CN112301731B - Heat-conducting nylon 6/graphene composite fiber and preparation method thereof - Google Patents
Heat-conducting nylon 6/graphene composite fiber and preparation method thereof Download PDFInfo
- Publication number
- CN112301731B CN112301731B CN202011208073.1A CN202011208073A CN112301731B CN 112301731 B CN112301731 B CN 112301731B CN 202011208073 A CN202011208073 A CN 202011208073A CN 112301731 B CN112301731 B CN 112301731B
- Authority
- CN
- China
- Prior art keywords
- nylon
- graphene
- oxide
- composite fiber
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 131
- 229920002292 Nylon 6 Polymers 0.000 title claims abstract description 87
- 239000000835 fiber Substances 0.000 title claims abstract description 87
- 239000002131 composite material Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims description 32
- 229910044991 metal oxide Inorganic materials 0.000 claims description 27
- 150000004706 metal oxides Chemical class 0.000 claims description 27
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 26
- 239000002105 nanoparticle Substances 0.000 claims description 25
- 239000007864 aqueous solution Substances 0.000 claims description 19
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 14
- 239000012279 sodium borohydride Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000002135 nanosheet Substances 0.000 claims description 12
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 12
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 11
- 238000005187 foaming Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000003093 cationic surfactant Substances 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical group [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- XVWVKJVRVKPADN-UHFFFAOYSA-M didecyl(dimethyl)azanium formate Chemical compound [O-]C=O.CCCCCCCCCC[N+](C)(C)CCCCCCCCCC XVWVKJVRVKPADN-UHFFFAOYSA-M 0.000 claims description 3
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000002073 nanorod Substances 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 4
- 238000010041 electrostatic spinning Methods 0.000 description 4
- 238000002074 melt spinning Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/35—Abrasion, pilling or fibrillation resistance
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a heat-conducting nylon 6/graphene composite fiber and a preparation method thereof. The composite fiber comprises 98.5-99.5% of nylon 6 and 0.5-1.5% of graphene by mass percent. The diameter of the nylon 6 fiber is 20-50 μm, the graphene is obtained by reducing graphene oxide, and the graphene oxide consists of 5-15% of graphene oxide with the average particle size of 0.05-0.2 μm and 85-95% of graphene oxide with the average particle size of 2-5 μm in percentage by mass. The composite fiber has the characteristics of heat conduction, wear resistance and the like, and can be widely applied to the fields of clothing, carpets, decorative cloth and the like.
Description
Technical Field
The invention belongs to the field of preparation of high polymer materials, and relates to a heat-conducting nylon 6/graphene composite fiber and a preparation method thereof.
Background
The nylon 6 fiber has the advantages of wear resistance, corrosion resistance, high modulus and the like, and is widely applied to the fields of clothing, carpets, decorative cloth and the like. However, nylon 6 fiber has the disadvantages of poor thermal conductivity, easy generation of static electricity, etc., and thus, the application of nylon 6 fiber in various fields is limited. The graphene has the advantages of excellent heat conductivity, high electron mobility and the like, and the excellent properties enable the graphene to be applied to the fields of heat dissipation, static resistance and the like. The preparation of the nylon 6/graphene composite fiber can integrate the advantages of two materials of nylon 6 and graphene, and expand the application field of the composite fiber.
The existing related research work is mainly to prepare the nylon 6/graphene composite fiber by adopting melt spinning and electrostatic spinning. For example, houwins et al (RSC Advances,2014,4 (10): 4848-4855) prepared graphene modified nylon 6 fibers using melt spinning and in situ polymerization. Xiaojianhuang et al (new material academic forum, 2014, 12, 114-117) take nylon 6 as a substrate, regulate and control the viscosity of a spinning solution by adding graphene oxide and reduced graphene oxide nanosheets, and prepare the graphene/nylon 6 composite fiber by adopting electrostatic spinning. However, in the nylon 6/graphene composite fiber prepared by melt spinning and electrostatic spinning, a large amount of graphene is coated inside the nylon 6 fiber, which is not beneficial to the conduction of heat on the surface of the composite fiber, so that the heat conductivity coefficient of the composite fiber is lower (less than 1W/mK). Therefore, the preparation of the nylon 6/graphene composite fiber with high thermal conductivity (more than 5W/mK) has many practical meanings.
