CN108149337A - A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof - Google Patents
A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof Download PDFInfo
- Publication number
- CN108149337A CN108149337A CN201711270979.4A CN201711270979A CN108149337A CN 108149337 A CN108149337 A CN 108149337A CN 201711270979 A CN201711270979 A CN 201711270979A CN 108149337 A CN108149337 A CN 108149337A
- Authority
- CN
- China
- Prior art keywords
- graphene
- jinlun
- master batch
- preparation
- fireproof fiber
- 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.)
- Pending
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
- D01F6/92—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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides a kind of graphene Jinlun-6 fireproof fiber, the fiber, and graphene content is 3.5 4.5%, and limit oxygen index is 35.5 36%.The present invention also provides a kind of preparation method of graphene Jinlun-6 fireproof fiber, the preparation methods, including preparing silica graphene composite porous material, graphene dispersion suspension is prepared, prepares flame retarding function master batch, melt spinning, it is cooled and shaped, stretches, winds, thermal finalization.The present invention overcomes influence of the addition to the viscosity and mobility of chinlon master batch of graphene, reduce the viscosity of melting chinlon master batch, improve the mobility of melting chinlon master batch.Graphene nylon fibre prepared by the present invention, graphene content are 3.5 4.5%, and it is 60 65N/tex to do fracture strength, and elongation at break 18 24%, Young's modulus is 2.3 2.8Gpa；Limit oxygen index is up to 35.5 36%.
Description
Technical field
The present invention relates to a kind of nylon fibre, particularly a kind of graphene Jinlun-6 fireproof fiber and preparation method thereof belongs to
Textile technology field.
Background technology
Polyamide fibre, i.e. Fypro, it is most prominent the advantages of be wearability higher than other fibers, it is higher than cotton wearability by 10
Times, some polyamide fibres are added in blended fabric, its wearability can be greatly improved.
Graphene is the two dimension crystalline substance of only one layer atomic thickness for being stripped out from graphite material, being made of carbon atom
Body has the characteristics that intensity is big, electrical and thermal conductivity performance is strong, graphene is added in the matrix of polyamide fibre, it is desirable to it is new to assign polyamide fibre
Performance.
When preparing graphene nylon fibre, the graphene of addition can reduce the processing fluidity of chinlon master batch, increase molten
Melt the viscosity of chinlon master batch, limit the addition of graphene.
When preparing the graphene nylon fibre with excellent flame retardant performance, additional addition fire retardant is generally required, still
The addition of fire retardant can influence the performances such as intensity, extensibility, elasticity modulus and the gas permeability of fiber.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of graphene Jinlun-6 fireproof fiber and preparation method thereof, with reality
Now following goal of the invention：
（1）Overcome the influence of the addition of graphene to the viscosity and mobility of chinlon master batch, reduce the viscosity of melting chinlon master batch.
（2）Overcoming intensity of the addition on nylon fibre, extensibility, elasticity modulus and the gas permeability of fire retardant influences, and improves
Intensity, extensibility, elasticity modulus and the gas permeability of fiber.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is：
A kind of preparation method of graphene Jinlun-6 fireproof fiber,
（1）Prepare silica-graphene composite porous material
Include the following steps：
The 8-11% that the graphene that grain size is 400-600 nanometers is pressed to the dry silicic acid quality to production adds in a concentration of 35-40%'s
In sodium silicate aqueous solution, sodium bicarbonate is added in, 55-65 is being warming up to the speed of 1-1.5 DEG C/min after being sufficiently stirred 1-2 hours
DEG C heat preservation, be carried out at the same time ultrasonic echography 2-3 hours, while then stirring under 42-50 revs/min of rate, be slowly added to
Dilute sulfuric acid adjusts pH to 5-6, up to no flocculent deposit and bubble generate；Graphene silicic acid gel substance is obtained after filtering, is taken off
After water, drying, for raising temperature to 155-165 DEG C, soaking time is powder after 4-5 hours to weight free of losses in 35-40 minutes
It is 1-1.5 microns that grain size is obtained after broken, and porosity is in 68-75%, silica-graphite of the aperture at 900 nanometers -1000 nanometers
Alkene composite porous material.
The sodium bicarbonate, quality are the 1.7-1.8% of sodium metasilicate quality；
The dehydration is preferably dehydrated 30-40 minutes, and rotating speed is 500-800 revs/min.
The drying, preferably 100-106 DEG C 2-3 hours dry.
（2）Prepare graphene dispersion suspension
By grain size be 350-400 nanometers of graphene dispersion in NMP carriers, high-speed stirred 2-3 hours is made into graphene content
Graphene dispersion suspension for 24-28%.
（3）Prepare flame retarding function master batch
Silica-graphene composite porous material and graphene dispersion suspension, dried PET material, auxiliary agent addition is close
Mixing in mill, the temperature of mixing is 130-135 DEG C, and the time is 10 minutes, then adds in fire retardant, and control mixing temperature is
150-155 DEG C, 20MPa is boosted to the speed of 2MPa/min, is kept for 5 minutes, is then depressurized to often with the speed of 1MPa/min
Pressure then after single screw extrusion machine extruding pelletization and recycling design NMP, obtains flame retarding function master batch.
The temperature of the single screw extrusion machine is 270-275 DEG C, and screw speed is 80 ~ 100 revs/min, Screw Extrusion pressure
For 2.5-3Mpa；
The fire retardant is made of decabromodiphenyl oxide and melamine cyanurate, mass ratio 1:1.5-2；
The fire retardant, adding proportion are the 10-15% of common PET material dry weight；
The auxiliary agent, adding proportion are the 3-4% of common PET material dry weight；
The auxiliary agent, in parts by weight, including following components：
10 parts of ethylene bis stearic acid amide, 2 parts of calcium stearate, 3 parts of water calcium lotion, 4 parts of isopropanolamine, 1 part of hydroxyl magnesium silicate, fat
2 parts of fat amine polyoxyethylene ether；
The water calcium lotion, model YZS-03D, solid content 45%, viscosity≤150mPa.s（25℃）；
The silica-graphene composite porous material expects the 28-32% of dry weight for PET；
Graphene powder in the graphene dispersion suspension expects the 13-16% of dry weight for PET.
The dried common PET material, water content 70ppm-80ppm.
（4）Melt spinning
Dried common PET material and flame retarding function master batch are sent into screw extruder heating melting, the mixture of molten condition
Be pressurized to 40-45MPa by booster pump, after squeeze into Super-high pressure kettle, 350-410Mpa is pressurized to the rate of 3-5MPa/min, protect
Pressure 4-5 hour after, be slowly decompressed to normal pressure state at 2-3 hour, then through manifold filter with metering pump distribution, then spinneret into
Tow；Spinning speed is 1300-1380m/min；
The screw extruder, the rotating speed of screw rod is 35-40r/min, and melting temperature is 280-290 DEG C；
The flame retarding function master batch account for it is dry after the mass fraction of the sum of common PET material and flame retarding function master batch be 30%-35%.
The dried common PET material, flame retarding function master batch, water content 70ppm-80ppm.
（5）It is cooled and shaped
Tow is molded by the cooling and shaping by ring wind quenching, and wind-warm syndrome is 17 DEG C -19 DEG C, and ring blowing speed is 1.4m/s-
1.8m/s。
（6）It stretches, wind, thermal finalization
It stretched, wound and thermal finalization using three groups of godets, the temperature of first group of godet is 120-130 DEG C, and rotating speed is
1000-1100m/min, the temperature of second group of godet is 185-190 DEG C, rotating speed 2900-2950m/min, third group seal wire
The temperature of roller is 165-170 DEG C, rotating speed 1500-1550m/min,
Total draw ratio is 2.0-2.5 times.
（7）Post processing
By conventional post processing, the graphene nylon fibre of the present invention is obtained.
By adopting the above-described technical solution, the present invention reach have the technical effect that：
（1）The present invention overcomes influence of the addition to the viscosity and mobility of chinlon master batch of graphene, and it is female to reduce melting polyamide fibre
The viscosity of grain improves the mobility of melting chinlon master batch.
（2）Graphene nylon fibre prepared by the present invention, graphene content are 3.5-4.5%, and it is 60- to do fracture strength
65N/tex, elongation at break 18-24%, Young's modulus 2.3-2.8Gpa；Limit oxygen index is up to 35.5-36%, and air penetrability is
240-242mm/s；The conductivity of fiber reaches 8.0-8.5 × 10-7S/cm, 260 DEG C of dry-hot shrinkages are less than 5.0%, in 390-400
DEG C hot melt contracting is less than 9%.
The Young's modulus of common polyamide fibre is easily deformed in 1.4Gpa or so.
Specific embodiment
The following describes the present invention in detail with reference to examples.Following embodiment will be helpful to those skilled in the art
The present invention is further understood, but the invention is not limited in any way.It should be pointed out that those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it can also make certain adjustments and improvements.These belong to the guarantor of the present invention
Protect range.
1 a kind of graphene Jinlun-6 fireproof fiber of embodiment and preparation method thereof
Include the following steps：
（1）Prepare silica-graphene composite porous material
Include the following steps：
The sodium metasilicate that the graphene that grain size is 400 nanometers is pressed to 8% addition a concentration of 35% of the dry silicic acid quality to production is water-soluble
In liquid, sodium bicarbonate is added in, 55 DEG C of heat preservations are being warming up to the speed of 1 DEG C/min after being sufficiently stirred 1 hour, are being carried out at the same time ultrasound
Wave ultrasound 2 hours while then stirring under 42 revs/min of rate, is slowly added to dilute sulfuric acid, pH to 5 is adjusted, up to no wadding
Shape precipitates and bubble generates；Graphene silicic acid gel substance is obtained after filtering, after dehydration, drying, temperature was increased in 35 minutes
To 155 DEG C, soaking time is after 4 hours to weight free of losses, and it is 1 micron that grain size is obtained after crushing, and porosity is 68%, aperture
In 900 nanometers of silica-graphene composite porous material.
The sodium bicarbonate, quality are the 1.7% of sodium metasilicate quality；
The dehydration is preferably dehydrated 30 minutes, and rotating speed is 800 revs/min.
The drying, preferably 100 DEG C dryings 3 hours.
（2）Prepare graphene dispersion suspension
By grain size be 350 nanometers of graphene dispersion in NMP carriers, high-speed stirred 2 hours, it is 24% to be made into graphene content
Graphene dispersion suspension.
（3）Prepare flame retarding function master batch
Silica-graphene composite porous material and graphene dispersion suspension, dried PET material, auxiliary agent addition is close
Mixing in mill, the temperature of mixing is 130 DEG C, and the time is 10 minutes, then adds in fire retardant, and control mixing temperature is 150 DEG C,
20MPa is boosted to the speed of 2MPa/min, is kept for 5 minutes, normal pressure is then depressurized to the speed of 1MPa/min, is then passed through
Single screw extrusion machine extruding pelletization simultaneously after recycling design NMP, obtains flame retarding function master batch.
The temperature of the single screw extrusion machine is 270 DEG C, and screw speed is 80 revs/min, and Screw Extrusion pressure is 2.5Mpa；
The fire retardant is made of decabromodiphenyl oxide and melamine cyanurate, mass ratio 1:1.5；
The fire retardant, adding proportion are the 10% of common PET material dry weight；
The auxiliary agent, adding proportion are the 3% of common PET material dry weight；
The auxiliary agent, in parts by weight, including following components：
10 parts of ethylene bis stearic acid amide, 2 parts of calcium stearate, 3 parts of water calcium lotion, 4 parts of isopropanolamine, 1 part of hydroxyl magnesium silicate, fat
2 parts of fat amine polyoxyethylene ether；
The water calcium lotion, model YZS-03D, solid content 45%, viscosity≤150mPa.s（25℃）；
The silica-graphene composite porous material expects the 28% of dry weight for PET；
Graphene powder in the graphene dispersion suspension expects the 13% of dry weight for PET.
The dried common PET material, water content 70ppm-80ppm.
（4）Melt spinning
Dried common PET material and flame retarding function master batch are sent into screw extruder heating melting, the mixture of molten condition
Be pressurized to 40MPa by booster pump, after squeeze into Super-high pressure kettle, 350Mpa, pressurize 4 hours are pressurized to the rate of 3MPa/min
Afterwards, normal pressure state slowly was decompressed at 2 hours, is then distributed through manifold filtering and metering pump, then spinneret is into tow；Spinning speed
It spends for 1300m/min；
The screw extruder, the rotating speed of screw rod is 35r/min, and melting temperature is 280 DEG C；
The flame retarding function master batch account for it is dry after the mass fraction of the sum of common PET material and flame retarding function master batch be 30%%.
The dried common PET material, flame retarding function master batch, water content 70ppm-80ppm.
（5）It is cooled and shaped
Tow is molded by the cooling and shaping by ring wind quenching, and wind-warm syndrome is 17 DEG C, and ring blowing speed is 1.4m/s.
（6）It stretches, wind, thermal finalization
It stretched, wound and thermal finalization using three groups of godets, the temperature of first group of godet is 120 DEG C, and rotating speed is
1000m/min, the temperature of second group of godet is 185 DEG C, rotating speed 2900m/min, and the temperature of third group godet is 165
DEG C, rotating speed 1500m/min,
Total draw ratio is 2.0 times.
（7）Post processing
By conventional post processing, the graphene nylon fibre of the present invention is obtained.
Graphene nylon fibre prepared by the embodiment of the present invention 1, graphene content are 3.5%, and it is 61N/ to do fracture strength
Tex, elongation at break 18%, Young's modulus are 2.3 Gpa, and limit oxygen index is up to 35.7%, air penetrability 241mm/s；Fiber
Conductivity up to 8.2 × 10-7S/cm。
2 a kind of graphene Jinlun-6 fireproof fiber of embodiment and preparation method thereof
Include the following steps：
（1）Prepare silica-graphene composite porous material
Include the following steps：
The sodium metasilicate that the graphene that grain size is 500 nanometers is pressed to 10% addition a concentration of 38% of the dry silicic acid quality to production is water-soluble
In liquid, sodium bicarbonate is added in, 60 DEG C of heat preservations are being warming up to the speed of 1.3 DEG C/min after being sufficiently stirred 2 hours, are being carried out at the same time super
Sound wave ultrasound 3 hours while then stirring under 50 revs/min of rate, is slowly added to dilute sulfuric acid, adjusts pH to 6, until nothing
Flocculent deposit and bubble generate；Graphene silicic acid gel substance is obtained after filtering, after dehydration, drying, temperature was increased in 38 minutes
Degree is to 162 DEG C, and soaking time is after 4-5 hours to weight free of losses, and it is 1.3 microns that grain size is obtained after crushing, and porosity exists
70%, silica-graphene composite porous material of the aperture at 970 nanometers.
The sodium bicarbonate, quality are the 1.8% of sodium metasilicate quality；
The dehydration is preferably dehydrated 40 minutes, and rotating speed is 800 revs/min.
The drying, preferably 106 DEG C dryings 2 hours.
（2）Prepare graphene dispersion suspension
By grain size be 400 nanometers of graphene dispersion in NMP carriers, high-speed stirred 2.5 hours, being made into graphene content is
25% graphene dispersion suspension.
（3）Prepare flame retarding function master batch
Silica-graphene composite porous material and graphene dispersion suspension, dried PET material, auxiliary agent addition is close
Mixing in mill, the temperature of mixing is 132 DEG C, and the time is 10 minutes, then adds in fire retardant, and control mixing temperature is 153 DEG C,
20MPa is boosted to the speed of 2MPa/min, is kept for 5 minutes, normal pressure is then depressurized to the speed of 1MPa/min, is then passed through
Single screw extrusion machine extruding pelletization simultaneously after recycling design NMP, obtains flame retarding function master batch.
The temperature of the single screw extrusion machine is 272 DEG C, and screw speed is 95 revs/min, and Screw Extrusion pressure is 2.8Mpa；
The fire retardant is made of decabromodiphenyl oxide and melamine cyanurate, mass ratio 1:1.7；
The fire retardant, adding proportion are the 12% of common PET material dry weight；
The auxiliary agent, adding proportion are the 3.3% of common PET material dry weight；
The auxiliary agent, in parts by weight, including following components：
10 parts of ethylene bis stearic acid amide, 2 parts of calcium stearate, 3 parts of water calcium lotion, 4 parts of isopropanolamine, 1 part of hydroxyl magnesium silicate, fat
2 parts of fat amine polyoxyethylene ether；
The water calcium lotion, model YZS-03D, solid content 45%, viscosity≤150mPa.s（25℃）；
The silica-graphene composite porous material expects the 30% of dry weight for PET；
Graphene powder in the graphene dispersion suspension expects the 15% of dry weight for PET.
The dried common PET material, water content 70ppm-80ppm.
（4）Melt spinning
Dried common PET material and flame retarding function master batch are sent into screw extruder heating melting, the mixture of molten condition
Be pressurized to 45MPa by booster pump, after squeeze into Super-high pressure kettle, 400Mpa, pressurize 4 hours are pressurized to the rate of 4MPa/min
Afterwards, normal pressure state slowly was decompressed at 2 hours, is then distributed through manifold filtering and metering pump, then spinneret is into tow；Spinning speed
It spends for 1380m/min；
The screw extruder, the rotating speed of screw rod is 40r/min, and melting temperature is 285 DEG C；
The flame retarding function master batch account for it is dry after the mass fraction of the sum of common PET material and flame retarding function master batch be 32%.
The dried common PET material, flame retarding function master batch, water content 70ppm-80ppm.
（5）It is cooled and shaped
Tow is molded by the cooling and shaping by ring wind quenching, and wind-warm syndrome is 18 DEG C, and ring blowing speed is 1.5m/s.
（6）It stretches, wind, thermal finalization
It stretched, wound and thermal finalization using three groups of godets, the temperature of first group of godet is 128 DEG C, and rotating speed is
1080m/min, the temperature of second group of godet is 190 DEG C, rotating speed 2900m/min, and the temperature of third group godet is 170
DEG C, rotating speed 1550m/min,
Total draw ratio is 2.4 times.
（7）Post processing
By conventional post processing, the graphene nylon fibre of the present invention is obtained.
Graphene nylon fibre prepared by the embodiment of the present invention 2, graphene content are 4.0%, and it is 65N/ to do fracture strength
Tex, elongation at break 24%, Young's modulus 2.8Gpa, limit oxygen index are up to 36%, air penetrability 242mm/s；The electricity of fiber
Conductance is up to 8.5 × 10-7S/cm。
3 a kind of graphene Jinlun-6 fireproof fiber of embodiment and preparation method thereof
Include the following steps：
（1）Prepare silica-graphene composite porous material
Include the following steps：
The sodium metasilicate that the graphene that grain size is 600 nanometers is pressed to 11% addition a concentration of 40% of the dry silicic acid quality to production is water-soluble
In liquid, sodium bicarbonate is added in, 65 DEG C of heat preservations are being warming up to the speed of 1.5 DEG C/min after being sufficiently stirred 1-2 hours, are being carried out at the same time
Ultrasonic echography 3 hours while then stirring under 50 revs/min of rate, is slowly added to dilute sulfuric acid, adjusts pH to 5, until
No flocculent deposit and bubble generate；Graphene silicic acid gel substance is obtained after filtering, after dehydration, drying, was increased in 40 minutes
Temperature is to 165 DEG C, and soaking time is after 5 hours to weight free of losses, and it is 1.5 microns that grain size is obtained after crushing, and porosity exists
75%, silica-graphene composite porous material of the aperture at 1000 nanometers.
The sodium bicarbonate, quality are the 1.8% of sodium metasilicate quality；
The dehydration is preferably dehydrated 40 minutes, and rotating speed is 500 revs/min.
The drying, preferably 100 DEG C dryings 2.5 hours.
（2）Prepare graphene dispersion suspension
By grain size be 400 nanometers of graphene dispersion in NMP carriers, high-speed stirred 3 hours, it is 28% to be made into graphene content
Graphene dispersion suspension.
（3）Prepare flame retarding function master batch
Silica-graphene composite porous material and graphene dispersion suspension, dried PET material, auxiliary agent addition is close
Mixing in mill, the temperature of mixing is 135 DEG C, and the time is 10 minutes, then adds in fire retardant, and control mixing temperature is 155 DEG C,
20MPa is boosted to the speed of 2MPa/min, is kept for 5 minutes, normal pressure is then depressurized to the speed of 1MPa/min, is then passed through
Single screw extrusion machine extruding pelletization simultaneously after recycling design NMP, obtains flame retarding function master batch.
The temperature of the single screw extrusion machine is 275 DEG C, and screw speed is 100 revs/min, and Screw Extrusion pressure is 3Mpa；
The fire retardant is made of decabromodiphenyl oxide and melamine cyanurate, mass ratio 1:2；
The fire retardant, adding proportion are the 15% of common PET material dry weight；
The auxiliary agent, adding proportion are the 4% of common PET material dry weight；
The auxiliary agent, in parts by weight, including following components：
10 parts of ethylene bis stearic acid amide, 2 parts of calcium stearate, 3 parts of water calcium lotion, 4 parts of isopropanolamine, 1 part of hydroxyl magnesium silicate, fat
2 parts of fat amine polyoxyethylene ether；
The water calcium lotion, model YZS-03D, solid content 45%, viscosity≤150mPa.s（25℃）；
The silica-graphene composite porous material expects the 32% of dry weight for PET；
Graphene powder in the graphene dispersion suspension expects the 16% of dry weight for PET.
The dried common PET material, water content 70ppm-80ppm.
（4）Melt spinning
Dried common PET material and flame retarding function master batch are sent into screw extruder heating melting, the mixture of molten condition
Be pressurized to 45MPa by booster pump, after squeeze into Super-high pressure kettle, 410Mpa, pressurize 4 hours are pressurized to the rate of 5MPa/min
Afterwards, normal pressure state slowly was decompressed at 2 hours, is then distributed through manifold filtering and metering pump, then spinneret is into tow；Spinning speed
It spends for 1380m/min；
The screw extruder, the rotating speed of screw rod is 40r/min, and melting temperature is 290 DEG C；
The flame retarding function master batch account for it is dry after the mass fraction of the sum of common PET material and flame retarding function master batch be 35%.
The dried common PET material, flame retarding function master batch, water content 70ppm-80ppm.
（5）It is cooled and shaped
Tow is molded by the cooling and shaping by ring wind quenching, 19 DEG C of wind-warm syndrome, and ring blowing speed is 1.8m/s.
（6）It stretches, wind, thermal finalization
It stretched, wound and thermal finalization using three groups of godets, the temperature of first group of godet is 130 DEG C, and rotating speed is
1100m/min, the temperature of second group of godet is 190 DEG C, rotating speed 2900m/min, and the temperature of third group godet is 170
DEG C, rotating speed 1550m/min,
Total draw ratio is 2.5 times.
（7）Post processing
By conventional post processing, the graphene nylon fibre of the present invention is obtained.
Graphene nylon fibre prepared by the embodiment of the present invention 3, graphene content are 4.5%, and it is 60N/ to do fracture strength
Tex, elongation at break 20%, Young's modulus 2.5Gpa, limit oxygen index are up to 35.6%, air penetrability 240mm/s；Fiber
Conductivity is up to 8.0 × 10-7S/cm。
The test method of air penetrability of the present invention is detected for GBT5453-1997 textile fabrics gas permeability.
Unless otherwise indicated, the percentage employed in the present invention is weight percent, ratio of the present invention,
For mass ratio.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (10)
1. a kind of graphene Jinlun-6 fireproof fiber, it is characterised in that：The fiber, graphene content be 3.5-4.5%, limit oxygen
Index is 35.5-36%.
2. a kind of graphene Jinlun-6 fireproof fiber according to claim 1, it is characterised in that：It is strong to do fracture for the fiber
It spends for 60-65N/tex, Young's modulus 2.3-2.8Gpa.
3. a kind of preparation method of graphene Jinlun-6 fireproof fiber, it is characterised in that：The preparation method, including preparing titanium dioxide
Silicon-graphene composite porous material prepares graphene dispersion suspension, prepares flame retarding function master batch, melt spinning is cooled to
Type is stretched, is wound, thermal finalization.
4. a kind of preparation method of graphene Jinlun-6 fireproof fiber according to claim 3, it is characterised in that：The preparation
Silica-graphene composite porous material with graphene dispersion suspension, dried PET is expected, helped by flame retarding function master batch
Agent carries out mixing, and the temperature of mixing is 130-135 DEG C, and the time is 10 minutes, then adds in fire retardant, and control mixing temperature is
150-155 DEG C, 20MPa is boosted to the speed of 2MPa/min, is kept for 5 minutes, is then depressurized to often with the speed of 1MPa/min
Pressure then after single screw extrusion machine extruding pelletization and recycling design NMP, obtains flame retarding function master batch.
5. a kind of preparation method of graphene Jinlun-6 fireproof fiber according to claim 4, it is characterised in that：The list spiral shell
The temperature of bar extruder is 270-275 DEG C, and screw speed is 80 ~ 100 revs/min, and Screw Extrusion pressure is 2.5-3Mpa.
6. a kind of preparation method of graphene Jinlun-6 fireproof fiber according to claim 4, it is characterised in that：It is described fire-retardant
Agent is made of decabromodiphenyl oxide and melamine cyanurate, mass ratio 1:1.5-2.
7. a kind of preparation method of graphene Jinlun-6 fireproof fiber according to claim 4, it is characterised in that：It is described fire-retardant
Agent, adding proportion are the 10-15% of common PET material dry weight；The auxiliary agent, adding proportion are common PET material dry weight
3-4%；The silica-graphene composite porous material expects the 28-32% of dry weight for PET；The graphene dispersion
Graphene powder in suspension expects the 13-16% of dry weight for PET.
8. a kind of preparation method of graphene Jinlun-6 fireproof fiber according to claim 4, it is characterised in that：It is described to help
Agent, in parts by weight, including following components：10 parts of ethylene bis stearic acid amide, 2 parts of calcium stearate, 3 parts of water calcium lotion, isopropyl
4 parts of hydramine, 1 part of hydroxyl magnesium silicate, 2 parts of aliphatic amine polyoxyethylene ether.
9. a kind of preparation method of graphene Jinlun-6 fireproof fiber according to claim 3, it is characterised in that：The melting
Dried common PET material and flame retarding function master batch are sent into screw extruder heating melting, the mixture of molten condition by spinning
Be pressurized to 40-45MPa by booster pump, after squeeze into Super-high pressure kettle, 350-410Mpa is pressurized to the rate of 3-5MPa/min, protect
Pressure 4-5 hour after, be slowly decompressed to normal pressure state at 2-3 hour, then through manifold filter with metering pump distribution, then spinneret into
Tow；Spinning speed is 1300-1380m/min.
10. a kind of preparation method of graphene Jinlun-6 fireproof fiber according to claim 9, it is characterised in that：The spiral shell
Bar extruder, the rotating speed of screw rod is 35-40r/min, and melting temperature is 280-290 DEG C；
The flame retarding function master batch account for it is dry after the mass fraction of the sum of common PET material and flame retarding function master batch be 30%-35%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711270979.4A CN108149337A (en) | 2017-12-05 | 2017-12-05 | A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711270979.4A CN108149337A (en) | 2017-12-05 | 2017-12-05 | A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108149337A true CN108149337A (en) | 2018-06-12 |
Family
ID=62465987
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711270979.4A Pending CN108149337A (en) | 2017-12-05 | 2017-12-05 | A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108149337A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109056147A (en) * | 2018-08-31 | 2018-12-21 | 宜兴中大纺织有限公司 | Imitative cotton face fabric and preparation method thereof is washed entirely |
| CN110306267A (en) * | 2019-06-17 | 2019-10-08 | 张家港市荣昌涤纶毛条有限公司 | The production technology of graphene fiber wool top |
| CN111379162A (en) * | 2020-04-01 | 2020-07-07 | 青岛大学 | Softening method of ramie fibers |
| CN111593429A (en) * | 2020-07-03 | 2020-08-28 | 南通文凯化纤有限公司 | Graphene nylon yarn and preparation method thereof |
| CN113417026A (en) * | 2021-07-23 | 2021-09-21 | 南通强生石墨烯科技有限公司 | Graphene high-thermal-insulation fiber and preparation method thereof |
| CN117285798A (en) * | 2022-10-17 | 2023-12-26 | 南通开普乐工程塑料有限公司 | High-temperature-resistant flame-retardant PET material for coil frameworks and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088385A (en) * | 2015-09-02 | 2015-11-25 | 太仓市宏亿化纤有限公司 | Flame-retarding polyamide fabric and preparation method thereof |
| CN106676664A (en) * | 2016-08-31 | 2017-05-17 | 浙江金旗新材料科技有限公司 | Flame-retardant and wear-resistant type chinlon 6 pre-oriented yarn |
| CN106811820A (en) * | 2016-04-01 | 2017-06-09 | 青岛大学 | A kind of preparation method of fire-retardant anti-molten droplet fiber |
| CN107119342A (en) * | 2017-06-05 | 2017-09-01 | 上海帕吉索纳米技术有限公司 | A kind of superelevation conductive graphene polyester fiber and preparation method thereof |
-
2017
- 2017-12-05 CN CN201711270979.4A patent/CN108149337A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088385A (en) * | 2015-09-02 | 2015-11-25 | 太仓市宏亿化纤有限公司 | Flame-retarding polyamide fabric and preparation method thereof |
| CN106811820A (en) * | 2016-04-01 | 2017-06-09 | 青岛大学 | A kind of preparation method of fire-retardant anti-molten droplet fiber |
| CN106676664A (en) * | 2016-08-31 | 2017-05-17 | 浙江金旗新材料科技有限公司 | Flame-retardant and wear-resistant type chinlon 6 pre-oriented yarn |
| CN107119342A (en) * | 2017-06-05 | 2017-09-01 | 上海帕吉索纳米技术有限公司 | A kind of superelevation conductive graphene polyester fiber and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109056147A (en) * | 2018-08-31 | 2018-12-21 | 宜兴中大纺织有限公司 | Imitative cotton face fabric and preparation method thereof is washed entirely |
| CN110306267A (en) * | 2019-06-17 | 2019-10-08 | 张家港市荣昌涤纶毛条有限公司 | The production technology of graphene fiber wool top |
| CN110306267B (en) * | 2019-06-17 | 2022-04-29 | 张家港市荣昌涤纶毛条有限公司 | Production process of graphene fiber wool tops |
| CN111379162A (en) * | 2020-04-01 | 2020-07-07 | 青岛大学 | Softening method of ramie fibers |
| CN111379162B (en) * | 2020-04-01 | 2022-06-17 | 青岛大学 | Softening method of ramie fibers |
| CN111593429A (en) * | 2020-07-03 | 2020-08-28 | 南通文凯化纤有限公司 | Graphene nylon yarn and preparation method thereof |
| CN113417026A (en) * | 2021-07-23 | 2021-09-21 | 南通强生石墨烯科技有限公司 | Graphene high-thermal-insulation fiber and preparation method thereof |
| CN113417026B (en) * | 2021-07-23 | 2022-03-29 | 南通强生石墨烯科技有限公司 | Graphene high-thermal-insulation fiber and preparation method thereof |
| CN117285798A (en) * | 2022-10-17 | 2023-12-26 | 南通开普乐工程塑料有限公司 | High-temperature-resistant flame-retardant PET material for coil frameworks and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108149337A (en) | A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof | |
| CN108316039B (en) | A kind of method that mechanical couplings chemistry alkali soluble method prepares aramid nano-fiber | |
| CN112301508B (en) | Silicon dioxide aerogel composite thermal insulation fabric and preparation method thereof | |
| CN108277548B (en) | Graphene polyester flame-retardant fiber and preparation method thereof | |
| AU2012224609A1 (en) | Method for dry spinning neutral and anionically modified cellulose and fibres made using the method | |
| CN109516763A (en) | A kind of cellulose fibre/SiO2Aerogel composite and its preparation and application | |
| CN107761249A (en) | A kind of Graphene glass fibrous composite and preparation method thereof | |
| CN109998199B (en) | Preparation method of anti-fogging and anti-haze mask material | |
| KR20110121722A (en) | Process for production of precursor fiber for preparing carbon fiber having high strength and high elastic modulus | |
| CN108047661A (en) | A kind of graphene dacron master grain and preparation method thereof | |
| CN105177751A (en) | Colored anti-ultraviolet profiled fine denier polyester filament and preparation method thereof | |
| CN109267164B (en) | Preparation method of cellulose graphene composite filament | |
| CN109183170B (en) | Preparation method of cellulose graphene composite short fiber | |
| CN110735198A (en) | modified PET polyester fiber, preparation method thereof and polyester fabric | |
| CN108486676B (en) | Nano cellulose modified acrylic fiber, preparation method and application thereof | |
| CN105401252A (en) | Preparation method of flame-retardant PET fiber | |
| CN106757511A (en) | The modified nylon fiber and its preparation technology of a kind of platelet of Graphene containing polymolecularity and liquid phase surface conductance film | |
| CN106566208B (en) | The non-conductive light-duty fishing rod composite material of high tenacity | |
| CN116024695A (en) | Light-colored light energy heating thermal fiber and preparation method thereof | |
| CN114177850B (en) | Air microcapsule and preparation method thereof, thermal cellulose fiber and preparation method and application thereof | |
| CN108395201B (en) | Preparation method of environment-friendly heat-insulation composite aerogel material | |
| CN108624984B (en) | Preparation method of cellulose silkworm silk protein composite fiber | |
| CN113024880A (en) | Preparation method of cellulose acetate nanofiber composite aerogel for heat preservation | |
| WO2016184390A1 (en) | Spinning forming method for coloured flame-retardant viscose filaments and staple fibres without dyeing | |
| CN115161792B (en) | Washable light thermal aerogel regenerated cellulose fiber and preparation method thereof |
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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20190203 Address after: 315400 28 Xingping Road, Zhongyi Ningbo ecological park, Yuyao, Ningbo, Zhejiang Applicant after: Yuyao Pajiso New Materials Technology Co., Ltd. Address before: Room 2088, Building 2, 3601 Dongfang Road, Pudong New Area, Shanghai, 200125 Applicant before: Shanghai Pajisuo nanotechnology Co. Ltd. |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180612 |