CN107164817B - A kind of preparation method of graphene-graphene oxide composite nylon fiber - Google Patents
A kind of preparation method of graphene-graphene oxide composite nylon fiber Download PDFInfo
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- CN107164817B CN107164817B CN201710419099.2A CN201710419099A CN107164817B CN 107164817 B CN107164817 B CN 107164817B CN 201710419099 A CN201710419099 A CN 201710419099A CN 107164817 B CN107164817 B CN 107164817B
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- graphene
- graphene oxide
- nylon fiber
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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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- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of graphene-graphene oxide composite nylon fiber preparation methods, including prepare graphene oxide nylon fiber, are oiled by oil nozzle and add reducing agent, hot-rolling heating reduction and etc.；The beneficial effects of the present invention are: first preparing graphene oxide nylon fiber, graphene oxide will not reunite, it is evenly distributed in the fibre, the graphene oxide of fiber sheath can be reduced into graphene in the case where hot-rolling heats by the reducing agent added in finish when fiber is oiled by oil nozzle, therefore foring fiber internal layer is graphene-graphene oxide composite nylon fiber that graphene oxide outer layer is graphene, and graphene granularity is small in outer layer and is evenly distributed；Furthermore, since graphene is lamellar structure, the crystallinity of external strata amide influences very little, but the multilayered structure of graphene oxide can reduce the crystallinity of internal layer polyamide, therefore the composite fibre internal layer density ratio outer layer density is small, so that fiber has preferable heat-blocking action.
Description
Technical field
The present invention relates to composite fibre field more particularly to a kind of graphene-graphene oxide composite nylon fiber systems
Preparation Method.
Background technique
Fypro, also known as nylon, are the first synthetic fibers occurred in the world, and nylon is that one kind contains amido bond
Chemical fibre, with there is functional group protein as, therefore nylon can directly contact the chemical fibre of skin as one kind
The characteristics such as dimension is widely used in textile industry, and nylon fiber has soft, moisture absorbing and sweat releasing, and easy coloring is colour-fast,
But also have and be easy aging, uvioresistant performance is poor, easy the disadvantages of playing electrostatic.Nowadays the development of nylon industry is from conventional life
The research and development that gradually turning functionization is modified are produced, a collection of functionalization composite nylon fiber successively occur, for example be added in nylon
Titanium dioxide improves nylon uvioresistant performance, and nano metal particles are added and increase nylon bactericidal property, and nano-graphite production is added
Exempt to contaminate black nylon fiber etc..
Graphene is presently found unique existing Two Dimensional Free state atom as a kind of novel two-dimension nano materials
Crystal, graphene are the two dimension monoatomic layer flake crystallines as made of the carbon atom honeycomb hexagonal structure close-packed arrays of sp2 hydridization
Body material has the structure of big pi-conjugated system and most thin single layer atomic thickness, this makes it possess unique light, electricity, magnetic, machine
The physical properties such as tool and chemical property, since discovery in 2004, graphene not only receives very big concern in pure science,
Also have in the specific practical application of the numerous areas such as electronics, optics, magnetics, biomedicine, catalysis, energy storage and sensor very high
Potentiality to be exploited and application value.
Graphene particles, which are added in nylon fiber, can make nylon fiber have the performances such as antibacterial bacteriostatic, antistatic,
The preparation of graphene composite nylon fiber is usually that graphene powder is first made into master batch and polyamide granules according to certain ratio
Melt spinning is carried out after example mixing, since the lamellar structure of graphene makes graphene easily reunite, will appear in melt
On the one hand the graphene particles of greater particle size, these bulky grains can block spinning pack to increasing production cost, on the other hand,
Graphene bulky grain in fiber will form stress concentration point, and when stretching is easily broken off, and reduce product quality.
Summary of the invention
The present invention for graphene reunion bring component blocking in existing graphene composite nylon fiber manufacturing process and
The easily broken problem of fiber provides a kind of preparation method of graphene-graphene oxide composite nylon fiber.
The technical scheme to solve the above technical problems is that
A kind of preparation method of graphene-graphene oxide composite nylon fiber, comprising the following steps:
1) graphene oxide and polyamide are prepared into graphene oxide master batch, polyamide granules is mixed with the master batch
Investment extruder carries out melt spinning after uniformly；
2) melt tow after spinning pack sprays oils through oil nozzle, and reducing agent is added in finish；
3) after oiling, graphene-graphene oxide composite nylon fiber is made after hot-rolling carries out hot gas spring in tow.
Wherein, mass fraction of the graphene oxide in master batch is 20%, and polyamide granules and master batch are 10 in mass ratio:
1-10:3；Finish is the white oil aqueous solution of mass fraction 15%, and mass fraction of the reducing agent in finish is 5-15%, reducing agent
For for one of sodium borohydride, sodium citrate；The temperature of hot-rolling is 100-140 DEG C.
The beneficial effects of the present invention are: first preparing graphene oxide nylon fiber, graphene oxide will not reunite, in fiber
In be evenly distributed, the reducing agent added in finish when fiber is oiled by oil nozzle can fiber sheath in the case where hot-rolling heats
Graphene oxide be reduced into graphene, therefore foring fiber internal layer is the graphene-that graphene oxide outer layer is graphene
Graphene oxide composite nylon fiber, and graphene granularity is small in outer layer and is evenly distributed；Further, since graphene is lamella
The crystallinity of structure, external strata amide influences very little, but the multilayered structure of graphene oxide can reduce the knot of internal layer polyamide
Brilliant degree, therefore the composite fibre internal layer density ratio outer layer density is small, so that fiber has preferable heat-blocking action.
Detailed description of the invention
Fig. 1 is graphene-graphene oxide composite nylon fiber production process figure, wherein
1 blending bucket；
2 screw extruders；
3 spinning packs；
4 finish casees；
5 oil nozzles；
6 hot-rollings；
7 package devices.
Specific embodiment
Below in conjunction with Fig. 1, present invention is described, and the given examples are served only to explain the present invention, is not intended to limit this hair
Bright range.
A kind of preparation method of graphene-graphene oxide composite nylon fiber, comprising the following steps:
1) graphene oxide and polyamide are prepared into graphene oxide master batch, the mass fraction of graphene oxide in master batch
It is 20%, polyamide granules and master batch 10:1-10:3 in mass ratio is put into extruder after mixing in blending bucket and are carried out
Melt spinning；
2) melt tow after spinning pack sprays oils through oil nozzle, and finish is the white oil of mass fraction 15% in finish case
Aqueous solution, is added with reducing agent in finish, and mass fraction of the reducing agent in finish is 5-15%, reducing agent be sodium borohydride,
One of sodium citrate；
3) tow through oil nozzle oil using temperature be 100-140 DEG C hot-rolling carry out hot gas spring after be made graphene-oxygen
Graphite alkene composite nylon fiber, it is coiled through package device package.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of graphene-graphene oxide composite nylon fiber preparation method, which comprises the following steps:
1) graphene oxide and polyamide are prepared into graphene oxide master batch, polyamide granules is uniformly mixed with the master batch
Investment extruder carries out melt spinning afterwards；
2) melt tow after spinning pack sprays oils through oil nozzle, and reducing agent is added in finish, and the finish is quality point
The white oil aqueous solution of number 15%, mass fraction of the reducing agent in finish are 5-15%, and the reducing agent is hydroboration
One of sodium, sodium citrate；
3) after oiling, graphene-graphene oxide composite nylon fiber is made after hot-rolling carries out hot gas spring in tow.
2. graphene according to claim 1-graphene oxide composite nylon fiber preparation method, which is characterized in that
Mass fraction of the graphene oxide described in the step 1) in the master batch is 20%, the polyamide granules and the mother
Grain is 10:1-10:3 in mass ratio.
3. graphene according to claim 1-graphene oxide composite nylon fiber preparation method, which is characterized in that
The temperature of hot-rolling described in the step 3) is 100-140 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710419099.2A CN107164817B (en) | 2017-06-06 | 2017-06-06 | A kind of preparation method of graphene-graphene oxide composite nylon fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710419099.2A CN107164817B (en) | 2017-06-06 | 2017-06-06 | A kind of preparation method of graphene-graphene oxide composite nylon fiber |
Publications (2)
| Publication Number | Publication Date |
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| CN107164817A CN107164817A (en) | 2017-09-15 |
| CN107164817B true CN107164817B (en) | 2019-03-26 |
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| CN109898173A (en) * | 2019-03-20 | 2019-06-18 | 江苏江山红化纤有限责任公司 | A kind of 6 fiber of colored polyamide and its production method |
| CN110886030A (en) * | 2019-12-20 | 2020-03-17 | 湖州拉杜拉塔服饰有限公司 | Preparation method of nylon yarn with good antibacterial and dyeing properties |
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| KR101233818B1 (en) * | 2011-06-07 | 2013-02-18 | 단국대학교 산학협력단 | Method for Preparing the Fiber Treated by Graphene |
| KR101830797B1 (en) * | 2012-04-16 | 2018-02-21 | 한국전자통신연구원 | Method of forming a Graphene fiber |
| CN102690426B (en) * | 2012-06-08 | 2013-11-06 | 浙江大学 | Method for preparing graphene/polymer composite material based on infrared irradiation |
| CN102828267B (en) * | 2012-09-10 | 2014-05-07 | 浙江大学 | Preparation method of conductive high-strength graphene-reinforced polymer fiber |
| CN103541043A (en) * | 2013-08-01 | 2014-01-29 | 华为技术有限公司 | Preparation method of electric graphene composite fiber |
| CN103603088B (en) * | 2013-10-22 | 2015-05-06 | 浙江大学 | Conductive fiber with scabbard type structure and preparation method thereof |
| CN105088415B (en) * | 2015-06-15 | 2018-01-05 | 中国科学技术大学 | A kind of wet spinning graphene oxide solution and preparation method thereof and a kind of graphene fiber and preparation method thereof |
| CN106676664B (en) * | 2016-08-31 | 2019-07-09 | 浙江金旗新材料科技有限公司 | A kind of 6 preoriented yarn of flame-proof abrasion-resistant type polyamide fibre |
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Address after: No. 2, 4 Street, Guan Zhuang, Muping District, Yantai, Shandong Applicant after: Yantai Energetic New Materials Co.,Ltd. Address before: 264000 AUCMA Street 101, Laishan Economic Development Zone, Yantai, Shandong. Applicant before: YANTAI SINAGRAPHENE Co.,Ltd. |
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Effective date of registration: 20220802 Address after: 265700 Donghai Industrial Park, Xufu street, Longkou City, Yantai City, Shandong Province Patentee after: Shandong Nanshan Science and Technology Research Institute Co.,Ltd. Address before: No. 2, 4 Street, Guan Zhuang, Muping District, Yantai, Shandong Patentee before: Yantai Energetic New Materials Co.,Ltd. |