Disclosure of Invention
The invention aims to solve the problems and the defects of the prior art and provides a heat-conducting nylon 6/graphene composite fiber and a preparation method thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the heat-conducting nylon 6/graphene composite fiber consists of 98.5-99.5% of nylon 6 and 0.5-1.5% of graphene by mass percentage, wherein the diameter of the nylon 6 fiber is 20-50 μm, and the graphene is obtained by reducing graphene oxide.
Further preferably, the graphene oxide is composed of 5-15% by mass of graphene oxide having an average particle size of 0.05-0.2 μm and 85-95% by mass of graphene oxide having an average particle size of 2-5 μm.
In order to achieve the purpose of the invention, the invention adopts another technical scheme that:
a preparation method of heat-conducting nylon 6/graphene composite fibers specifically comprises the following steps:
step one, adding 5-15% of graphene oxide with the average particle size of 0.05-0.2 mu m by mass and 85-95% of graphene oxide with the average particle size of 2-5 mu m by mass into deionized water, and performing ultrasonic dispersion for 15 minutes to obtain 0.1-0.5mg/mL graphene oxide aqueous solution;
secondly, putting the nylon 6 fiber with the mass ratio of 98.5-99.5% into a cationic surfactant with the concentration of 0.1-0.5mol/L, a metal oxide solution with the particle size of 5-50nm and a prefabricated graphene oxide aqueous solution with the mass ratio of 0.1-0.5mg/mL, wherein the soaking time is 5-30 minutes respectively, so as to obtain the nylon 6/metal oxide/graphene oxide composite fiber;
step three, placing the nylon 6/metal oxide/graphene oxide composite fiber prepared in the step two into a sodium borohydride aqueous solution with the concentration of 0.1-0.5mol/L for foaming for 5-20 minutes, and simultaneously utilizing proton hydrogen released by the hydrolysis of the metal oxide catalytic sodium borohydride to reduce graphene oxide to obtain the nylon 6/metal oxide/graphene composite fiber with a porous structure;
and step four, putting the nylon 6/metal oxide/graphene composite fiber prepared in the step three into a 0.5-1.5% dilute hydrochloric acid solution to remove the metal oxide, and washing with deionized water for 3 times to finally obtain the nylon 6/graphene composite fiber with a porous structure.
The further preferred technical scheme is as follows:
in the first step, the two graphene oxides are added into deionized water to obtain 0.1-0.5mg/mL graphene oxide aqueous solution, wherein the mass ratio of the graphene oxide with the average particle size of 0.1 mu m is 10% and the mass ratio of the graphene oxide with the average particle size of 3 mu m is 90%;
in the second step, the mass ratio of the nylon 6 fiber is 99%, the concentration of the cationic surfactant is 0.2-0.3mol/L, the metal oxide is nanoparticles, the particle size is 10-15nm, the mass ratio of the graphene oxide is 1%, the concentration is 0.2-0.3mg/mL, and the soaking time is 10-15 minutes for the cationic surfactant solution and 10-15 minutes for the metal oxide solution, and 20-25 minutes for the graphene oxide solution, so that the nylon 6/metal oxide nanoparticles/graphene oxide composite fiber is obtained;
thirdly, the concentration of the sodium borohydride is 0.3-0.5 mol per liter, the foaming time is 10-15 minutes, and the nylon 6/metal oxide nano-particles/graphene composite fiber with a porous structure is obtained;
step four, the concentration of the dilute hydrochloric acid solution is 1-1.5%.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the nylon 6/graphene composite fiber with the porous structure is prepared by using nylon 6, a cationic surfactant, graphene oxide and metal oxide nanoparticles as raw materials through the steps of reduction, foaming and the like, the raw materials are easy to obtain, the process is simple, the cost is low, the thermal conductivity and the wear resistance are good, and the thermal conductivity coefficient is larger than 5W/mK through detection and is far better than the thermal conductivity coefficient of the nylon 6/graphene composite fiber prepared by melt spinning and electrostatic spinning at present and smaller than 1W/mK.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
Detailed Description
The technical scheme of the invention is clearly and completely described below by combining the attached drawings in the embodiment of the invention.
Example 1
1. A preparation method of heat-conducting nylon 6/graphene composite fibers comprises the following specific steps:
(1) Preparation of aqueous graphene oxide solution
Adding graphene oxide with the average particle size of 0.2 mu m in a mass ratio of 5% and the average particle size of 2 mu m in a mass ratio of 95% into deionized water, and performing ultrasonic dispersion for 15 minutes to obtain a 0.5mg/mL graphene oxide aqueous solution;
(2) Preparation of nylon 6/nickel oxide nanosheet/graphene oxide composite fiber
Putting 99% by mass of nylon 6 fibers into a hexadecyl trimethyl ammonium bromide solution with the concentration of 0.2mol/L, a nickel oxide nanosheet solution with the particle size of 15nm and a prefabricated 0.2mg/mL graphene oxide aqueous solution with the mass ratio of 1% in sequence, wherein the soaking time is 10 minutes for the hexadecyl trimethyl ammonium bromide solution and 15 minutes for the nickel oxide nanosheet solution, and the soaking time is 25 minutes for the graphene oxide solution, so as to obtain the nylon 6/nickel oxide nanosheet/graphene oxide composite fibers;
(3) Preparation of nylon 6/nickel oxide nanosheet/graphene composite fiber
Placing the nylon 6/nickel oxide nanosheet/graphene oxide composite fiber into a sodium borohydride aqueous solution with the concentration of 0.2mol per liter for foaming for 15 minutes, and simultaneously utilizing proton hydrogen released by the nickel oxide nanosheet through catalyzing hydrolysis of the sodium borohydride to reduce and oxidize the graphene to obtain the nylon 6/nickel oxide nanosheet/graphene composite fiber with a porous structure;
(4) Preparation of nylon 6/graphene composite fiber
And (3) putting the nylon 6/nickel oxide nanosheet/graphene composite fiber into a 1% dilute hydrochloric acid solution to remove the nickel oxide nanosheet, and washing with deionized water for 3 times to finally obtain the nylon 6/graphene composite fiber with a porous structure.
2. Advantageous effects
The heat conductivity coefficient of the heat-conducting nylon 6/graphene composite fiber prepared in the embodiment is 6.1W/mK through detection.
Example 2
1. A preparation method of a heat-conducting nylon 6/graphene composite fiber comprises the following specific steps:
(1) Preparation of aqueous graphene oxide solution
Adding graphene oxide with the average particle size of 0.1 micrometer in mass ratio of 10% and 3 micrometer in mass ratio of 90% into deionized water, and performing ultrasonic dispersion for 15 minutes to obtain a 0.2mg/mL graphene oxide aqueous solution;
(2) Preparation of nylon 6/cobaltosic oxide nanoparticle/graphene oxide composite fiber
Sequentially putting nylon 6 fibers with the mass ratio of 98.5% into a dodecyl trimethyl ammonium chloride solution with the concentration of 0.5mol/L, a cobaltosic oxide nanoparticle solution with the particle size of 50nm and a prefabricated graphene oxide aqueous solution with the mass ratio of 0.2mg/mL, wherein the soaking time is 20 minutes for the dodecyl trimethyl ammonium chloride solution, 25 minutes for the cobaltosic oxide nanoparticle solution and 20 minutes for the graphene oxide solution, so as to obtain the nylon 6/cobaltosic oxide nanoparticle/graphene oxide composite fibers;
(3) Preparation of nylon 6/cobaltosic oxide nanoparticle/graphene composite fiber
The nylon 6/cobaltosic oxide nano particles/graphene oxide composite fiber is placed into a sodium borohydride aqueous solution with the concentration of 0.5mol/L for foaming for 10 minutes, and meanwhile, proton hydrogen released by the hydrolysis of sodium borohydride is catalyzed by the cobaltosic oxide nano particles to reduce graphene oxide, so that the nylon 6/cobaltosic oxide nano particles/graphene oxide composite fiber with a porous structure is obtained;
(4) Preparation of nylon 6/graphene composite fiber
And (3) putting the nylon 6/cobaltosic oxide nano particles/graphene composite fiber into a 0.5% diluted hydrochloric acid solution to remove the cobaltosic oxide nano particles, and washing with deionized water for 3 times to finally obtain the nylon 6/graphene composite fiber with a porous structure.
2. Advantageous effects
The heat conductivity coefficient of the heat-conducting nylon 6/graphene composite fiber prepared by the embodiment is 5.6W/mK through detection.
Example 3
1. A preparation method of heat-conducting nylon 6/graphene composite fibers comprises the following specific steps:
(1) Preparation of aqueous graphene oxide solution
Adding graphene oxide with the average particle size of 0.05 microns in mass ratio of 15% and 2 microns in mass ratio of 85% into deionized water, and performing ultrasonic dispersion for 15 minutes to obtain a 0.05mg/mL graphene oxide aqueous solution;
(2) Preparation of nylon 6/ferroferric oxide nanoparticle/graphene oxide composite fiber
Putting nylon 6 fibers with the mass ratio of 99.5% into a bis-decyl dimethyl ammonium formate solution with the concentration of 0.1mol/L, a ferroferric oxide nanoparticle solution with the particle size of 5nm and a prefabricated graphene oxide aqueous solution with the mass ratio of 0.5% in sequence, wherein the soaking time is 5 minutes for the bis-decyl dimethyl ammonium formate solution, 15 minutes for the ferroferric oxide nanoparticle solution and 30 minutes for the graphene oxide solution, and thus obtaining the nylon 6/ferroferric oxide nanoparticle/graphene oxide composite fibers;
(3) Preparation of nylon 6/ferroferric oxide nanoparticle/graphene composite fiber
Placing the nylon 6/cobaltosic oxide nano particles/graphene oxide composite fiber into a sodium borohydride aqueous solution with the concentration of 0.1mol/L for foaming for 20 minutes, and simultaneously utilizing proton hydrogen released by the hydrolysis of sodium borohydride under the catalysis of ferroferric oxide nano particles to reduce graphene oxide to obtain the nylon 6/ferroferric oxide nano particles/graphene oxide composite fiber with a porous structure;
(4) Preparation of nylon 6/graphene composite fiber
And (3) putting the nylon 6/ferroferric oxide nano particles/graphene composite fibers into a 2% dilute hydrochloric acid solution to remove the ferroferric oxide nano particles, and washing with deionized water for 3 times to finally obtain the nylon 6/graphene composite fibers with porous structures.
2. Advantageous effects
The heat conductivity coefficient of the heat-conducting nylon 6/graphene composite fiber prepared by the embodiment is 5.5W/mK through detection.
Claims (6)
1. The heat-conducting nylon 6/graphene composite fiber is characterized by comprising 98.5-99.5% of nylon 6 fiber and 0.5-1.5% of graphene by mass percent, wherein the diameter of the nylon 6 fiber is 20-50 mu m, and the graphene is obtained by reducing graphene oxide; the graphene oxide consists of 5-15% by mass of graphene oxide with the average particle size of 0.05-0.2 mu m and 85-95% by mass of graphene oxide with the average particle size of 2-5 mu m; and is prepared by the following steps:
step one, adding 5-15% of graphene oxide with the average particle size of 0.05-0.2 mu m by mass and 85-95% of graphene oxide with the average particle size of 2-5 mu m by mass into deionized water, and performing ultrasonic dispersion for 15 minutes to obtain 0.1-0.5mg/mL graphene oxide aqueous solution;
secondly, sequentially putting the nylon 6 fibers with the mass ratio of 98.5-99.5% into a cationic surfactant with the concentration of 0.1-0.5mol/L, a metal oxide solution with the particle size of 5-50nm and a prefabricated graphene oxide aqueous solution with the mass ratio of 0.5-1.5% with the concentration of 0.1-0.5mg/mL, and soaking for 5-30 minutes respectively to obtain the nylon 6/metal oxide/graphene oxide composite fibers;
step three, placing the nylon 6/metal oxide/graphene oxide composite fiber prepared in the step two into a sodium borohydride aqueous solution with the concentration of 0.1-0.5mol per liter for foaming for 5-20 minutes, and simultaneously reducing graphene oxide by proton hydrogen released by the hydrolysis of sodium borohydride under the catalysis of metal oxide to obtain the nylon 6/metal oxide/graphene oxide composite fiber with a porous structure;
and step four, putting the nylon 6/metal oxide/graphene composite fiber prepared in the step three into a 0.5-2% dilute hydrochloric acid solution to remove the metal oxide, and washing with deionized water for 3 times to finally obtain the nylon 6/graphene composite fiber with a porous structure.
2. The preparation method of the heat-conducting nylon 6/graphene composite fiber according to claim 1, characterized by comprising the following steps:
step one, adding 5-15% of graphene oxide with the average particle size of 0.05-0.2 mu m by mass and 85-95% of graphene oxide with the average particle size of 2-5 mu m by mass into deionized water, and performing ultrasonic dispersion for 15 minutes to obtain 0.1-0.5mg/mL graphene oxide aqueous solution;
secondly, sequentially putting the nylon 6 fibers with the mass ratio of 98.5-99.5% into a cationic surfactant with the concentration of 0.1-0.5mol/L, a metal oxide solution with the particle size of 5-50nm and a prefabricated graphene oxide aqueous solution with the mass ratio of 0.5-1.5% with the concentration of 0.1-0.5mg/mL, and soaking for 5-30 minutes respectively to obtain the nylon 6/metal oxide/graphene oxide composite fibers;
step three, placing the nylon 6/metal oxide/graphene oxide composite fiber prepared in the step two into a sodium borohydride aqueous solution with the concentration of 0.1-0.5mol per liter for foaming for 5-20 minutes, and simultaneously reducing graphene oxide by proton hydrogen released by the hydrolysis of sodium borohydride under the catalysis of metal oxide to obtain the nylon 6/metal oxide/graphene oxide composite fiber with a porous structure;
and step four, putting the nylon 6/metal oxide/graphene composite fiber prepared in the step three into a 0.5-2% dilute hydrochloric acid solution to remove the metal oxide, and washing with deionized water for 3 times to finally obtain the nylon 6/graphene composite fiber with a porous structure.
3. The method of claim 2, wherein the cationic surfactant is cetyl trimethyl ammonium bromide, dodecyl trimethyl ammonium chloride or didecyl dimethyl ammonium formate.
4. The preparation method of the heat-conducting nylon 6/graphene composite fiber according to claim 2, wherein the metal oxide is nickel oxide, cobaltosic oxide or ferroferric oxide.
5. The preparation method of the heat-conducting nylon 6/graphene composite fiber according to claim 4, wherein the nickel oxide, the cobaltosic oxide and the ferroferric oxide are in the shapes of nanoparticles, nanorods or nanosheets.
6. The preparation method of the heat-conducting nylon 6/graphene composite fiber according to claim 2, wherein the foaming time of hydrolysis of sodium borohydride is 15-60 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011208073.1A CN112301731B (en) | 2020-11-03 | 2020-11-03 | Heat-conducting nylon 6/graphene composite fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011208073.1A CN112301731B (en) | 2020-11-03 | 2020-11-03 | Heat-conducting nylon 6/graphene composite fiber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112301731A CN112301731A (en) | 2021-02-02 |
| CN112301731B true CN112301731B (en) | 2022-12-27 |
Family
ID=74332461
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011208073.1A Active CN112301731B (en) | 2020-11-03 | 2020-11-03 | Heat-conducting nylon 6/graphene composite fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112301731B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108709A (en) * | 2014-07-25 | 2014-10-22 | 深圳新宙邦科技股份有限公司 | Porous graphene and preparation method thereof |
| CN105442302A (en) * | 2015-12-07 | 2016-03-30 | 江南石墨烯研究院 | Water treatment composite weaving net based on oxidized graphene and preparation method and application thereof |
| CN105484016A (en) * | 2015-12-28 | 2016-04-13 | 宁国市龙晟柔性储能材料科技有限公司 | Preparation method of graphene composite conductive fiber |
| CN108085966A (en) * | 2017-12-21 | 2018-05-29 | 河南新野纺织股份有限公司 | A kind of preparation method of graphene composite conductive fiber textile |
| CN109267326A (en) * | 2018-07-20 | 2019-01-25 | 华中科技大学 | Multi-element doping carbon nano pipe array modifying carbon fibers and the preparation method and application thereof |
| CN109368620A (en) * | 2018-12-11 | 2019-02-22 | 中国科学院兰州化学物理研究所 | A kind of preparation method of extra small sub-nanometer hole porous graphene |
| CN109734081A (en) * | 2019-03-18 | 2019-05-10 | 新奥石墨烯技术有限公司 | Mesoporous template and preparation method thereof, three-dimensional meso-hole graphene and preparation method thereof, energy storage material and battery |
| CN111576037A (en) * | 2020-05-28 | 2020-08-25 | 浙江倪阮新材料有限公司 | Preparation method of three-dimensional porous graphene/nano zinc oxide modified nylon 6 fiber composite material |
| CN111809388A (en) * | 2020-07-02 | 2020-10-23 | 浙江理工大学 | Preparation method and application of graphene manganese ferrite coating fabric |
-
2020
- 2020-11-03 CN CN202011208073.1A patent/CN112301731B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108709A (en) * | 2014-07-25 | 2014-10-22 | 深圳新宙邦科技股份有限公司 | Porous graphene and preparation method thereof |
| CN105442302A (en) * | 2015-12-07 | 2016-03-30 | 江南石墨烯研究院 | Water treatment composite weaving net based on oxidized graphene and preparation method and application thereof |
| CN105484016A (en) * | 2015-12-28 | 2016-04-13 | 宁国市龙晟柔性储能材料科技有限公司 | Preparation method of graphene composite conductive fiber |
| CN108085966A (en) * | 2017-12-21 | 2018-05-29 | 河南新野纺织股份有限公司 | A kind of preparation method of graphene composite conductive fiber textile |
| CN109267326A (en) * | 2018-07-20 | 2019-01-25 | 华中科技大学 | Multi-element doping carbon nano pipe array modifying carbon fibers and the preparation method and application thereof |
| CN109368620A (en) * | 2018-12-11 | 2019-02-22 | 中国科学院兰州化学物理研究所 | A kind of preparation method of extra small sub-nanometer hole porous graphene |
| CN109734081A (en) * | 2019-03-18 | 2019-05-10 | 新奥石墨烯技术有限公司 | Mesoporous template and preparation method thereof, three-dimensional meso-hole graphene and preparation method thereof, energy storage material and battery |
| CN111576037A (en) * | 2020-05-28 | 2020-08-25 | 浙江倪阮新材料有限公司 | Preparation method of three-dimensional porous graphene/nano zinc oxide modified nylon 6 fiber composite material |
| CN111809388A (en) * | 2020-07-02 | 2020-10-23 | 浙江理工大学 | Preparation method and application of graphene manganese ferrite coating fabric |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112301731A (en) | 2021-02-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111501329B (en) | Preparation method of nickel hydroxide/polyetheramine modified carbon fiber | |
| CN110102754A (en) | A kind of heavy-duty vehicle dry clutch copper based powder metallurgy friction material and preparation method thereof | |
| CN111455208B (en) | Nano modified aluminum alloy material, preparation method thereof and energy-saving and environment-friendly electric power fitting manufactured by nano modified aluminum alloy material | |
| CN104446306A (en) | Submicron inorganic whisker aerogel thermal insulation composite and preparation method thereof | |
| CN109776851A (en) | A kind of bacteria cellulose/metal sulfide plural gel and preparation method thereof and conductive processing method | |
| CN113846482A (en) | Preparation method of carbon fiber/rare earth oxide nanowire mixed reinforcement, material obtained by preparation method and application of material | |
| CN109609113A (en) | A kind of heat-resistance type composite clean fracturing fluid and preparation method thereof | |
| CN102580549A (en) | Method for preparing carbon nano tube modified bipolar membrane with anion groups | |
| CN106334502A (en) | Preparation method of reduced-oxidized graphene/aspergillus niger cellulose aerogel | |
| CN102703936A (en) | Carbon nano tube/cobalt composite coating and preparation method thereof | |
| CN112301731B (en) | Heat-conducting nylon 6/graphene composite fiber and preparation method thereof | |
| CN106752713B (en) | Wear-resistant aluminum alloy profile and preparation method thereof | |
| CN106957503A (en) | Polytetrafluoroethylene (PTFE)/Polyimide/Nano silica self-lubricating material and preparation method thereof | |
| CN101886022A (en) | Preparation method of high-efficiency water-based lubricating liquid based on carbon nano-tube | |
| CN110304622A (en) | A kind of preparation method of graphene film | |
| CN106925312A (en) | One kind carbonization grapheme modified composite of molybdenum doping linear polymer and preparation method thereof | |
| CN106747265A (en) | A kind of aerogel composite and its preparation method based on self assembly opacifier fiber | |
| WO2023109667A1 (en) | Rare earth modified graphene copper-based composite material, preparation method thereof and application | |
| CN110282952A (en) | The composite material and preparation method for having electromagnetic shielding and shape-memory properties | |
| CN109554063B (en) | Graphene modified phenolic resin heat-resistant and wear-resistant coating and preparation method thereof | |
| CN110715005A (en) | Preparation method of high-thermal-conductivity copper-based brake pad with orientation structure | |
| CN106189151A (en) | A kind of composite glass fiber reinforced polyester glass-reinforced plastic material and preparation method thereof | |
| CN111534050B (en) | Carbon fiber composite material with multi-scale high-temperature-resistant interface structure and preparation method thereof | |
| CN109505037B (en) | Composite reinforced material with interpenetrating network structure and preparation method thereof | |
| CN116376520B (en) | Preparation method of carboxymethyl chitosan reinforced nano boron nitride aerogel composite phase change material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |