CN108411400A - Graphene fiber and preparation method thereof - Google Patents
Graphene fiber and preparation method thereof Download PDFInfo
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- CN108411400A CN108411400A CN201810197194.7A CN201810197194A CN108411400A CN 108411400 A CN108411400 A CN 108411400A CN 201810197194 A CN201810197194 A CN 201810197194A CN 108411400 A CN108411400 A CN 108411400A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- Chemical Kinetics & Catalysis (AREA)
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- Textile Engineering (AREA)
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- Carbon And Carbon Compounds (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of preparation methods of graphene fiber, include the following steps:1) mixed-powder being made of graphene, graphene carbon and graphite grinding is made to the superfines of granularity≤0.2 micron;2) base-material is PP or at least one of PA or PET, 2% 49% of 50%~90% base-material and the superfines weight in step 1) in total weight are mixed, then the polymer spinning-aid agent that mass concentration is 1%~8% is added, it is melted after being sufficiently stirred 20 40min, melting temperature is 260 286 DEG C, obtains mixture;3) mixture is granulated by dual-screw pelletizer, forms graphene master batch;4) graphene master batch and remaining base-material slice are heated to 260 DEG C~286 DEG C, form it into melt, by melt through screw extruder, spinneret orifice is expressed to by metering pump, be allowed to be formed in thread shape intake air, it is condensed and form slice;5) slice in step 4) is bent by cooling and solidifying, drawing-off, forms graphene fiber.The graphene fiber that the present invention produces and the fabric fabric being thus process improve human body surface microcirculation in antibacterial, uvioresistant, emitting far-infrared, releasing negative oxygen ion, and many aspects such as strengthen immunity have significant health-care effect.
Description
Technical field
The present invention relates to graphene fiber production field, more particularly to a kind of graphene fiber and preparation method thereof.
Background technology
Carbon is a kind of nonmetalloid, is located at the second round IVA race of the periodic table of elements.Latin language is Carbonium, meaning
For " coal, charcoal ".Carbon can in chemistry self in conjunction with and form a large amount of compounds, on biology and commercial be important point
Son.Most of molecules all contain carbon in organism.Graphite is carbon a kind of important form, graphite present in nature
A kind of allotrope of elemental carbon, the periphery of each carbon atom links the other three carbon atom, and (arrangement mode is in cellular
Multiple hexagons) with Covalent bonding together, constitute covalent molecule.Since each carbon atom can release an electronics, those electricity
Son can move freely, and belong to electric conductor.Graphite is the most soft mineral of one of which, it widely used, including manufacture spraying
Material and lubricant.
Graphene carbon is one kind in graphite, and existing way is different with the carbon compound in nature, be by
Manually some chemically or physically by way of prepare a kind of carbon simple substance to be formed, had on two dimensional surface by the carbon atom of hydridization
Sequence arranges, it is considered to be the basic composition unit of each dimension carbon material.Unique structure imparts the excellent performance of graphene,
It is especially more prominent in electricity, optics, calorifics, mechanics etc..Graphene is current most thin material known in the world, monolithic
Layer graphene thickness is the material of current resistivity minimum in the world, resistivity ratio copper or silver are lower, only only there are about 0.335nm
10~6 Ω/cm.Graphene has superpower electronic conduction ability, electron mobility higher than carbon nanotube and monocrystalline silicon, is more than
15000cm2/Vs;There is graphene the mechanical property of superelevation, fracture strength 130Gpa, highest Young's modulus to reach 1TPa simultaneously,
Active force between its molecule is extremely strong, it is difficult to be dissolved in water and other organic solvents.A series of this excellent properties is it in material, device
The fields such as part provide wide application prospect.
The common preparation method of graphene:
Mechanical stripping method or micromechanics stripping method are a kind of simplest methods, i.e., directly by graphene platelet from larger
It is stripped down on crystal.
Epitaxy method-Epitaxial Growth method:Using rare metal ruthenium as growth substrate, the atomic structure of matrix is utilized
" kind " has gone out graphene.It allows C atoms to penetrate into ruthenium at 1150 DEG C first, is subsequently cooled to 850 DEG C, a large amount of carbon absorbed before
Atom will float to ruthenium surface, form the single layer of carbon atom " isolated island " of lens shape in entire stromal surface, " isolated island " is gradually long
Greatly, finally grow up to one layer of complete graphene.First layer coverage rate is up to after 80%, and the second layer starts to grow, the graphene of bottom
Preceding layer and matrix are nearly completely separated after being formed there are strong reciprocation, the second layer between matrix, only remaining light current
Coupling, has been made single-layer graphene thin slice in this way.
The direct stripping method of liquid and gas:The method is directly graphite or expanded graphite (EG) (generally by quickly rising
Temperature obtains Surface oxygen-containing groups removing to 1000 DEG C or more) it is added in certain organic solvent or water, by ultrasonic wave, heating
Or the effect of air-flow prepares certain density single-layer or multi-layer graphene.
Graphite oxide reduction method:It is that graphite flake is dispersed in strong oxidizing property mixed acid that graphite oxide reduction method, which prepares graphene,
In, then such as concentrated nitric acid and the concentrated sulfuric acid are added potassium permanganate or potassium chlorate are strong etc. oxidizing obtains graphite oxide (GO)
The hydrosol, graphene oxide is obtained using supersound process, and graphene is obtained finally by reduction.
Instantly, graphene material is merged with high molecular material and manufactured new graphene fiber is becoming one
The graphene functional fibre of the new trend of kind, unlike material and function constantly emerges in succession.Wherein, add in chemical fibre
Graphene fiber made of graphene material is entered, has had the health-care effect for the function of human body that increases significantly, and has been weighed
The verification of prestige testing department is approved by market and vast consumer gradually.
However current graphene fiber, fiber have a single function, health-care effect is poor, fiber functional performance unobvious, production
It is complicated for operation, it largely puts into production to it and brings certain difficulty.
Invention content
The technical problem to be solved in the present invention is to provide a kind of fiber is vdiverse in function, good health care effect, fiber functional performance
Apparent graphene fiber.
In order to solve the above-mentioned technical problem, the technical scheme is that:A kind of preparation method of graphene fiber, including
Following steps:
1) the ultra-fine of granularity≤0.2 micron is made in the mixed-powder being made of graphene, graphene carbon and graphite grinding
Powder;
2) by the 2%- of PP or PA or PET50%~90% and the superfines weight in step 1) in base-material total weight
Then 49% mixing is added the polymer spinning-aid agent that mass concentration is 1%~8%, is melted after being sufficiently stirred 20-40min, melted
Temperature is 260-286 DEG C;
3) mixture obtained in step 2) is granulated by dual-screw pelletizer, forms graphene master batch;
4) graphene master batch and remaining base-material slice are heated to 260 DEG C~286 DEG C, melt are formed it into, by melt
Through screw extruder, spinneret orifice is expressed to by metering pump, is allowed to be formed in thread shape intake air, it is condensed and form slice;
5) slice forms graphene fiber by cooling and solidifying, drawing-off bending.
In this preparation method, base-material is therefore applied widely regardless of whether drying, and simplifies workflow.
Preferably, the mixed-powder in step 1) is made of each component of following parts by weight:Graphene 0.05~50
Part, 0.5~20 part of graphene carbon, 0.05~10 part of graphite.
Preferably, the weight ratio of base-material slice and mixed-powder is 2-200:1.
Preferably, in step 2), the polymer spinning-aid agent dissolved by low boiling point organic solvent after again with base-material
Slice and superfines are sufficiently stirred.
Preferably, in the present invention, low boiling point organic solvent is acetone or alcohol.
Preferably, the polymer spinning-aid agent is titanate esters series or silane series:The titanate esters series packet
It includes:Three isostearic acid titanate esters of isopropyl or isopropyl stearyl-methylpropenyl titanate esters;The silane series
Including:R- coloured glaze base trimethoxy silanes or r- coloured glaze base trimethoxy silanes or r- glycidoxypropyl trimethoxy silanes, or
Bis- (r- triethoxy silicon substrates propyl) four coloured glazes.
The graphene purity is 99.99%.Electric conductivity is high.
The invention also discloses the graphene fibers made by above-mentioned preparation method.
Using above-mentioned technical proposal, since the present invention is the high purity graphite alkene material using a certain amount of natural graphite
Powder, the graphene fiber thus produced and the fabric fabric being thus process, antibacterial, uvioresistant,
Emitting far-infrared, releasing negative oxygen ion, improves human body surface microcirculation, and many aspects such as strengthen immunity have significant protect
Strong effect.Far infrared transmissivity increases 90%, and the simple far-infrared fabric than being currently known increases 10%.
Unique texture possessed by graphene in graphene fiber can intensify ambient air, generate negative oxygen ion, clearly
New air;Graphene can intensify skin immune cells, reinforce the phagocytosis of reticuloendothelial cell, reach the antibacterial work(of anti-inflammatory
Energy.
And the preparation method of the graphene fiber in the present invention can be used for making various long filaments such as PP, polyamide fibre, PET, short
Fibrous materials, the preparation methods of common graphite alkene fiber such as silk are only used for doing filament fiber.
Specific implementation mode
In the present invention, polymer spinning-aid agent is commercially available, and in the present invention, graphene purity is 99.99%.
The specific implementation mode of the present invention is described further below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but does not constitute limitation of the invention.In addition, invention described below
Involved technical characteristic can be combined with each other as long as they do not conflict with each other in each embodiment.
Embodiment 1:
A kind of preparation method of graphene fiber, includes the following steps:
It 1) will be by each component of parts by weight:The mixed powder of 10 parts of 50 parts of graphene, 20 parts of graphene carbon and graphite compositions
The superfines of granularity≤0.2 micron is made in end grinding;
2) base-material is PP or at least one of PA or PET, by 50%~90% base-material and step 1) in total weight
In superfines weight 2%-49% mixing, base-material slice is 2-200 with the weight ratio of mixed-powder:1, then it is added
The polymer spinning-aid agent that mass concentration is 1%~8%, melts after being sufficiently stirred 20-40min, and melting temperature is 260-286 DEG C,
Obtain mixture;Wherein, it is filled again with base-material slice and superfines after polymer spinning-aid agent is dissolved by low boiling point organic solvent
Divide stirring;
3) mixture obtained in step 2) is granulated by dual-screw pelletizer, forms graphene master batch;
4) graphene master batch and remaining base-material slice are heated to 260 DEG C~286 DEG C, melt are formed it into, by melt
Through screw extruder, spinneret orifice is expressed to by metering pump, is allowed to be formed in thread shape intake air, it is condensed and form slice;
5) slice in step 4) is bent by cooling and solidifying, drawing-off, forms graphene fiber.
In the present invention, low boiling point organic solvent is acetone or alcohol.
Polymer spinning-aid agent is that titanate esters series includes:Three isostearic acid titanate esters of isopropyl or isopropyl stearoyl
Base-methylpropenyl titanate esters;The silane series includes:R- coloured glaze base trimethoxy silanes or r- coloured glaze base trimethoxy silicon
Alkane or r- glycidoxypropyls trimethoxy silane or bis- (r- triethoxy silicon substrates propyl) four coloured glazes.
Embodiment 2:
A kind of preparation method of graphene fiber, includes the following steps:
It 1) will be by each component of parts by weight:0.05 part of 0.05 part of graphene, 0.5 part of graphene carbon and graphite form mixed
Close the superfines that granularity≤0.2 micron is made in powder mull;
2) base-material is PP or at least one of PA or PET, by 50%~90% base-material and step 1) in total weight
In superfines weight 2%-49% mixing, base-material slice is 2-200 with the weight ratio of mixed-powder:1, then it is added
The polymer spinning-aid agent that mass concentration is 1%~8%, melts after being sufficiently stirred 20-40min, and melting temperature is 260-286 DEG C,
Obtain mixture;Wherein, it is filled again with base-material slice and superfines after polymer spinning-aid agent is dissolved by low boiling point organic solvent
Divide stirring;
3) mixture obtained in step 2) is granulated by dual-screw pelletizer, forms graphene master batch;
4) graphene master batch and remaining base-material slice are heated to 260 DEG C~286 DEG C, melt are formed it into, by melt
Through screw extruder, spinneret orifice is expressed to by metering pump, is allowed to be formed in thread shape intake air, it is condensed and form slice;
5) slice in step 4) is bent by cooling and solidifying, drawing-off, forms graphene fiber.
In the present invention, low boiling point organic solvent is acetone or alcohol.
Polymer spinning-aid agent is that titanate esters series includes:Three isostearic acid titanate esters of isopropyl or isopropyl stearoyl
Base-methylpropenyl titanate esters;The silane series includes:R- coloured glaze base trimethoxy silanes or r- coloured glaze base trimethoxy silicon
Alkane or r- glycidoxypropyls trimethoxy silane or bis- (r- triethoxy silicon substrates propyl) four coloured glazes.
Embodiment 3:
A kind of preparation method of graphene fiber, includes the following steps:
It 1) will be by each component of parts by weight:The mixed-powder of 5 parts of 20 parts of graphene, 10 parts of graphene carbon and graphite compositions
The superfines of granularity≤0.2 micron is made in grinding;
2) base-material is PP or at least one of PA or PET, by 50%~90% base-material and step 1) in total weight
In superfines weight 2%-49% mixing, base-material slice is 200 with the weight ratio of mixed-powder:1, matter is then added
The polymer spinning-aid agent for measuring a concentration of 1%~8%, melts after being sufficiently stirred 20-40min, and melting temperature is 286 DEG C, is mixed
Close object;Wherein, it is sufficiently stirred again with base-material slice and superfines after polymer spinning-aid agent is dissolved by low boiling point organic solvent;
3) mixture obtained in step 2) is granulated by dual-screw pelletizer, forms graphene master batch;
4) graphene master batch and remaining base-material slice are heated to 260 DEG C~286 DEG C, melt are formed it into, by melt
Through screw extruder, spinneret orifice is expressed to by metering pump, is allowed to be formed in thread shape intake air, it is condensed and form slice;
5) slice in step 4) is bent by cooling and solidifying, drawing-off, forms graphene fiber.
In the present invention, low boiling point organic solvent is acetone or alcohol.
Polymer spinning-aid agent is that titanate esters series includes:Three isostearic acid titanate esters of isopropyl or isopropyl stearoyl
Base-methylpropenyl titanate esters;The silane series includes:R- coloured glaze base trimethoxy silanes or r- coloured glaze base trimethoxy silicon
Alkane or r- glycidoxypropyls trimethoxy silane or bis- (r- triethoxy silicon substrates propyl) four coloured glazes.
The present invention is the high purity graphite alkene material powder using a certain amount of natural graphite, the graphite thus produced
Alkene fiber and the fabric fabric being thus process bear oxygen in antibacterial, uvioresistant, emitting far-infrared, release
Ion, improves human body surface microcirculation, and many aspects such as strengthen immunity have significant health-care effect.Far infrared transmissivity increases
It is added to 90%, the simple far-infrared fabric than being currently known increases 10%.
Claims (8)
1. a kind of preparation method of graphene fiber, it is characterised in that:Include the following steps:
1) mixed-powder being made of graphene, graphene carbon and graphite grinding is made to the superfines of granularity≤0.2 micron;
2) base-material is PP or at least one of PA or PET, will 50%~90% base-material in total weight in step 1)
The 2%-49% of superfines weight is mixed, and the polymer spinning-aid agent that mass concentration is 1%~8% is then added, is sufficiently stirred
It is melted after 20-40min, melting temperature is 260-286 DEG C, obtains mixture;
3) mixture obtained in step 2) is granulated by dual-screw pelletizer, forms graphene master batch;
4) graphene master batch and remaining base-material slice are heated to 260 DEG C~286 DEG C, melt are formed it into, by melt through spiral shell
Bar extruder is expressed to spinneret orifice by metering pump, is allowed to be formed in thread shape intake air, condensed and form slice;
5) slice in step 4) is bent by cooling and solidifying, drawing-off, forms graphene fiber.
2. the preparation method of graphene fiber as described in claim 1, it is characterised in that:Mixed-powder in step 1) is ultra-fine
Powder is made of each component of following parts by weight:0.05~50 part of graphene, 0.5~20 part of graphene carbon, graphite 0.05~
10 parts.
3. the preparation method of graphene fiber as claimed in claim 2, it is characterised in that:Base-material is sliced the weight with mixed-powder
Amount ratio is 2-200:1.
4. the preparation method of graphene fiber as described in claim 1, it is characterised in that:In step 2), the polymer
Spinning-aid agent is sufficiently stirred with base-material slice and superfines again after being dissolved by low boiling point organic solvent.
5. the preparation method of graphene fiber as claimed in claim 4, it is characterised in that:The low boiling point organic solvent is
Acetone or alcohol.
6. the preparation method of graphene fiber as described in claim 4 or 5, it is characterised in that:The polymer spinning-aid agent
For titanate esters series or silane series:The titanate esters series includes:Three isostearic acid titanate esters of isopropyl or isopropyl
Stearyl-methylpropenyl titanate esters;The silane series includes:R- coloured glaze base trimethoxy silanes or r- coloured glaze base front threes
Oxysilane or r- glycidoxypropyls trimethoxy silane or bis- (r- triethoxy silicon substrates propyl) four coloured glazes.
7. the preparation method of graphene fiber as claimed in claim 6, it is characterised in that:The graphene purity is
99.99%.
8. the graphene fiber made by a kind of preparation method as described in claim 1-7.
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CN110195266A (en) * | 2019-06-17 | 2019-09-03 | 扬州市维纳复合材料科技有限公司 | A kind of production method of functional fibre |
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CN112301454A (en) * | 2020-10-22 | 2021-02-02 | 山东理工大学 | Preparation method of PET-based graphene conductive fibers |
CN113235181A (en) * | 2021-06-03 | 2021-08-10 | 张敏洁 | Preparation method of soybean graphene fibers |
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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 |
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CN113897699A (en) * | 2021-10-25 | 2022-01-07 | 南通强生石墨烯科技有限公司 | Graphene uvioresistant regenerated fiber and preparation method thereof |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110195266A (en) * | 2019-06-17 | 2019-09-03 | 扬州市维纳复合材料科技有限公司 | A kind of production method of functional fibre |
CN110195266B (en) * | 2019-06-17 | 2021-08-17 | 扬州市维纳复合材料科技有限公司 | Production method of functional fiber |
US11162273B2 (en) * | 2019-08-01 | 2021-11-02 | Markus Hutnak | Outdoor equipment |
CN111778581A (en) * | 2020-06-17 | 2020-10-16 | 安徽三宝棉纺针织投资有限公司 | Far infrared heating and weather-resistant graphene polyamide yarn and preparation process thereof |
CN111778581B (en) * | 2020-06-17 | 2022-10-11 | 安徽三宝棉纺针织投资有限公司 | Far infrared heating and weather-resistant graphene nylon yarn and preparation process thereof |
CN112301454A (en) * | 2020-10-22 | 2021-02-02 | 山东理工大学 | Preparation method of PET-based graphene conductive fibers |
CN113235181A (en) * | 2021-06-03 | 2021-08-10 | 张敏洁 | Preparation method of soybean graphene fibers |
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 |
CN113897699A (en) * | 2021-10-25 | 2022-01-07 | 南通强生石墨烯科技有限公司 | Graphene uvioresistant regenerated fiber and preparation method thereof |
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