CN106676664B - A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre - Google Patents
A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre Download PDFInfo
- Publication number
- CN106676664B CN106676664B CN201610774733.XA CN201610774733A CN106676664B CN 106676664 B CN106676664 B CN 106676664B CN 201610774733 A CN201610774733 A CN 201610774733A CN 106676664 B CN106676664 B CN 106676664B
- Authority
- CN
- China
- Prior art keywords
- flame
- spinning
- polyamide fibre
- resistant type
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to spinning fields, disclose a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre, the preparation method comprises the following steps: (1) mixing: polycaprolactam slice, fire-retardant particle, wear-resisting functions master batch are mixed；(2) melt: by material, heating melting is squeezed in screw extruder；(3) spinning: the material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream, then forms monofilament after quenching；(4) oiling cluster: carrying out oiling cluster at nozzle, forms tow；(5) pre- network: tow carries out pre- network on pre- Network device；(6) wind: tow is wound molding at winding head.6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre of the invention also has the characteristics that outstanding anti-flammability, wearability on the basis of keeping original performance.Some high fire-retardances are applicable to require, in the specific area of high abrasion requirement.
Description
Technical field
The present invention relates to spinning field more particularly to a kind of 6 preoriented yarns of flame-proof abrasion-resistant type polyamide fibre.
Background technique
Preoriented yarn refers to the degree of orientation obtained through high speed spinning in not being completely stretched between orientation silk and drawn yarn
Chemical-fibres filaments, compared with undrawn yarn, it have a degree of orientation, stability is good, be usually used as draw false twisting deformation
The dedicated silk of silk (DTY).Polyamide fibre 6 is one of common textile fabric, has a series of excellent performance, is widely used in taking
Each domain is led in dress, home textile, decoration, agricultural, fishery etc..
Application No. is 201110432639.3 Chinese patents to disclose the porous fine denier polyamide fiber 6 preoriented yarn of one kind, system
Standby technique and its equipment.It is added in the screw melt extrusion step with the random of methacrylate, maleic anhydride and benzene alkene
Copolymer additives；The breaking strength of obtained preoriented yarn is 3.45 ± 0.25cN/dex, and elongation at break is 80 ± 20%.
Present invention improves over conventional FDY equipment and relevant manufacturing conditions, have efficiently controlled spinneret draft forming process
Middle aggregated structure adjustment, high order is orientated and the supramolecular structure of crystallization, further increases melt mixed uniformity and pressure is steady
Qualitative, the winding tensile and item of effectively adjustment and control strand do uneven rate, after improving porous micro Denier polyamide fibre 6POY
Tensile property.The product that the technical solution provides can reach the maximization of company interest.
Although can be improved melt mixed uniformity and pressure stability in 6 production method of polyamide fibre of above-mentioned patent, having
The winding tensile and item of effect adjustment and control strand do uneven rate, improve the post-tensioning of porous fine denier polyamide fiber 6 POY
Energy.
But its product lacks the functionality such as anti-flammability, wearability, can not be applied to some high fire-retardances requirements, high abrasion is wanted
In the specific area asked.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of 6 preoriented yarns of flame-proof abrasion-resistant type polyamide fibre.System of the present invention
6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre obtained also has outstanding anti-flammability, wearability on the basis of keeping original performance
The features such as.Some high fire-retardances are applicable to require, in the specific area of high abrasion requirement.
The specific technical proposal of the invention is: a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre, the preparation method is as follows:
(1) mixing: polycaprolactam slice, fire-retardant particle, wear-resisting functions master batch are mixed, wherein the fire-retardant particle accounts for
The 0.5-1.5% of gross mass, the wear-resisting functions master batch account for the 1-3% of gross mass.
(2) melt: by mixed material, heating melting is squeezed in screw extruder.
(3) spinning: the material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream,
Then monofilament is formed after quenching.
(4) oiling cluster: carrying out oiling cluster at nozzle, forms tow.
(5) pre- network: the tow carries out pre- network on pre- Network device.
(6) wind: the tow of pre- network is wound molding, wherein winding speed is after seal wire at winding head
4300-4500m/min。
The present invention carries out mixing before melting to polycaprolactam, and fire-retardant particle can effectively improve the anti-flammability of fiber
Can, fiber is applied in the field that high fire-retardance requires.Wear-resisting functions master batch can further increase the wear-resisting of polyamide fibre
Performance enables fiber to apply in the field that high abrasion requires.
Preferably, the fire-retardant particle is ammonium polyphosphate of the degree of polymerization not less than 1000, hollow glass micropearl, magnesia stone
At least one of powder, mullite powder.Above-mentioned material has outstanding flame retardant property, and also can be improved the wear-resisting of fiber simultaneously
Property and intensity.Good dispersion and in mixing, in spinning solution.
Preferably, the hollow glass micropearl, magnesia mountain flour, mullite powder pass through the modification of silane coupling agent.
Hollow glass micropearl, magnesia mountain flour, mullite powder after modification be not easy to reunite in spinning solution, further increases its point
Dissipate property.
Preferably, the fire-retardant particle is micron order or nanoscale.
Preferably, the wear-resisting functions master batch the preparation method comprises the following steps: by concentration be 8-12wt% graphene oxide it is water-soluble
Liquid is heated to 50-60 DEG C, and the water-soluble polyamic acid solution that dropwise addition concentration is 4-6wt% into graphene oxide water solution is 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, stands 10-16h under room temperature, 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 350-400 DEG C with the heating rate of 5-7 DEG C/min, 2-3h is kept the temperature, then with 7-
The heating rate of 9 DEG C/min is continuously heating to 500-550 DEG C, keeps the temperature 4-5h, then takes out reactant, wash away miscellaneous in reactant
It is dried after matter, graphene aerogel dry powder is made after finally crushing；By polyether polyol, polymethylene polyphenyl polyisocyanate cyanogen
Acid esters, glycerine, triethylene diamine, graphene aerogel dry powder and water mixing, stir foaming, normal at a temperature of 50-60 DEG C
Temperature is lower to stand aging 0.5-1h, finally crushes and obtains wear-resisting functions master batch；Wherein, in parts by mass, the polyether polyol is
40-50 parts, 60-70 parts of poly methylene poly phenyl poly isocyanate, 2-3 parts of glycerine, 0.2-0.4 parts of triethylene diamine, graphite
30-40 parts of alkene aeroge dry powder, 4-8 parts of water.
Wear-resisting functions master batch made from the above method, due to having the presence of graphene, wear-resisting property with super strength；And
During the preparation process, first water-soluble polyamic acid solution is added drop-wise in graphene oxide water solution, carries out cross-linking reaction, formed
Sol form, the colloidal sol have network pore structure because of the crosslinking of substance.Then the heating of two step ladders is carried out to colloidal sol, the
When one step heats, moisture evaporation in colloidal sol, water-soluble polyamic acid occurs the sub- amidation of heat and is converted into polyimides, at this time oxygen
Graphite alkene is further crosslinked with polyimides, and graphene oxide is also reduced to graphene, generates a large amount of three-dimensional pore spaces.?
When two-step heating, part skeletal substance is carbonized in colloidal sol, volatile substances volatilization, so that its space originally occupied is formed
Gap becomes aeroge, and the stability of the graphene aerogel obtained at this time is good, and wearability is high.Then, by graphene aerogel
Dry powder and polyether polyol, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene aerogel dry powder
It mixes, and foams with water, the wear-resisting functions masterbatch of foam powdery is obtained after aging, drying and crushing, glycerine is as friendship
Join agent, triethylene diamine is carried on the surface of foam powder as foaming agent, graphene aerogel dry powder as catalyst, water.
The wear-resisting functions masterbatch has wear-resisting functions, and light weight simultaneously, and density is small, and porosity is high, moreover it is possible to fire-retardant particle be cooperated to improve
Flame retardant effect, and compatibility height, dispersion effect are good in spinning solution.
Preferably, the partial size of the wear-resisting functions master batch is 0.4-10 microns.
Preferably, hot-melt extrusion technology is divided into 4 processes in step (2), melting temperature be respectively as follows: 245-250 DEG C,
250-255℃、255-260℃、250-255℃。
Preferably, quenching temperature is 18-22 DEG C in step (3), cold air blast velocity 0.5-0.6m/s.
Preferably, during step (4) oils, contain epoxy resin, the epoxy resin in the spinning oil that oils
Dosage be preoriented yarn quality 0.2-0.4%.
Epoxy resin is added in spinning oil, epoxy resin is attached to fiber surface after oiling, in subsequent 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 with polyamide at a higher temperature, can improve molecular weight as the chain extender of polyamide.
Since the resistance to ag(e)ing of polyamide fibre is poor, it is easy to be degraded by after high temperature and long-time illumination, fibre property is caused to decline.
The addition of epoxy resin is capable of the degradation of impedance macromole polyamide, and can be attached the polyamide molecule of degradation,
Molecular weight is improved, to prevent fiber aging, keeps fibre property.But if mixing process by epoxy resin before melting
Middle addition, since subsequent spinning process temperature is higher, epoxy resin can shift to an earlier date to be reacted with spinning solution, to be unable to reach
Effect.And the addition of excessive functional additive, it will affect the spinnability of spinning solution.The present invention is in fatliquoring stage by asphalt mixtures modified by epoxy resin
Rouge is attached to fiber surface, then penetrates into fibrous inside by stretching, will not only react with spinning solution, but also not
It will affect the spinnability of spinning solution.
Preferably, the pressure of the pre- Network device is 0.8-1.0bar.
The present invention combines raw material of the invention, is set accordingly to the technological parameter in spinning process, so that fire-retardant
Particle, wear-resisting functions master batch, epoxy resin etc. are uniformly distributed in the fibre, good dispersion.Especially for the infiltration of epoxy resin
Thoroughly, the process requirement specific aim after spinning is set, to improve its permeability.
It is compared with the prior art, the beneficial effects of the present invention are: 6 preorientation of flame-proof abrasion-resistant type polyamide fibre produced by the present invention
Silk, on the basis of keeping original performance, also has the characteristics that outstanding anti-flammability, wearability.It is applicable to some high resistants
In the specific area that combustion requires, high abrasion requires.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1
A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre, the preparation method is as follows:
(1) mixing: polycaprolactam slice, the fire-retardant particle of nanoscale, wear-resisting functions master batch are mixed, wherein the resistance
Combustion particle accounts for the 1% of gross mass, and the wear-resisting functions master batch accounts for the 2% of gross mass.
Wherein, the fire-retardant particle is the mixture of ammonium polyphosphate of the degree of polymerization not less than 1000, hollow glass micropearl.And
And the hollow glass micropearl passes through the modification of silane coupling agent.
The wear-resisting functions master batch the preparation method comprises the following steps: by concentration be 10wt% graphene oxide water solution be heated to 55
DEG C, the water-soluble polyamic acid solution that concentration is 5wt% is added dropwise into graphene oxide water solution and is stirred simultaneously, wherein
The dripping quantity of water-soluble polyamic acid solution is 2.5 times of graphene oxide water solution volume, and being uniformly dispersed after dropwise addition, it is molten to be formed
Glue stands 13h under room 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 375 DEG C with the heating rate of 6 DEG C/min, 2.5h is kept the temperature, then continues to heat up with the heating rate of 8 DEG C/min
To 525 DEG C, 4.5h is kept the temperature, reactant is then taken out, is dried after washing away the impurity in reactant, stone is made after finally crushing
Black alkene aeroge dry powder；By polyether polyol, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene
Aeroge dry powder and water mixing, foaming is stirred at a temperature of 55 DEG C, stands aging 45min at normal temperature, finally crushes and obtains grain
The wear-resisting functions master batch that diameter is 0.4-1 microns.
Wherein, in parts by mass, the polyether polyol is 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) melt: by mixed material, heating melting is squeezed in screw extruder.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melting temperature are respectively as follows: 248 DEG C, 253 DEG C, 258 DEG C, 253 DEG C.
(3) spinning: the 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, cold air blast velocity 0.55m/s.
(4) oiling cluster: carrying out oiling cluster at nozzle, forms tow.(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) wind: the tow of pre- network is wound molding, wherein winding speed is after seal wire at winding head
4300m/min。
Embodiment 2
A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre, the preparation method is as follows:
(1) mixing: polycaprolactam slice, the fire-retardant particle of nanoscale, wear-resisting functions master batch are mixed, wherein the resistance
Combustion particle accounts for the 0.5% of gross mass, and the wear-resisting functions master batch accounts for the 1% of gross mass.
Wherein, the fire-retardant particle is magnesia mountain flour.Also, the magnesia mountain flour passes through at the modification of silane coupling agent
Reason.
The wear-resisting functions master batch the preparation method comprises the following steps: by concentration be 8wt% graphene oxide water solution be heated to 50
DEG C, the water-soluble polyamic acid solution that concentration is 4wt% is added dropwise into graphene oxide water solution 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 room 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, 3h is kept the temperature, is then continuously heating to 500 with the heating rate of 7 DEG C/min
DEG C, 5h is kept the temperature, reactant is then taken out, is dried after washing away the impurity in reactant, graphene gas is made after finally crushing
Gel dry powder；By polyether polyol, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene aerogel
Dry powder and water mixing, at 50 °C stirring foaming stand aging 1h at normal temperature, and finally crushing and obtaining partial size is that 5-10 is micro-
The wear-resisting functions master batch of rice.
Wherein, in parts by mass, the polyether polyol is 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) melt: by mixed material, heating melting is squeezed in screw extruder.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melting temperature are respectively as follows: 245 DEG C, 250 DEG C, 255 DEG C, 250 DEG C.
(3) spinning: the 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, cold air blast velocity 0.5m/s.
(4) oiling cluster: carrying out oiling cluster at nozzle, forms tow.During oiling, the spinning oil that oils
In contain epoxy resin, the dosage 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) wind: the tow of pre- network is wound molding, wherein winding speed is after seal wire at winding head
4400m/min。
Embodiment 3
A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre, the preparation method is as follows:
(1) mixing: polycaprolactam slice, micron-sized fire-retardant particle, wear-resisting functions master batch are mixed, wherein the resistance
Combustion particle accounts for the 1.5% of gross mass, and the wear-resisting functions master batch accounts for the 3% of gross mass.
Wherein, the fire-retardant particle is mullite powder.Also, the mullite powder passes through at the modification of silane coupling agent
Reason.
The wear-resisting functions master batch the preparation method comprises the following steps: by concentration be 12wt% graphene oxide water solution be heated to 60
DEG C, the water-soluble polyamic acid solution that concentration is 6wt% is added dropwise into graphene oxide water solution 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 room 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, 2h is kept the temperature, is then continuously heating to 550 with the heating rate of 9 DEG C/min
DEG C, 4h is kept the temperature, reactant is then taken out, is dried after washing away the impurity in reactant, graphene gas is made after finally crushing
Gel dry powder；By polyether polyol, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene aerogel
Dry powder and water mixing, foaming is stirred at a temperature of 60 DEG C, stands aging 0.5h at normal temperature, and finally crushing and obtaining partial size is 1-5
The wear-resisting functions master batch of micron.
Wherein, in parts by mass, the polyether polyol 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) melt: by mixed material, heating melting is squeezed in screw extruder.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melting temperature are respectively as follows: 250 DEG C, 255 DEG C, 260 DEG C, 255 DEG C.
(3) spinning: the 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, cold air blast velocity 0.6m/s.
(4) oiling cluster: carrying out oiling cluster at nozzle, forms tow.During oiling, the spinning oil that oils
In contain epoxy resin, the dosage 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) wind: the tow of pre- network is wound molding, wherein winding speed is after seal wire at winding head
4500m/min。
Embodiment 4
A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre, the preparation method is as follows:
(1) mixing: polycaprolactam slice, the fire-retardant particle of nanoscale, wear-resisting functions master batch are mixed, wherein the resistance
Combustion particle accounts for the 0.5% of gross mass, and the wear-resisting functions master batch accounts for the 2.5% of gross mass.
Wherein, the fire-retardant particle is the ammonium polyphosphate that the degree of polymerization is not less than 1000.
The wear-resisting functions master batch the preparation method comprises the following steps: by concentration be 9wt% graphene oxide water solution be heated to 58
DEG C, the water-soluble polyamic acid solution that concentration is 4.5wt% is added dropwise into graphene oxide water solution and is stirred simultaneously,
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
Colloidal sol stands 14h under room temperature, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is transferred to inert gas environment
In, colloidal sol is warming up to 380 DEG C with the heating rate of 6 DEG C/min, 3h is kept the temperature, then with the heating rate of 8 DEG C/min after of continuing rising
Temperature keeps the temperature 5h, then takes out reactant, be dried after washing away the impurity in reactant to 520 DEG C, and stone is made after finally crushing
Black alkene aeroge dry powder；By polyether polyol, poly methylene poly phenyl poly isocyanate, glycerine, triethylene diamine, graphene
Aeroge dry powder and water mixing, foaming is stirred at a temperature of 55 DEG C, stands aging 0.5h at normal temperature, finally crushes and obtains partial size
For 0.4-2 microns of wear-resisting functions master batch.
Wherein, in parts by mass, the polyether polyol is 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) melt: by mixed material, heating melting is squeezed in screw extruder.Hot-melt extrusion technology is divided into 4 mistakes
Journey, melting temperature are respectively as follows: 245 DEG C, 255 DEG C, 260 DEG C, 255 DEG C.
(3) spinning: the 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, cold air blast velocity 0.6m/s.
(4) oiling cluster: carrying out oiling cluster at nozzle, forms tow.During oiling, the spinning oil that oils
In contain epoxy resin, the dosage 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) wind: the tow of pre- network is wound molding, wherein winding speed is after seal wire at winding head
4450m/min。
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (6)
1. a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre, it is characterised in that the preparation method is as follows:
(1) mixing: polycaprolactam slice, the fire-retardant particle of nanoscale, wear-resisting functions master batch are mixed, wherein described fire-retardant
Grain accounts for the 0.5-1.5% of gross mass, and the wear-resisting functions master batch accounts for the 1-3% of gross mass；Fire-retardant particle is not less than for the degree of polymerization
At least one of 1000 ammonium polyphosphate, hollow glass micropearl, magnesia mountain flour, mullite powder；
The wear-resisting functions master batch the preparation method comprises the following steps: by concentration be 8-12wt% graphene oxide water solution be heated to 50-60
DEG C, the water-soluble polyamic acid solution that concentration is 4-6wt% is added dropwise into graphene oxide water solution and is stirred simultaneously,
The dripping quantity of middle water-soluble polyamic acid solution is 2-3 times of graphene oxide water solution volume, is uniformly dispersed to be formed after dropwise addition
Colloidal sol stands 10-16h under room temperature, is washed away the unreacting substance in colloidal sol with water；Then colloidal sol is transferred to inert gas ring
In border, colloidal sol is warming up to 350-400 DEG C with the heating rate of 5-7 DEG C/min, 2-3h is kept the temperature, then with the liter of 7-9 DEG C/min
Warm rate is continuously heating to 500-550 DEG C, keeps the temperature 4-5h, then takes out reactant, done after washing away the impurity in reactant
It is dry, graphene aerogel dry powder is made after finally crushing；By polyether polyol, poly methylene poly phenyl poly isocyanate, the third three
Alcohol, triethylene diamine, graphene aerogel dry powder and water mixing, stir foaming at a temperature of 50-60 DEG C, stand at normal temperature old
Change 0.5-1h, finally crushes and obtain wear-resisting functions master batch；Wherein, in parts by mass, the polyether polyol be 40-50 parts, it is more
60-70 parts of polymethylene polyphenyl polyisocyanates, 2-3 parts of glycerine, 0.2-0.4 parts of triethylene diamine, graphene aerogel are dry
30-40 parts of powder, 4-8 parts of water；
(2) melt: by mixed material, heating melting is squeezed in screw extruder；
(3) spinning: the material after melting carries out spinning in filament spinning component, sprays from spinneret and forms melt stream, then
Monofilament is formed after quenching；
(4) oiling cluster: carrying out oiling cluster at nozzle, forms tow；Wherein, contain asphalt mixtures modified by epoxy resin in the spinning oil to oil
Rouge, the dosage of the epoxy resin are the 0.2-0.4% of preoriented yarn quality；
(5) pre- network: the tow carries out pre- network on pre- Network device；
(6) wind: the tow of pre- network is wound molding after seal wire at winding head, and wherein winding speed is 4300-
4500m/min。
2. a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre as described in right wants 1, which is characterized in that the hollow glass micropearl,
Magnesia mountain flour, mullite powder pass through the modification of silane coupling agent.
