CN108277548A - A kind of graphene terylene fire resistance fibre and preparation method thereof - Google Patents
A kind of graphene terylene fire resistance fibre and preparation method thereof Download PDFInfo
- Publication number
- CN108277548A CN108277548A CN201810040880.3A CN201810040880A CN108277548A CN 108277548 A CN108277548 A CN 108277548A CN 201810040880 A CN201810040880 A CN 201810040880A CN 108277548 A CN108277548 A CN 108277548A
- Authority
- CN
- China
- Prior art keywords
- graphene
- fire resistance
- preparation
- resistance fibre
- terylene fire
- 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.)
- Granted
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)
- Inorganic Fibers (AREA)
Abstract
The present invention provides a kind of graphene terylene fire resistance fibre, the fiber, and graphene content is 1.5 3.5%, and it is 6.1 6.5cN/dtex to do fracture strength, and limit oxygen index is 31 33%；The present invention also provides a kind of preparation method of graphene terylene fire resistance fibre, the preparation methods, including prepare silica graphene composite porous material, prepare graphene dispersion suspension, prepare mixed function master batch, melt spinning, cooling and shaping, drawing-off.Graphene terylene fire resistance fibre prepared by the present invention, graphene content are 1.5 3.5%, and it is 6.1 6.5cN/dtex to do fracture strength, and elongation at break 6.0 7.3%, for 200 DEG C of dry-hot shrinkages less than 0.8 1.2%, limit oxygen index is up to 31 33%；Graphene terylene fire resistance fibre of the present invention, chance high temperature melting shrinkage is low, and collapsing rate is less than 2 3% in 20 minutes under 500 600 DEG C of ignition temperatures.
Description
Technical field
The present invention relates to a kind of polyester fiber, especially a kind of graphene terylene fire resistance fibre and preparation method thereof belongs to
Textile technology field.
Background technology
Terylene is world wide production maximum, and most widely used synthetic fibers kind, terylene accounts for world's synthetic fibers yield
60% or more.
Graphene has very high electric conductivity, is the material of resistivity minimum in the world, graphene can be added to fibre
It ties up in material, improves the electric conductivity of fiber；Graphene also has antibiotic property, anti-flammability and radiation resistance, can assign fiber system
The different function of product.
Deficiency is existing for prior art preparation graphene terylene fire resistance fibre：
（1）In order to reduce influence of the graphene to fiber mechanical performance and spinnability, graphene in the fibre additive amount generally compared with
Few, therefore, the strength and anti-flammability of the graphene terylene fire resistance fibre of prior art preparation are relatively low, generally require additional addition
Fire retardant could improve the flame retardant property of fiber.
（2）The graphene terylene fire resistance fibre of prior art preparation, there are high temperature collapsing, the problem of scalding is dripped in melting.
Invention content
In view of the deficiencies of the prior art, a kind of graphene terylene fire resistance fibre of present invention offer and preparation method thereof, with reality
Now following goal of the invention：
（1）The graphene terylene fire resistance fibre of preparation, intensity is high, flame retardant property is good；
（2）The graphene terylene fire resistance fibre of preparation meets high temperature not collapsing.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is：
A kind of graphene terylene fire resistance fibre, the fiber, graphene content are 1.5-3.5%, and it is 6.1- to do fracture strength
6.5cN/dtex, limit oxygen index 31-33%.
It is to be further improved to above-mentioned technical proposal below：
The fiber, under 500-600 DEG C of ignition temperature, the collapsing rate in 20 minutes is less than 2-3%.
A kind of preparation method of graphene terylene fire resistance fibre, the preparation method, including prepare silica-graphene
Composite porous material prepares graphene dispersion suspension, prepares mixed function master batch, melt spinning, cooling and shaping, drawing-off.
It is described to prepare silica-graphene composite porous material, include the following steps：
The graphene that grain size is 300-500 nanometers is added a concentration of 30-40%'s by the 6-10% to the dry silicic acid quality of production
In sodium silicate aqueous solution, sodium bicarbonate is added, is to slowly warm up to 50-60 DEG C of guarantor after being sufficiently stirred 2-3 hours in 50-70 minutes
Temperature, ultrasonic echography 2-3 hours while stirring under 30-40 revs/min of rate, are slowly added to dilute sulfuric acid, adjust pH to 5-
6, up to no flocculent deposit and bubble generate；Graphene silicic acid gel substance is obtained after filtering, after dehydration, drying, at 20-30 points
Temperature is increased in clock to 150-160 DEG C, soaking time is after 4-5 hours to weight free of losses, and it is 3-3.5 that grain size is obtained after crushing
Micron, porosity is in 60-70%, silica-graphene composite porous material of the aperture at 600 nanometers -1000 nanometers.
The sodium bicarbonate, quality are the 1.5-1.7% of sodium metasilicate quality；
The filtering, preferably sheet frame filter are filtered, and use intermittent pressure pump by frequency conversion rate for 0.16-0.20Mpa/10 seconds
Rate boost or depressurization, 0.5-0.8Mpa is maintained, after obtaining silicic acid gel substance；
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；
Grain size is 200-400 nanometer of graphene dispersion in NMP carriers, at a high speed by the preparation graphene dispersion suspension
Stirring 2-3 hours is made into the graphene dispersion suspension that graphene content is 20-25%.
The preparation mixed function master batch, by silica-graphene composite porous material and graphene dispersion suspension,
Mixing in mixer is added in PET material, auxiliary agent ethylene bis stearic acid amide and calcium stearate after drying, and extruding pelletization simultaneously recycles molten
After agent NMP, mixed function master batch is obtained.
The auxiliary agent is ethylene bis stearic acid amide and calcium stearate, ratio 3:2, adding proportion is that PET expects drying
The 3-4% of weight；
The silica-graphene composite porous material expects the 30-35% of dry weight for PET；
Graphene powder in the graphene dispersion suspension expects the 10-15% of dry weight for PET.
Common PET material after drying and mixed function master batch are sent into screw extruder heating melting, melted by the melt spinning
The mixture for melting state is pressurized to 30-50MPa by booster pump, after squeeze into Super-high pressure kettle, be pressurized in 1-2 hours in kettle
300-500Mpa was slowly decompressed to normal pressure state after pressurize 4-6 hours at 2-3 hours, then through manifold filtering and metering pump
Distribution, then spinneret is at tow, spinning speed 1200-1300m/min；
The metering pump is preferably 1950-2050g/min for amount.
The mixed function master batch account for it is dry after the mass fraction of the sum of common PET material and mixed function master batch be 15%-
25%。
Tow is molded by the cooling and shaping by ring wind quenching, and the ring blowing temperature is 16 DEG C -19 DEG C, the ring
Blowing speed is 8.0m/s-10.0m/s.
The drawing-off, total draft multiple are 1.4-1.8 times；First drafting machine speed is 50m/min-60m/min, is led
The temperature for stretching bath is 80 DEG C -90 DEG C, and the second drafting machine speed is 135m/min-185m/min, and the temperature of heater box is 110
DEG C -120 DEG C, third drafting machine speed is 165m/min-195m/min.
The spinning further includes vacuum drum drying；The vacuum drum drying, first by common PET material vacuum drum
The drying temperature of drying machine, vacuum drum drying machine is 180 DEG C -185 DEG C, and dry 6h-7.5h adds mixed function mother
Grain, mixed function master batch final mass score are 15%-25%, and total drying time is 16h-18h, and water content is in 80ppm-
90ppm then completes drying.
The spinning further includes thermal finalization；The thermal finalization, by the as-spun fibre after drawing-off by curling, oiling treatment
Afterwards, thermal finalization is carried out by heat setting machine, the heat setting temperature is 180 DEG C -185 DEG C, and the heat-setting time is
16min-20min。
By adopting the above-described technical solution, having the technical effect that of reaching of the present invention：
（1）Graphene terylene fire resistance fibre prepared by the present invention, graphene content are 1.5-3.5%, and it is 6.1- to do fracture strength
6.5cN/dtex, elongation at break 6.0-7.3%, 3% corresponding stress of elongation are not less than 4.8 cN/dtex, 200 DEG C of xeothermic contractions
Rate is less than 0.8-1.2%, and limit oxygen index is up to 31-33%.
（2）Graphene terylene fire resistance fibre prepared by the present invention, chance high temperature melting shrinkage is low, in 500-600 DEG C of ignition point temperature
It spends collapsing rate in lower 20 minutes and is less than 2-3%.
（3）Graphene terylene fire resistance fibre prepared by the present invention, fiber regain are 12.5-13.5%, the conductivity of fiber
Up to 8.2-8.7 × 10-7S/cm。
Fiber prepared by the present invention is used primarily in carpet, filler, ornament materials etc..
Specific implementation mode
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 skilled 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 terylene fire resistance fibre of embodiment and preparation method thereof
Include the following steps：
（1）Prepare silica-graphene composite porous material
1）The graphene that grain size is 300-350 nanometers is pressed to the silicic acid of 6% addition a concentration of 30% to the dry silicic acid quality of production
In sodium water solution, sodium bicarbonate is added, is to slowly warm up to 50-52 DEG C of heat preservation after being sufficiently stirred 2-2.5 hours in 50 minutes, surpasses
Sound wave ultrasound 2 hours while stirring under 30 revs/min of rate, is slowly added to dilute sulfuric acid, adjusts pH to 5, until without cotton-shaped
Precipitation and bubble generate.
The flocculent deposit is siliceous colloid, mainly the mixture of silicic acid, two silicic acid, orthosilicic acid, metasilicic acid.
The sodium bicarbonate, quality are the 1.5% of sodium metasilicate quality.
2）Using the filter cloth tissue of+9000 mesh flannelette of+8000 mesh silk of+6000 mesh stainless steel filtering net of 5000 mesh flannelette（On
The arrangement for stating filter cloth is from outside to inside）Sheet frame filter filtering, use intermittent pressure pump by frequency conversion rate for 0.16Mpa/10
The rate boosting of second, maintains 0.5Mpa, is dehydrated 30 minutes after obtaining silicic acid gel substance, and rotating speed is 500 revs/min.
3）By dewatered graphene-silica-gel mixture, after 2 hours dry at 100-102 DEG C, temperature is increased in 20 minutes
Degree is to 150 DEG C, and soaking time is 4 hours to after weight free of losses, and it is 3 microns that grain size is obtained after crushing, and porosity is 60%, hole
Silica-graphene composite porous material A of the diameter at 600 nanometers.
（2）Prepare graphene dispersion suspension
It is 200 nanometers of graphene dispersion in NMP carriers by grain size, high-speed stirred 2-3 hours, being made into graphene content is
The graphene dispersion suspension B of 20% favorable dispersibility.
（3）Prepare mixed function master batch
By step（1）The silica of gained-graphene composite porous material A and step（2）The graphene dispersion of gained is suspended
Mixing in mixer is added in liquid B, PET material, auxiliary agent ethylene bis stearic acid amide and calcium stearate, through double-screw extruding pelletizing and returns
After receiving solvent NMP, mixed function master batch is obtained.
The auxiliary agent is ethylene bis stearic acid amide and calcium stearate, ratio 3:2, adding proportion is that PET expects drying
The 3% of weight.
The silica-graphene composite porous material, expect dry weight for PET 30%；
Graphene powder in the graphene dispersion suspension, expect dry weight for PET 10%；
（4）Spinning
1）Vacuum drum is dried：First by common PET material vacuum drum drying machine, the drying temperature of vacuum drum drying machine is
180 DEG C DEG C, dry 6h, mixed function master batch is added, mixed function master batch final mass score is 15%, total drying time
For 16h, water content then completes drying in 80ppm.
2）Melt spinning：Common PET material and mixed function master batch are sent into screw extruder heating melting after will be dry, molten
The mixture for melting state is pressurized to 30MPa by booster pump, after squeeze into Super-high pressure kettle, be pressurized to 300Mpa in 1 hour in kettle,
After pressurize 4 hours, it slowly was decompressed to normal pressure state at 2 hours, is then distributed through manifold filtering and metering pump, then pass through spinneret
Plate spinneret is at tow, and the screw rod and manifold spin manifold temperature of the screw extruder are 285 DEG C, and the hole diameter of spinneret is
The layout of 0.6mm, hole count 6000, the spinneret are 20 circles；
The metering pump is 1950g/min, spinning speed 1200m/min for amount.
3）It is cooled and shaped
Tow is molded by ring wind quenching, the ring blowing temperature is 16 DEG C, and the ring blowing speed is 8.0m/s.
4）Drawing-off
As-spun fibre after boundling is passed sequentially through into the first drafting machine, drawing-off bath, the second drafting machine, heater box and third drawing-off
Machine stretches, and total draft multiple is 1.4 times；
The first drafting machine speed is 50m/min, and the temperature of drawing-off bath is 80 DEG C, and the second drafting machine speed is 135m/
The temperature of min, heater box are 110 DEG C, and third drafting machine speed is 165m/min.
5）Thermal finalization
By the as-spun fibre after drawing-off after curling, oiling treatment, thermal finalization, the thermal finalization temperature are carried out by heat setting machine
Degree is 180 DEG C, and the heat-setting time is 16min.
6）Cut-out
Graphene polyester staple fiber finished product is made after cut-out.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 1, it is 6.1cN/dtex, extension at break to do fracture strength
Rate 6.0%, 3% corresponding stress of elongation are not less than 4.8 cN/dtex, and 200 DEG C of dry-hot shrinkages are less than 1.2%, and limit oxygen index is high
Up to 31%.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 1, chance high temperature melting shrinkage is low, in 500 DEG C of ignition point temperature
It spends collapsing rate in lower 20 minutes and is less than 3%.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 1, fiber regain are 12.5%, the conductivity of fiber
Up to 8.2 × 10-7S/cm。
2 a kind of graphene terylene fire resistance fibre of embodiment and preparation method thereof
Include the following steps：
（1）Prepare silica-graphene composite porous material
1）The graphene that grain size is 370-4100 nanometers is pressed to the silicic acid of 8% addition a concentration of 35% to the dry silicic acid quality of production
In sodium water solution, sodium bicarbonate is added, is to slowly warm up to 57 DEG C of heat preservations, ultrasound after being sufficiently stirred 2.5 hours in 55-58 minutes
Wave ultrasound 2.6 hours while stirring under 33-35 revs/min of rate, is slowly added to dilute sulfuric acid, adjusts pH to 5.4, until
No flocculent deposit and bubble generate.
The flocculent deposit is siliceous colloid, mainly the mixture of silicic acid, two silicic acid, orthosilicic acid, metasilicic acid.
The sodium bicarbonate, quality are the 1.6% of sodium metasilicate quality.
2）Using the filter cloth tissue of+9000 mesh flannelette of+8000 mesh silk of+6000 mesh stainless steel filtering net of 5000 mesh flannelette（On
The arrangement for stating filter cloth is from outside to inside）Sheet frame filter filtering, use intermittent pressure pump by frequency conversion rate for 0.17Mpa/10
The rate boost or depressurization of second, maintains 0.7Mpa, is dehydrated 30 minutes after obtaining silicic acid gel substance, and rotating speed is 700 revs/min.
3）Dewatered graphene-silica-gel mixture is increased into temperature after 2.5 hours dry at 105 DEG C in 27 minutes
To 158 DEG C, soaking time is 4.5 hours to after weight free of losses, and it is 3.2 microns that grain size is obtained after crushing, porosity 68%,
Silica-graphene composite porous material A of the aperture at 850 nanometers.
（2）Prepare graphene dispersion suspension
It is 280-290 nanometers of graphene dispersion in NMP carriers by grain size, high-speed stirred 2-3 hours is made into graphene content
For the graphene dispersion suspension B of 22% favorable dispersibility.
（3）Prepare mixed function master batch
By step（1）The silica of gained-graphene composite porous material A and step（2）The graphene dispersion of gained is suspended
Mixing in mixer is added in liquid B, PET material, auxiliary agent ethylene bis stearic acid amide and calcium stearate, through double-screw extruding pelletizing and returns
After receiving solvent NMP, mixed function master batch is obtained.
The auxiliary agent is ethylene bis stearic acid amide and calcium stearate, ratio 3:2, adding proportion is that PET expects drying
The 3.3% of weight.
The silica-graphene composite porous material, expect dry weight for PET 32%；
Graphene powder in the graphene dispersion suspension, expect dry weight for PET 13%.
（4）Spinning
1）Vacuum drum is dried：First by common PET material vacuum drum drying machine, the drying temperature of vacuum drum drying machine is
180 DEG C DEG C, dry 7h, mixed function master batch is added, mixed function master batch final mass score is 20%, total drying time
For 16h, water content then completes drying in 82ppm.
2）Melt spinning：Common PET material and mixed function master batch are sent into screw extruder heating melting after will be dry, molten
The mixture for melting state is pressurized to 45MPa by booster pump, after squeeze into Super-high pressure kettle, be pressurized in 1.7 hours in kettle
450Mpa was slowly decompressed to normal pressure state after pressurize 5 hours at 2-3 hours, was then distributed through manifold filtering and metering pump,
Again by spinneret spinneret at tow, the screw rod and manifold spin manifold temperature of the screw extruder are 292 DEG C, the spinneret
Panel aperture is 0.6mm, and the layout of hole count 6000, the spinneret is 20 circles；
The metering pump is 1985g/min, spinning speed 1245-1250m/min for amount.
3）It is cooled and shaped
Tow is molded by ring wind quenching, the ring blowing temperature is 18 DEG C, and the ring blowing speed is 8.5m/s.
4）Drawing-off
As-spun fibre after boundling is passed sequentially through into the first drafting machine, drawing-off bath, the second drafting machine, heater box and third drawing-off
Machine stretches, and total draft multiple is 1.7 times；
The first drafting machine speed is 28m/min, and the temperature of drawing-off bath is 85 DEG C, and the second drafting machine speed is 170m/
The temperature of min, heater box are 114 DEG C, and third drafting machine speed is 182m/min.
5）Thermal finalization
By the as-spun fibre after drawing-off after curling, oiling treatment, thermal finalization, the thermal finalization temperature are carried out by heat setting machine
Degree is 185 DEG C, and the heat-setting time is 17min.
6）Cut-out
Graphene polyester staple fiber finished product is made after cut-out.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 2, it is 6.5cN/dtex, extension at break to do fracture strength
Rate 7.3%, 3% corresponding stress of elongation are not less than 4.8 cN/dtex, and 200 DEG C of dry-hot shrinkages are less than 0.8%, and limit oxygen index is high
Up to 33%.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 2, chance high temperature melting shrinkage is low, in 600 DEG C of ignition point temperature
It spends collapsing rate in lower 20 minutes and is less than 2%.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 2, fiber regain are 13.5%, the conductivity of fiber
Up to 8.7 × 10-7S/cm。
3 a kind of graphene terylene fire resistance fibre of embodiment and preparation method thereof
Include the following steps：
（1）Prepare silica-graphene composite porous material
1）The graphene that grain size is 500 nanometers is pressed to the sodium metasilicate water of 10% addition a concentration of 40% to the dry silicic acid quality of production
In solution, sodium bicarbonate is added, is to slowly warm up to 60 DEG C of heat preservations, ultrasonic echography after being sufficiently stirred 2-3 hours in 70 minutes
2-3 hours, while stirring under 40 revs/min of rate, be slowly added to dilute sulfuric acid, adjust pH to 6, until no flocculent deposit with
Bubble generates.
The flocculent deposit is siliceous colloid, mainly the mixture of silicic acid, two silicic acid, orthosilicic acid, metasilicic acid.
The sodium bicarbonate, quality are the 1.7% of sodium metasilicate quality.
2）Using the filter cloth tissue of+9000 mesh flannelette of+8000 mesh silk of+6000 mesh stainless steel filtering net of 5000 mesh flannelette（On
The arrangement for stating filter cloth is from outside to inside）Sheet frame filter filtering, use intermittent pressure pump by frequency conversion rate for 0.20Mpa/10
The rate boost or depressurization of second, maintains 0.8Mpa, is dehydrated 40 minutes after obtaining silicic acid gel substance, and rotating speed is 800 revs/min.
3）By dewatered graphene-silica-gel mixture, after 3 hours dry at 100 DEG C, temperature is increased extremely in 30 minutes
160 DEG C, it to grain size after weight free of losses, is obtained after crushing is 3.5 microns that soaking time, which is 5 hours, and porosity is 70%, aperture
In 1000 nanometers of silica-graphene composite porous material A.
（2）Prepare graphene dispersion suspension
It is 400 nanometers of graphene dispersion in NMP carriers by grain size, high-speed stirred 3 hours, it is 25% to be made into graphene content
Favorable dispersibility graphene dispersion suspension B.
（3）Prepare mixed function master batch
By step（1）The silica of gained-graphene composite porous material A and step（2）The graphene dispersion of gained is suspended
Mixing in mixer is added in liquid B, PET material, auxiliary agent ethylene bis stearic acid amide and calcium stearate, through double-screw extruding pelletizing and returns
After receiving solvent NMP, mixed function master batch is obtained.
The auxiliary agent is ethylene bis stearic acid amide and calcium stearate, ratio 3:2, adding proportion is that PET expects drying
The 4% of weight.
The silica-graphene composite porous material, expect dry weight for PET 35%；
Graphene powder in the graphene dispersion suspension, expect dry weight for PET 15%.
（4）Spinning
1）Vacuum drum is dried：First by common PET material vacuum drum drying machine, the drying temperature of vacuum drum drying machine is
185 DEG C, dry 7.5h, mixed function master batch is added, mixed function master batch final mass score is 25%, and total drying time is
18h, water content then complete drying in 90ppm.
2）Melt spinning：Common PET material and mixed function master batch are sent into screw extruder heating melting after will be dry, molten
The mixture for melting state is pressurized to 50MPa by booster pump, after squeeze into Super-high pressure kettle, be pressurized in 1-2 hours in kettle
500Mpa was slowly decompressed to normal pressure state after pressurize 6 hours at 2-3 hours, was then distributed through manifold filtering and metering pump,
Again by spinneret spinneret at tow, the screw rod and manifold spin manifold temperature of the screw extruder are 295 DEG C, the spinneret
Panel aperture is 0.6mm, and the layout of hole count 6000, the spinneret is 20 circles,
The metering pump is 2000g/min, spinning speed 1280m/min for amount.
3）It is cooled and shaped
Tow is molded by ring wind quenching, the ring blowing temperature is 18 DEG C, and the ring blowing speed is 10.0m/s.
4）Drawing-off
As-spun fibre after boundling is passed sequentially through into the first drafting machine, drawing-off bath, the second drafting machine, heater box and third drawing-off
Machine stretches, and total draft multiple is 1.8 times；
The first drafting machine speed is 60m/min, and the temperature of drawing-off bath is 90 DEG C, and the second drafting machine speed is 180m/
The temperature of min, heater box are 118 DEG C, and third drafting machine speed is 195m/min.
5）Thermal finalization
By the as-spun fibre after drawing-off after curling, oiling treatment, thermal finalization, the thermal finalization temperature are carried out by heat setting machine
Degree is 185 DEG C, and the heat-setting time is 20min.
6）Cut-out
Graphene polyester staple fiber finished product is made after cut-out.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 3, it is 6.2cN/dtex, extension at break to do fracture strength
Rate 6.5%, 3% corresponding stress of elongation are not less than 4.8 cN/dtex, and 200 DEG C of dry-hot shrinkages are less than 1.1%, and limit oxygen index is high
Up to 32%.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 3, chance high temperature melting shrinkage is low, in 500 DEG C of ignition point temperature
It spends collapsing rate in lower 20 minutes and is less than 3%.
Graphene terylene fire resistance fibre prepared by the embodiment of the present invention 3, fiber regain are 12.6%, the conductivity of fiber
Up to 8.3 × 10-7S/cm。
Fiber prepared by the present invention is used primarily in carpet, filler, ornament materials etc..
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
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.
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 terylene fire resistance fibre, it is characterised in that：The fiber, graphene content are 1.5-3.5%, do fracture
Intensity is 6.1-6.5cN/dtex, limit oxygen index 31-33%.
2. a kind of graphene terylene fire resistance fibre according to claim 1, it is characterised in that：The fiber, in 500-600
Under DEG C ignition temperature, the collapsing rate in 20 minutes is less than 2-3%.
3. a kind of preparation method of graphene terylene fire resistance fibre, it is characterised in that：The preparation method, including prepare titanium dioxide
Silicon-graphene composite porous material prepares graphene dispersion suspension, prepares mixed function master batch, melt spinning, is cooled to
Type, drawing-off.
4. a kind of preparation method of graphene terylene fire resistance fibre according to claim 3, it is characterised in that：The preparation
Silica-graphene composite porous material, includes the following steps：
The graphene that grain size is 300-500 nanometers is added a concentration of 30-40%'s by the 6-10% to the dry silicic acid quality of production
In sodium silicate aqueous solution, sodium bicarbonate is added, is to slowly warm up to 50-60 DEG C of guarantor after being sufficiently stirred 2-3 hours in 50-70 minutes
Temperature, ultrasonic echography 2-3 hours while stirring under 30-40 revs/min of rate, are slowly added to dilute sulfuric acid, adjust pH to 5-
6, up to no flocculent deposit and bubble generate；Graphene silicic acid gel substance is obtained after filtering, after dehydration, drying, at 20-30 points
Temperature is increased in clock to 150-160 DEG C, soaking time is after 4-5 hours to weight free of losses, and it is 3-3.5 that grain size is obtained after crushing
Micron, porosity is in 60-70%, silica-graphene composite porous material of the aperture at 600 nanometers -1000 nanometers.
5. a kind of preparation method of graphene terylene fire resistance fibre according to claim 3, it is characterised in that：The preparation
Grain size is 200-400 nanometers of graphene dispersion in NMP carriers by graphene dispersion suspension, high-speed stirred 2-3 hours,
It is made into the graphene dispersion suspension that graphene content is 20-25%.
6. a kind of preparation method of graphene terylene fire resistance fibre according to claim 3, it is characterised in that：The preparation
Silica-graphene composite porous material is expected with the PET after graphene dispersion suspension, drying, is helped by mixed function master batch
Mixing in mixer is added with calcium stearate in agent ethylene bis stearic acid amide, and extruding pelletization simultaneously after recycling design NMP, is mixed
Functional agglomerate.
7. a kind of preparation method of graphene terylene fire resistance fibre according to claim 6, it is characterised in that：Described helps
Agent is ethylene bis stearic acid amide and calcium stearate, ratio 3:2, adding proportion is the 3-4% that PET expects dry weight；
The silica-graphene composite porous material expects the 30-35% of dry weight for PET；
Graphene powder in the graphene dispersion suspension expects the 10-15% of dry weight for PET.
8. a kind of preparation method of graphene terylene fire resistance fibre according to claim 3, it is characterised in that：The melting
Common PET material after drying and mixed function master batch are sent into screw extruder heating melting, the mixture warp of molten condition by spinning
Cross booster pump and be pressurized to 30-50MPa, after squeeze into Super-high pressure kettle, 300-500Mpa, pressurize 4-6 are pressurized in 1-2 hours in kettle
After hour, slowly normal pressure state was decompressed at 2-3 hour, then through manifold filter with metering pump distribution, then spinneret is at tow,
Spinning speed is 1200-1300m/min；
The mixed function master batch account for it is dry after the mass fraction of the sum of common PET material and mixed function master batch be 15%-25%.
9. a kind of preparation method of graphene terylene fire resistance fibre according to claim 3, it is characterised in that：The cooling
Molding, tow is molded by ring wind quenching, and the ring blowing temperature is 16 DEG C -19 DEG C, and the ring blowing speed is 8.0m/s-
10.0m/s。
10. a kind of preparation method of graphene terylene fire resistance fibre according to claim 3, it is characterised in that：It is described to lead
It stretches, total draft multiple is 1.4-1.8 times；First drafting machine speed is 50m/min-60m/min, and the temperature of drawing-off bath is
80 DEG C -90 DEG C, the second drafting machine speed is 135m/min-185m/min, and the temperature of heater box is 110 DEG C -120 DEG C, and third is led
It is 165m/min-195m/min to stretch machine speed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810040880.3A CN108277548B (en) | 2018-01-16 | 2018-01-16 | Graphene polyester flame-retardant fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810040880.3A CN108277548B (en) | 2018-01-16 | 2018-01-16 | Graphene polyester flame-retardant fiber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108277548A true CN108277548A (en) | 2018-07-13 |
| CN108277548B CN108277548B (en) | 2020-08-11 |
Family
ID=62803717
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810040880.3A Active CN108277548B (en) | 2018-01-16 | 2018-01-16 | Graphene polyester flame-retardant fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108277548B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110565200A (en) * | 2019-09-16 | 2019-12-13 | 浙江尤夫科技工业有限公司 | Flame-retardant polyester industrial yarn and preparation method thereof |
| CN111349983A (en) * | 2018-12-20 | 2020-06-30 | 大连道源新材料科技有限公司 | Flame-retardant fabric, high-temperature-resistant layer cloth and preparation method thereof |
| CN113718366A (en) * | 2021-09-18 | 2021-11-30 | 南通强生石墨烯科技有限公司 | Graphene super-strong flame-retardant fiber and preparation method thereof |
| CN116716678A (en) * | 2023-06-19 | 2023-09-08 | 石家庄市神鹿经编有限公司 | Flame-retardant polyester and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105177753A (en) * | 2015-10-21 | 2015-12-23 | 东华大学 | Preparation method of military anti-dripping anti-static high-tenacity flame-retardant polyester |
| CN105200547A (en) * | 2015-10-19 | 2015-12-30 | 沙嫣 | Preparation method of graphene-polyester nano-composite fiber |
| CN106811819A (en) * | 2016-04-01 | 2017-06-09 | 青岛大学 | A kind of preparation method of anti-molten droplet fiber |
| CN106807250A (en) * | 2017-01-19 | 2017-06-09 | 青岛大学 | A kind of preparation method of graphene oxide/silica/high molecular polymer composite nanometer filtering film |
| CN106810830A (en) * | 2016-04-01 | 2017-06-09 | 青岛大学 | A kind of fire-retardant anti-molten droplet master batch and preparation method thereof |
| 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 |
-
2018
- 2018-01-16 CN CN201810040880.3A patent/CN108277548B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200547A (en) * | 2015-10-19 | 2015-12-30 | 沙嫣 | Preparation method of graphene-polyester nano-composite fiber |
| CN105177753A (en) * | 2015-10-21 | 2015-12-23 | 东华大学 | Preparation method of military anti-dripping anti-static high-tenacity flame-retardant polyester |
| CN106811819A (en) * | 2016-04-01 | 2017-06-09 | 青岛大学 | A kind of preparation method of anti-molten droplet fiber |
| CN106810830A (en) * | 2016-04-01 | 2017-06-09 | 青岛大学 | A kind of fire-retardant anti-molten droplet master batch and preparation method thereof |
| CN106807250A (en) * | 2017-01-19 | 2017-06-09 | 青岛大学 | A kind of preparation method of graphene oxide/silica/high molecular polymer composite nanometer filtering film |
| 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 (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349983A (en) * | 2018-12-20 | 2020-06-30 | 大连道源新材料科技有限公司 | Flame-retardant fabric, high-temperature-resistant layer cloth and preparation method thereof |
| CN110565200A (en) * | 2019-09-16 | 2019-12-13 | 浙江尤夫科技工业有限公司 | Flame-retardant polyester industrial yarn and preparation method thereof |
| CN110565200B (en) * | 2019-09-16 | 2022-03-25 | 浙江尤夫科技工业有限公司 | Flame-retardant polyester industrial yarn and preparation method thereof |
| CN113718366A (en) * | 2021-09-18 | 2021-11-30 | 南通强生石墨烯科技有限公司 | Graphene super-strong flame-retardant fiber and preparation method thereof |
| CN116716678A (en) * | 2023-06-19 | 2023-09-08 | 石家庄市神鹿经编有限公司 | Flame-retardant polyester and preparation method thereof |
| CN116716678B (en) * | 2023-06-19 | 2024-04-26 | 石家庄市神鹿经编有限公司 | Flame-retardant polyester and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108277548B (en) | 2020-08-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108277548A (en) | A kind of graphene terylene fire resistance fibre and preparation method thereof | |
| CN108149337A (en) | A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof | |
| WO2018014510A1 (en) | Method for preparing cellulose fibre | |
| CN106435830A (en) | High strength chitosan complex fiber and preparing method thereof | |
| CN104372443B (en) | A kind of manufacture method of uvioresistant chopped fiber | |
| CN107955984B (en) | Graphene grafted polysaccharide Lyocell fiber and preparation method thereof | |
| CN106835345B (en) | Nano-cellulose composite PVA material and preparation method and application thereof | |
| CN109505033A (en) | The preparation method of Cellulose nanocrystal enhancing alginic acid composite fibre | |
| CN107955988B (en) | Preparation method of viscose containing chitin | |
| CN108047661A (en) | A kind of graphene dacron master grain and preparation method thereof | |
| WO2022252955A1 (en) | Hydroxylated alginate fiber and preparation method therefor | |
| CN105177751A (en) | Colored anti-ultraviolet profiled fine denier polyester filament and preparation method thereof | |
| CN104389039A (en) | Method for producing temperature-regulating viscose fibers | |
| CN105400109A (en) | Modified polyvinylalcohol foamed plastic and preparation method thereof | |
| CN114108118A (en) | Lyocell fiber and preparation method thereof | |
| CN110760943B (en) | Preparation and application of fresh flower fiber filament for spinning | |
| CN105887236A (en) | Artificial wig fibers containing peacock feather and having heat accumulation effect | |
| CN105544284A (en) | Medical silk paper and preparation method thereof | |
| CN108624974B (en) | Preparation method of pearl fiber | |
| CN110453311A (en) | A kind of warming chitin fiber and preparation method thereof | |
| CN114516677B (en) | Non-woven fabric for water purification and preparation method thereof | |
| CN108048954B (en) | Method for directly preparing carrageenan fibers from red algae extract | |
| EP3369859A1 (en) | High performance natural silk fiber and preparation method thereof | |
| CN105951212A (en) | Airy artificial wig fiber containing peacock feather | |
| CN106381541B (en) | Preparation method of enteromorpha carbon nano-material regenerated cellulose blend fiber |
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 |
Effective date of registration: 20190212 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. |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200702 Address after: 200125, room 2, building 3601, 2088 Dongfang Road, Shanghai, Pudong New Area Applicant after: SHANGHAI PGS NANOTECH Co.,Ltd. Address before: Yuyao City, Zhejiang province 315400 Ningbo Zhongyi Ningbo ecological park Hing Rd No. 28 Applicant before: Yuyao Pajiso New Materials Technology Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |