CN106498537A - The preparation method of Graphene nylon fibre - Google Patents
The preparation method of Graphene nylon fibre Download PDFInfo
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- CN106498537A CN106498537A CN201610888499.3A CN201610888499A CN106498537A CN 106498537 A CN106498537 A CN 106498537A CN 201610888499 A CN201610888499 A CN 201610888499A CN 106498537 A CN106498537 A CN 106498537A
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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
-
- 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
-
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of preparation method of Graphene nylon fibre, comprises the steps:(1) Graphene inserted sheet dispersion slurries are prepared:First in the deionized water by graphene dispersion in container, the concentration of Graphene is 10%wt;Add surface conditioning agent again, grind in the presence of mill is situated between, stand 4 hours, the slurries for then taking out top half in container disperse slurries as Graphene inserted sheet;(2) pump in the synthesis reaction vessel for include caprolactam after Graphene inserted sheet being disperseed screen cloth of the slurries through 5 microns and reacted, the Graphene slices of caprone of 0.5 3%wt of graphene-containing is obtained;(3), after be well mixed Graphene slices of caprone and dried by preset ratio with slices of caprone, Graphene nylon fibre, 0.5 3%wt of graphene-containing wherein in Graphene nylon fibre are obtained by drawing process.Obtained in of the invention, Graphene nylon fibre proterties uniformity is good, and common nylon fibre can be made to become the nylon fibre with conduction, anti-electromagnetic wave, antistatic and high-efficiency shielding far infrared characterization.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene nylon fibre.
Background technology
Graphene is the most guiding and strategic new industry in the world today, has huge development potentiality and market
Vigor.China is one of current Graphene research and application and development country the most active, and Graphene amount of the application for patent occupies the world
Leading position, and a series of Graphene application novel products are have developed in the field such as semiconductor and lithium ion battery.
Graphene is the most thin and most hard nano material for finding in the world so far, but its engineer applied is necessary
Carrier to be had.Graphene is used in the preparation of film at present, and the film that with the addition of Graphene can be used on research and development new forms of energy battery,
Can solve the problems, such as that new energy car battery off-capacity and charging interval are long;If Graphene is painted on display screen table
Face, it is possible to develop transparent flexible display screen;If it is added in coating, then this coating is not only without first
Aldehyde, moreover it is possible to adsorb the formaldehyde in air with purify air.
But at present, Graphene is added to also highly difficult in nylon fibre, although be no lack of the trial of this respect, but obtained
Homogeneity of product is poor, and the improvement to nylon fibre performance is very limited, and preparation cost is high, in the urgent need to a kind of economical and efficient
Graphene nylon fibre preparation method.
Content of the invention
The purpose of the present invention is that homogeneity of product obtained in the current Graphene nylon fibre preparation method of solution is poor, right
The improvement of nylon fibre performance is very limited, and the high technical problem of preparation cost.
In order to solve above-mentioned technical problem, the present invention provides a kind of preparation method of Graphene nylon fibre, including as follows
Step:
(1) Graphene inserted sheet dispersion slurries are prepared:The Graphene of particle diameter≤0.5 μm is first placed in the Ball-stirring mill of vertical grinding
In, deionized water is added, the concentration of Graphene is 10%wt;Add surface conditioning agent again, 2-4 is ground in the presence of mill is situated between little
Shi Hou, after adding surface conditioning agent continuation grinding 1 hour, obtains Graphene slurries, the Graphene slurries is put into container
Interior standing 4 hours, the slurries for then taking out top half in container disperse slurries as Graphene inserted sheet;
(2) Graphene slices of caprone is prepared:In pumping into after the Graphene inserted sheet is disperseed screen cloth of the slurries through 5 microns
Synthetic reaction is carried out in synthesis reaction vessel containing caprolactam, the Graphene slices of caprone of graphene-containing 0.5-3%wt is obtained;
(3) Graphene nylon fibre is prepared:The Graphene slices of caprone is mixed by preset ratio with slices of caprone
After even and dry, Graphene nylon fibre, wherein graphene-containing 0.5-3% in Graphene nylon fibre are obtained by drawing process
wt.
Further, surface conditioning agent described in step (1) is low-carbon (LC) polyhydroxy-alcohol, Long carbon chain unit alcohol, Long carbon chain list
First acid, low-carbon (LC) polyhydroxy-acid, organic amine surfactant, esters surface active agent, nonionic surfactant, hydroxyl
High molecular polymer and its esters and carboxylic high molecular polymer and the one kind in its esters, or more than two of which mixed
Compound.
Further, the low-carbon (LC) polyhydroxy-alcohol is in glycerine, pentaerythrite, BDO and Shan Li sugar alcohols
Kind, or mixture more than two of which.
Further, the Long carbon chain unit alcohol is the one kind in octadecyl alcolol and laruyl alcohol, or is octadecyl alcolol and laruyl alcohol
Mixture;
The sour one kind in myristic acid, azelaic acid and laurate of the Long carbon chain unit, or mixing more than two of which
Thing.
Further, the low-carbon (LC) polyhydroxy-acid is the one kind in citric acid, tartaric acid or P-hydroxybenzoic acid, or wherein
Two or more mixtures.
Further, the organic amine surfactant is the one kind in N- isopropyl alcohols amine and triethanolamine, or
N- isopropyl alcohols amine and the mixture of triethanolamine;
The esters surface active agent is the one kind in dibutyl phthalate and dioctyl phthalate, or adjacent benzene
Dibutyl carboxylic acid and the mixture of dioctyl phthalate.
Further, the nonionic surfactant is this one kind in 20 of polysorbas20, polysorbate40 or department, or wherein
Two or more mixtures.
Further, the high molecular polymer and its esters of the hydroxyl be polyethylene glycol 1500, Macrogol 4000,
One kind in PMA, butyl polyacrylate and Sodium Polyacrylate, or mixture more than two of which;
The carboxylic high molecular polymer and its esters are polyethylene glycol 1500, Macrogol 4000, polyacrylic acid
One kind in methyl esters, butyl polyacrylate and Sodium Polyacrylate, or mixture more than two of which.
Further, inorganic abrading-ball of mill Jie described in step (1) for diameter 0.5-5 millimeters, the material of the inorganic abrading-ball
Matter is inorganic quartz, zirconium or aluminum oxide.
Further, the speed that grinds described in step (1) is 200-350 rev/min.
Good using Graphene nylon fibre proterties uniformity obtained in the present invention, become can common nylon fibre and have
The nylon fibre of conduction, anti-electromagnetic wave, antistatic and high-efficiency shielding far infrared characterization, substantially improves the thing of common nylon fibre
Reason and chemical property, so as to widen use range, can be widely used for the field of textiles such as wearable product.
Specific embodiment
Presently in connection with embodiment, the present invention is further detailed explanation, and application of the invention is not limited to following
Embodiment, falls within protection scope of the present invention to any pro forma accommodation done by the present invention.
The preparation method of the Graphene nylon fibre of the present invention, comprises the steps:
(1) Graphene inserted sheet dispersion slurries are prepared:The Graphene of particle diameter≤0.5 μm is first placed in the Ball-stirring mill of vertical grinding
In, deionized water is added, the concentration of Graphene is 10%wt;Add surface conditioning agent again, 2-4 is ground in the presence of mill is situated between little
Shi Hou, after adding surface conditioning agent continuation grinding 1 hour, obtains Graphene slurries, the Graphene slurries is put into container
Interior standing 4 hours, the slurries for then taking out top half in container disperse slurries as Graphene inserted sheet;
Specifically, although Graphene lamellar spacing is in nanoscale, it is micron order on XY directions.Reason from ultra-fine grain
By setting out, this lamella particle easily mutually adsorbs between the layers, is easily formed in the course of the polymerization process and is reunited, is caused in fiber
Middle affect fiber intensity, institute for the present invention Graphene needs carry out decentralized processing by following technique, as further
The raw material of super-fine processing:
100 grams of graphene powder is placed in the Ball-stirring mill of vertical grinding, add 400 ml deionized waters, add
0.2-1.0 gram of surface conditioning agent, is the ball milling made of aluminum oxide 4 hours of 0.5-5mm by sphere diameter, adds 0.1
After gram surface conditioning agent continues grinding 1 hour, Graphene slurries are obtained;Mechanical dispersion of this process by means of grinding so that stone
Fully infiltrate between black alkene layer and layer surface, so as to no longer mutually adsorb, form the slurries containing Graphene;
Above-mentioned Graphene slurries are placed in 500 milliliters of glass dish, 4 hours are stood, is taken slurries top half, as
The Graphene inserted sheet dispersion slurries that can directly use;
(2) Graphene slices of caprone is prepared:Pump into after Graphene inserted sheet is disperseed screen cloth of the slurries through 5 microns and include 2-
Synthetic reaction is carried out in the synthesis reaction vessel of 5kg caprolactams, and the Graphene slices of caprone of graphene-containing 0.5-3%wt is obtained;
(3) Graphene nylon fibre is prepared:Graphene slices of caprone is well mixed simultaneously by preset ratio with slices of caprone
After drying, Graphene nylon fibre, wherein graphene-containing 0.5-3%wt in Graphene nylon fibre are obtained by drawing process;
Such as, the product such as fine-denier (≤1.5 denier) or middle denier (more than 1.5 denier) can be processed into.