3. a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre as described in claim 1, which is characterized in that the wear-resisting functions are female
The partial size of grain is 0.4-10 microns.
4. a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre as described in claim 1, which is characterized in that heat fusing in step (2)
Extruding is divided into 4 processes, and melting temperature is respectively as follows: 245-250 DEG C, 250-255 DEG C, 255-260 DEG C, 250-255 DEG C.
5. a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre as described in claim 1, which is characterized in that blowing is cold in step (3)
But temperature is 18-22 DEG C, cold air blast velocity 0.5-0.6m/s.
6. a kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre as described in claim 1, which is characterized in that the pre- Network device
Pressure is 0.8-1.0bar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610774733.XA CN106676664B (en) | 2016-08-31 | 2016-08-31 | A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610774733.XA CN106676664B (en) | 2016-08-31 | 2016-08-31 | A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106676664A CN106676664A (en) | 2017-05-17 |
| CN106676664B true CN106676664B (en) | 2019-07-09 |
Family
ID=58839988
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610774733.XA Active CN106676664B (en) | 2016-08-31 | 2016-08-31 | A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106676664B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107164817B (en) * | 2017-06-06 | 2019-03-26 | 烟台市烯能新材料有限责任公司 | A kind of preparation method of graphene-graphene oxide composite nylon fiber |
| CN107313126B (en) * | 2017-06-30 | 2019-12-17 | 福建锦江科技有限公司 | Method for producing graphene modified polyamide-6 fiber through high-speed spinning |
| CN107723825B (en) * | 2017-10-28 | 2020-12-15 | 淮北新兴皇苑制衣有限公司 | Preparation method of enhanced acrylic fibers for wearing |
| CN108149337A (en) * | 2017-12-05 | 2018-06-12 | 上海帕吉索纳米技术有限公司 | A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof |
| CN110484993A (en) * | 2019-09-02 | 2019-11-22 | 福州高科新技术开发有限公司 | A kind of antibacterial wear-resisting and waterproof washes the preparation method of 6 preoriented yarn of polyamide fibre |
| CN110713709A (en) * | 2019-09-26 | 2020-01-21 | 江阴市强力化纤有限公司 | Production method of flame-retardant polyamide-6 chips |
| CN115369500A (en) * | 2022-08-11 | 2022-11-22 | 福建景丰科技有限公司 | Preparation method of graphene high-strength polyamide 6 fiber |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604175A (en) * | 2012-02-23 | 2012-07-25 | 北京化工大学 | Method for preparing graphene oxide/white carbon black/rubber nanocomposite |
| CN102943313A (en) * | 2012-11-14 | 2013-02-27 | 浙江益南纤维科技有限公司 | Production process of nylon-6 |
| CN103031638A (en) * | 2012-12-14 | 2013-04-10 | 常熟市凯鑫地毯有限公司 | Carpet yarn manufacture method |
| CN103265685A (en) * | 2013-05-28 | 2013-08-28 | 江苏华大新材料有限公司 | Microporous polyether urethane elastomer composite material and preparation method thereof |
| CN103409843A (en) * | 2013-09-02 | 2013-11-27 | 江苏红豆实业股份有限公司 | Preparation method of polyamide fiber with uvioresistant function |
| CN103951973A (en) * | 2014-05-12 | 2014-07-30 | 安徽孟凌精密电子有限公司 | Graphite fibre nylon formula |
| CN104862811A (en) * | 2015-04-24 | 2015-08-26 | 浙江美丝邦化纤有限公司 | Functional nylon 6 fiber production method |
| CN105586658A (en) * | 2016-03-04 | 2016-05-18 | 济南圣泉集团股份有限公司 | Modified chinlon fiber, preparation method and application |
-
2016
- 2016-08-31 CN CN201610774733.XA patent/CN106676664B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604175A (en) * | 2012-02-23 | 2012-07-25 | 北京化工大学 | Method for preparing graphene oxide/white carbon black/rubber nanocomposite |
| CN102943313A (en) * | 2012-11-14 | 2013-02-27 | 浙江益南纤维科技有限公司 | Production process of nylon-6 |
| CN103031638A (en) * | 2012-12-14 | 2013-04-10 | 常熟市凯鑫地毯有限公司 | Carpet yarn manufacture method |
| CN103265685A (en) * | 2013-05-28 | 2013-08-28 | 江苏华大新材料有限公司 | Microporous polyether urethane elastomer composite material and preparation method thereof |
| CN103409843A (en) * | 2013-09-02 | 2013-11-27 | 江苏红豆实业股份有限公司 | Preparation method of polyamide fiber with uvioresistant function |
| CN103951973A (en) * | 2014-05-12 | 2014-07-30 | 安徽孟凌精密电子有限公司 | Graphite fibre nylon formula |
| CN104862811A (en) * | 2015-04-24 | 2015-08-26 | 浙江美丝邦化纤有限公司 | Functional nylon 6 fiber production method |
| CN105586658A (en) * | 2016-03-04 | 2016-05-18 | 济南圣泉集团股份有限公司 | Modified chinlon fiber, preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106676664A (en) | 2017-05-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106676664B (en) | A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre | |
| JP7032826B2 (en) | Vegetable polyester filament yarn and its manufacturing method | |
| CN106637441B (en) | A kind of 6 preoriented yarn of anti-bacterial wear-resisting polyamide fibre | |
| US3382305A (en) | Process for preparing oriented microfibers | |
| CN106633834A (en) | Black masterbatch, nylon 6 fiber and preparation method of black masterbatch and nylon 6 fiber | |
| CN101302666A (en) | Processing technology of melt-spun antibacterial spandex filament | |
| CN106948026A (en) | A kind of fiber of white bamboo carbon chinlon 6 and its production method | |
| CN108977922A (en) | A kind of production method of modified nylon long filament | |
| CN103114344A (en) | Porous superfine denier polyester pre-oriented yarn and preparation method thereof | |
| CN110004508B (en) | Melt-spun spandex color master batch and preparation method thereof | |
| CN109023564A (en) | A kind of preparation method of polylactic acid coloured cut staple | |
| CN109234820A (en) | A kind of preparation method of polylactic acid short-fiber | |
| WO2018040691A1 (en) | Multi-hole ultra-soft superfine denier polyester fibre and preparation method therefor | |
| CN101463505A (en) | Negative ion polypropylene hollow air deformation fibre, preparation and use thereof | |
| KR100960048B1 (en) | Process for preparing dope dyed polyester fiber and the dope dyed polyester fiber | |
| CN106978644B (en) | A kind of 6 high oriented yarn of anti-bacterial wear-resisting polyamide fibre | |
| CN110670167A (en) | Preparation method of antibacterial polyester staple fibers | |
| CN106978636B (en) | A kind of warming 6 high oriented yarn of wear-resisting type polyamide fibre | |
| CN106978634B (en) | A kind of warming 6 preoriented yarn of wear-resisting type polyamide fibre | |
| JP7140950B2 (en) | Hyaluronic acid microcapsules, fibers containing same, method of preparation and use | |
| CN102517679A (en) | Porous microfine denier polyamide 6 pre-oriented yarn, its preparation method and device | |
| US4166091A (en) | Production of plexifilament strands | |
| CN104562275A (en) | Porous micro-fine denier nylon 6 POY filament yarns and preparation method thereof | |
| CN104562250A (en) | Micro-porous fine denier nylon 6 three-difference fiber and preparation method and application thereof | |
| CN104674358B (en) | Specially-shaped spinneret plate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |