and stone is obtained after finally crushing
Black alkene aeroge dry powder；By PPG, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, Graphene
Aeroge dry powder and water mix, and stirring foaming, stands at normal temperatures aging 0.5h at a temperature of 55 DEG C, finally crush and obtain particle diameter
For the wear-resisting functions master batch of 0.4-2 microns.
Wherein, in parts by mass, the PPG be 45 parts, 65 parts of poly methylene poly phenyl poly isocyanate, third
2 parts of triol, 0.3 part of triethylene diamine, 35 parts of graphene aerogel dry powder, 5 parts of water.
（2）Melting：By mixed material in screw extruder plus hot-melt extrusion technology.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melt temperature is respectively：245℃、255℃、260℃、255℃.
（3）Spinning：Material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream,
Then monofilament is formed after quenching.Wherein, quenching temperature is 19 DEG C, and cold air blast velocity is 0.6m/s.
（4）Oil boundling：The boundling that oils is carried out at nozzle, tow is formed.During oiling, the spinning oil for oiling
In contain epoxy resin, the consumption of the epoxy resin is the 0.3% of preoriented yarn quality.
（5）Pre- network：The tow carries out pre- network on pre- Network device.The pressure of the pre- Network device is 0.95bar.
（6）Winding：The tow of pre- network is wound shaping after seal wire, at winding head, and wherein winding speed is
4450m/min。
Raw materials used in the present invention, equipment, unless otherwise noted, is the conventional raw material, equipment of this area；In the present invention
Method therefor, unless otherwise noted, is the conventional method of this area.
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions, every according to the present invention
Any simple modification, change and equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (9)
1. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6, it is characterised in that preparation method is as follows：
（1）Batch mixing：By polycaprolactam section, antibacterial granule, the mixing of wear-resisting functions master batch, wherein the antibacterial granule accounts for total matter
The 1.5-2.5% of amount, the wear-resisting functions master batch accounts for the 1-3% of gross mass；
（2）Melting：By mixed material in screw extruder plus hot-melt extrusion technology；
（3）Spinning：Material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream, then
Monofilament is formed after quenching；
（4）Oil boundling：The boundling that oils is carried out at nozzle, tow is formed；
（5）Pre- network：The tow carries out pre- network on pre- Network device；
（6）Winding：The tow of pre- network is wound shaping after seal wire, at winding head, and wherein winding speed is 4300-
4500m/min。
2. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as claimed in claim 1, it is characterised in that the antibacterial granule
Preparation method is：Shitosan is added and is uniformly dispersed into water, preparation obtains the chitosan solution that concentration is 1-3wt%, poly- to shell
Add silver nitrate of the quality for 0.5-0.7 times of shitosan in sugar juice, after stirring, solution ph is controlled 4, in dark
Solution is heated to into 40-50 DEG C under environment, 3-4h is incubated, isolated solid is then centrifuged for, it is molten after solid is cleaned, be dried
In sodium hydroxide solution, the sodium borohydride of 0.01-0.02 times of solid masses is added in sodium hydroxide solution, pH is into for regulation
Property, successively through stirring, centrifugation is obtained antibacterial granule after dry, pulverize.
3. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as claimed in claim 1 or 2, it is characterised in that the antibacterial granule
For micron order or nanoscale.
4. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as claimed in claim 1, it is characterised in that the wear-resisting functions are female
Grain preparation method be：Graphene oxide water solution of the concentration for 8-12wt% is heated to into 50-60 DEG C, to graphene oxide water
Concentration is added dropwise in solution for the water-soluble polyamic acid solution of 4-6wt% and is stirred simultaneously, wherein water-soluble polyamic acid is molten
The dripping quantity of liquid is 2-3 times of graphene oxide water solution volume, is uniformly dispersed to form colloidal sol after dropwise addition, and under normal temperature 10- is stood
16h, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is transferred in inert gas environment, with 5-7 DEG C/min's
Colloidal sol is warming up to 350-400 DEG C by heating rate, is incubated 2-3h, is then continuously heating to the heating rate of 7-9 DEG C/min
500-550 DEG C, 4-5h is incubated, then takes out reactant, washed away and be dried after the impurity in reactant, be obtained after finally crushing
Graphene aerogel dry powder；By PPG, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphite
Alkene aeroge dry powder and water mix, and stirring foaming, stands at normal temperatures aging 0.5-1h at a temperature of 50-60 DEG C, finally crushes
Obtain wear-resisting functions master batch；Wherein, in parts by mass, the PPG is 40-50 parts, many isocyanides of polymethylene polyphenyl
Acid esters 60-70 parts, glycerine 2-3 parts, triethylene diamine 0.2-0.4 parts, graphene aerogel dry powder 30-40 parts, water 4-8 parts.
5. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as described in claim 1 or 4, it is characterised in that the wear-resisting functions
The particle diameter of master batch is 0.4-10 microns.
6. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as claimed in claim 1, it is characterised in that step（2）Middle heat fusing
Extruding is divided into 4 processes, and its melt temperature is respectively：245-250℃、250-255℃、255-260℃、250-255℃.
7. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as claimed in claim 1, it is characterised in that step（3）Middle blowing is cold
But temperature is 18-22 DEG C, and cold air blast velocity is 0.5-0.6m/s.
8. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as claimed in claim 1, it is characterised in that step（4）Oil process
In, epoxy resin is contained in the spinning oil for oiling, the consumption of the epoxy resin is the 0.2-0.4% of preoriented yarn quality.
9. a kind of preoriented yarn of anti-bacterial wear-resisting polyamide fibre 6 as claimed in claim 1, it is characterised in that the pre- Network device
Pressure is 0.8-1.0bar.
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