Preferably, in step (1), surface conditioning agent is that low-carbon (LC) polyhydroxy-alcohol, Long carbon chain unit alcohol, Long carbon chain unit are sour, low
Carbon polyhydroxy-acid, organic amine surfactant, esters surface active agent, nonionic surfactant, the macromolecule of hydroxyl
Polymer and its esters and carboxylic high molecular polymer and the one kind in its esters, or mixture more than two of which.
Preferably, low-carbon (LC) polyhydroxy-alcohol is the one kind in glycerine, pentaerythrite, BDO and Shan Li sugar alcohols, or its
In two or more mixture.
Preferably, Long carbon chain unit alcohol is the one kind in octadecyl alcolol and laruyl alcohol, or the mixing for octadecyl alcolol and laruyl alcohol
Thing;
The sour one kind in myristic acid, azelaic acid and laurate of Long carbon chain unit, or mixture more than two of which.
Preferably, low-carbon (LC) polyhydroxy-acid be citric acid, tartaric acid or P-hydroxybenzoic acid in one kind, or two of which with
On mixture.
Preferably, organic amine surfactant is the one kind in N- isopropyl alcohols amine and triethanolamine, or N- isopropyls
Ethylethanolamine and the mixture of triethanolamine;
Esters surface active agent is the one kind in dibutyl phthalate and dioctyl phthalate, or O-phthalic
Dibutyl phthalate and the mixture of dioctyl phthalate.
Preferably, nonionic surfactant is this one kind in 20 of polysorbas20, polysorbate40 or department, or two of which with
On mixture.
Preferably, the high molecular polymer and its esters of hydroxyl is polyethylene glycol 1500, Macrogol 4000, polypropylene
One kind in sour methyl esters, butyl polyacrylate and Sodium Polyacrylate, or mixture more than two of which;
Carboxylic high molecular polymer and its esters be polyethylene glycol 1500, Macrogol 4000, PMA,
One kind in butyl polyacrylate and Sodium Polyacrylate, or mixture more than two of which.
Preferably, inorganic abrading-ball of mill Jie in step (1) for diameter 0.5-5 millimeters, the material of inorganic abrading-ball is inorganic
Quartz, zirconium or aluminum oxide.
Preferably, in step (1), the speed of grinding is 200-350 rev/min.
In addition, obtained Graphene inserted sheet dispersion slurries can also be added directly in fibrous raw material slurries, such as in step (1)
The synthesising fibre raw slurry such as viscose glue, acrylic fibers, or other raw slurries, by decentralized processing, then by the slurry of graphene-containing
Routinely technique is processed into Graphene viscose rayon or Graphene acrylic fiber, wherein Graphene for wire drawing workshop section of the liquid in chemical fibre factory
Addition preferably control in the range of 0.5~0.3%wt (in terms of contained synthetic fiber material dry weight in slurries);
For the slurry of fibre stuff or other fibers with semi-synthetic property, including made with soybean protein half
The slurry of synthesising property, after equally can adding Graphene and be disperseed according to above-mentioned addition manner, can be added by original technique
Work is into fiber product.
In a word, other equivalents such as every fibrous raw material being processed in the way of slurry, as long as add this wherein
What the Graphene inserted sheet dispersion slurries of invention were further synthesized is regarded as protection scope of the present invention.
With the above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete
Various change and modification can be carried out entirely in the range of without departing from this invention technological thought.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determine its technical scope according to right.
Claims (10)
1. the preparation method of Graphene nylon fibre, it is characterised in that comprise the steps:
(1) Graphene inserted sheet dispersion slurries are prepared:First the Graphene of particle diameter≤0.5 μm is placed in the Ball-stirring mill of vertical grinding,
Deionized water is added, the concentration of Graphene is 10%wt;Add surface conditioning agent again, in the presence of mill is situated between, grinds 2-4 hours
Afterwards, after adding surface conditioning agent continuation grinding 1 hour, Graphene slurries are obtained, the Graphene slurries is put in container
4 hours are stood, the slurries for then taking out top half in container disperse slurries as Graphene inserted sheet;
(2) Graphene slices of caprone is prepared:Pump into after the Graphene inserted sheet is disperseed screen cloth of the slurries through 5 microns and include oneself
Synthetic reaction is carried out in the synthesis reaction vessel of lactams, and the Graphene slices of caprone of graphene-containing 0.5-3%wt is obtained;
(3) Graphene nylon fibre is prepared:The Graphene slices of caprone is well mixed simultaneously by preset ratio with slices of caprone
After drying, Graphene nylon fibre, wherein graphene-containing 0.5-3%wt in Graphene nylon fibre are obtained by drawing process.
2. the preparation method of Graphene nylon fibre according to claim 1, it is characterised in that table described in step (1)
Face inorganic agent is low-carbon (LC) polyhydroxy-alcohol, Long carbon chain unit alcohol, the acid of Long carbon chain unit, low-carbon (LC) polyhydroxy-acid, the work of organic amine surface
Property agent, esters surface active agent, nonionic surfactant, the high molecular polymer of hydroxyl and its esters and carboxylic height
One kind in Molecularly Imprinted Polymer and its esters, or mixture more than two of which.
3. the preparation method of Graphene nylon fibre according to claim 2, it is characterised in that the low-carbon (LC) polyhydroxy-alcohol
For the one kind in glycerine, pentaerythrite, BDO and Shan Li sugar alcohols, or mixture more than two of which.
4. the preparation method of Graphene nylon fibre according to claim 3, it is characterised in that the Long carbon chain unit alcohol
One kind in for octadecyl alcolol and laruyl alcohol, or the mixture for octadecyl alcolol and laruyl alcohol;
The sour one kind in myristic acid, azelaic acid and laurate of the Long carbon chain unit, or mixture more than two of which.
5. the preparation method of Graphene nylon fibre according to claim 4, it is characterised in that the low-carbon (LC) polyhydroxy-acid
For the one kind in citric acid, tartaric acid or P-hydroxybenzoic acid, or mixture more than two of which.
6. the preparation method of Graphene nylon fibre according to claim 5, it is characterised in that the organic amine surface
Activating agent is the one kind in N- isopropyl alcohols amine and triethanolamine, or the mixture of N- isopropyl alcohols amine and triethanolamine;
The esters surface active agent is the one kind in dibutyl phthalate and dioctyl phthalate, or O-phthalic
Dibutyl phthalate and the mixture of dioctyl phthalate.
7. the preparation method of Graphene nylon fibre according to claim 6, it is characterised in that the non-ionic surface is lived
Property agent be this one kind in 20 of polysorbas20, polysorbate40 or department, or mixture more than two of which.
8. the preparation method of Graphene nylon fibre according to claim 7, it is characterised in that the high score of the hydroxyl
Sub- polymer and its esters are polyethylene glycol 1500, Macrogol 4000, PMA, butyl polyacrylate and polypropylene
One kind in sour sodium, or mixture more than two of which;
The carboxylic high molecular polymer and its esters be polyethylene glycol 1500, Macrogol 4000, PMA,
One kind in butyl polyacrylate and Sodium Polyacrylate, or mixture more than two of which.
9. the preparation method of Graphene nylon fibre according to claim 1, it is characterised in that grind described in step (1)
The inorganic abrading-ball being situated between for diameter 0.5-5 millimeters, the material of the inorganic abrading-ball is inorganic quartz, zirconium or aluminum oxide.
10. the preparation method of Graphene nylon fibre according to claim 1, it is characterised in that step is ground described in (1)
The speed of mill is 200-350 rev/min.
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106995945A (en) * | 2017-05-11 | 2017-08-01 | 广州江鼎电子科技有限公司 | A kind of preparation method of the good graphene conductive yarn of ductility |
CN107313126A (en) * | 2017-06-30 | 2017-11-03 | 福建锦江科技有限公司 | A kind of method that the fiber of graphene modified nylon 6 is produced by high speed spinning |
CN107353419A (en) * | 2017-08-21 | 2017-11-17 | 郑行良 | A kind of preparation method of graphene chinlon master batch and fiber |
CN107739468A (en) * | 2017-06-13 | 2018-02-27 | 绍兴标点纺织科技有限公司 | A kind of compound PP fibers of graphene and preparation method |
CN108070936A (en) * | 2017-12-06 | 2018-05-25 | 三橡股份有限公司 | A kind of Train brake hose nylon fibre, preparation method and the usage |
CN108727808A (en) * | 2017-04-21 | 2018-11-02 | 山东圣泉新材料股份有限公司 | - 6 agglomerate material of polyamide, the fiber and purposes comprising it of graphene modification |
CN108968175A (en) * | 2018-09-13 | 2018-12-11 | 江苏红豆实业股份有限公司 | Graphene antistatic sweater |
CN109233191A (en) * | 2018-07-26 | 2019-01-18 | 苏州汉力新材料有限公司 | A kind of preparation method of phenolic resin compound insulating material |
CN109880169A (en) * | 2019-01-08 | 2019-06-14 | 常州兴烯石墨烯科技有限公司 | Modified white graphite alkene nylon compound slice of a kind of in-situ polymerization and preparation method thereof |
CN110453302A (en) * | 2019-04-19 | 2019-11-15 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene nylon fibre |
CN110699772A (en) * | 2019-11-21 | 2020-01-17 | 秦皇岛中科瀚祺科技有限公司 | Graphene/nylon fiber composite material and preparation method and application thereof |
CN115341294A (en) * | 2021-05-13 | 2022-11-15 | 中国石油化工股份有限公司 | Thermoplastic fiber and preparation method of co-woven reinforced composite material thereof |
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CN105463612A (en) * | 2015-12-17 | 2016-04-06 | 中国科学院重庆绿色智能技术研究院 | Graphene quantum dot reinforced polyarmide fiber and preparation method thereof |
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CN103215689A (en) * | 2013-05-09 | 2013-07-24 | 苏州大学 | Preparation method of graphene modified nylon 6 fiber |
CN104562276A (en) * | 2014-12-05 | 2015-04-29 | 淮安锦纶化纤有限公司 | Method for modifying chinlon 6 fibers and modified product |
CN105463612A (en) * | 2015-12-17 | 2016-04-06 | 中国科学院重庆绿色智能技术研究院 | Graphene quantum dot reinforced polyarmide fiber and preparation method thereof |
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CN106995945A (en) * | 2017-05-11 | 2017-08-01 | 广州江鼎电子科技有限公司 | A kind of preparation method of the good graphene conductive yarn of ductility |
CN107739468A (en) * | 2017-06-13 | 2018-02-27 | 绍兴标点纺织科技有限公司 | A kind of compound PP fibers of graphene and preparation method |
CN107313126B (en) * | 2017-06-30 | 2019-12-17 | 福建锦江科技有限公司 | Method for producing graphene modified polyamide-6 fiber through high-speed spinning |
CN107313126A (en) * | 2017-06-30 | 2017-11-03 | 福建锦江科技有限公司 | A kind of method that the fiber of graphene modified nylon 6 is produced by high speed spinning |
CN107353419A (en) * | 2017-08-21 | 2017-11-17 | 郑行良 | A kind of preparation method of graphene chinlon master batch and fiber |
CN108070936A (en) * | 2017-12-06 | 2018-05-25 | 三橡股份有限公司 | A kind of Train brake hose nylon fibre, preparation method and the usage |
CN109233191A (en) * | 2018-07-26 | 2019-01-18 | 苏州汉力新材料有限公司 | A kind of preparation method of phenolic resin compound insulating material |
CN108968175A (en) * | 2018-09-13 | 2018-12-11 | 江苏红豆实业股份有限公司 | Graphene antistatic sweater |
CN109880169A (en) * | 2019-01-08 | 2019-06-14 | 常州兴烯石墨烯科技有限公司 | Modified white graphite alkene nylon compound slice of a kind of in-situ polymerization and preparation method thereof |
CN109880169B (en) * | 2019-01-08 | 2021-04-27 | 常州兴烯石墨烯科技有限公司 | In-situ polymerization modified white graphene nylon composite slice and preparation method thereof |
CN110453302A (en) * | 2019-04-19 | 2019-11-15 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene nylon fibre |
CN110699772A (en) * | 2019-11-21 | 2020-01-17 | 秦皇岛中科瀚祺科技有限公司 | Graphene/nylon fiber composite material and preparation method and application thereof |
CN110699772B (en) * | 2019-11-21 | 2022-03-18 | 秦皇岛中科瀚祺科技有限公司 | Graphene/nylon fiber composite material and preparation method and application thereof |
CN115341294A (en) * | 2021-05-13 | 2022-11-15 | 中国石油化工股份有限公司 | Thermoplastic fiber and preparation method of co-woven reinforced composite material thereof |
CN115341294B (en) * | 2021-05-13 | 2024-05-17 | 中国石油化工股份有限公司 | Preparation method of thermoplastic fiber and co-woven reinforced composite material thereof |
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