CN107164817A - 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 PDF

Info

Publication number
CN107164817A
CN107164817A CN201710419099.2A CN201710419099A CN107164817A CN 107164817 A CN107164817 A CN 107164817A CN 201710419099 A CN201710419099 A CN 201710419099A CN 107164817 A CN107164817 A CN 107164817A
Authority
CN
China
Prior art keywords
graphene
graphene oxide
nylon fiber
fiber
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710419099.2A
Other languages
Chinese (zh)
Other versions
CN107164817B (en
Inventor
李恕广
李泰胧
孙健
于永杰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Nanshan Science And Technology Research Institute Co ltd
Original Assignee
Yantai Sinagraphene Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Yantai Sinagraphene Co Ltd filed Critical Yantai Sinagraphene Co Ltd
Priority to CN201710419099.2A priority Critical patent/CN107164817B/en
Publication of CN107164817A publication Critical patent/CN107164817A/en
Application granted granted Critical
Publication of CN107164817B publication Critical patent/CN107164817B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/90Monocomponent 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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/08Chemical 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

Abstract

The invention discloses a kind of preparation method of graphene graphene oxide composite nylon fiber, including prepare graphene oxide nylon fiber, oiled addition reducing agent by oil nozzle, the step such as hot-rolling heating reduction;The beneficial effects of the invention are as follows:First prepare 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 by the reducing agent added when fiber is oiled by oil nozzle in finish in the case where hot-rolling is heated, therefore it is the graphene graphene oxide composite nylon fiber that graphene oxide outer layer is graphene to form fiber internal layer, and graphene granularity is small in outer layer and is evenly distributed;In addition, because graphene is lamellar structure, the crystallinity of external strata acid amides influences very little, but the sandwich construction 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

A kind of preparation method of graphene-graphene oxide composite nylon fiber
Technical field
The present invention relates to the system in composite fibre field, more particularly to a kind of graphene-graphene oxide composite nylon fiber Preparation Method.
Background technology
Fypro, also known as nylon, are the first synthetic fibers occurred in the world, and nylon is that one kind contains amido link Chemical fibre, with the functional group as protein, therefore nylon is fine as a kind of chemistry that can directly contact skin Dimension is widely used in textile industry, and nylon fiber has soft a, moisture absorbing and sweat releasing, the characteristic such as easy coloring is colour-fast, But also there is easy aging, uvioresistant performance is poor, the shortcomings of easily playing electrostatic.Nowadays the development of nylon industry is from conventional life The production research and development that progressively turning functionization is modified, successively occur in that a collection of functionalization composite nylon fiber, such as are added in nylon Titanium dioxide improves nylon uvioresistant performance, adds nano metal particles increase nylon bactericidal property, adds nano-graphite production Exempt from dye black nylon fiber etc..
Graphene, as a kind of new two-dimension nano materials, is the Two Dimensional Free state atom for the unique presence having now been found that Crystal, graphene is by the two-dimentional monoatomic layer flake crystalline of the cellular hexagonal structure close-packed arrays of carbon atom of sp2 hydridization Body material, the structure with big pi-conjugated system and most thin individual layer atomic thickness, this causes it to possess the light of uniqueness, electricity, magnetic, machine The physical properties such as tool and chemical property, since being found from 2004, graphene not only receives very big concern in pure science, Also have very high in the specific practical application of the numerous areas such as electronics, optics, magnetics, biomedicine, catalysis, energy storage and sensor 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 master batch, and polyamide granules according to certain ratio Melt spinning is carried out after example mixing, because the lamellar structure of graphene causes graphene easily to reunite, therefore is occurred in melt On the one hand the graphene particles of greater particle size, these bulky grains can block spinning pack to increase production cost, on the other hand, Graphene bulky grain in fiber can form stress concentration point, be easily broken off during stretching, reduce product quality.
The content of the invention
The present invention be directed to graphene in existing graphene composite nylon fiber manufacturing process reunite the component that brings block and There is provided a kind of preparation method of graphene-graphene oxide composite nylon fiber for the problem of fiber is easily broken.
The technical scheme that the present invention solves above-mentioned technical problem is as follows:
A kind of preparation method of graphene-graphene oxide composite nylon fiber, comprises the following steps:
1) graphene oxide and polyamide are prepared into graphene oxide master batch, polyamide granules is mixed with the master batch Input extruder carries out melt spinning after uniform;
2) tow is oiled through oil nozzle after melt sprays through spinning pack, and reducing agent is added with 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 are 10 in mass ratio with master batch: 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 kind in sodium borohydride, sodium citrate;The temperature of hot-rolling is 100-140 DEG C.
The beneficial effects of the invention are as follows:Graphene oxide nylon fiber is first prepared, graphene oxide will not reunite, in fiber In be evenly distributed, the reducing agent added when fiber is oiled by oil nozzle in finish can fiber sheath in the case where hot-rolling is heated Graphene oxide be reduced into graphene, therefore form fiber internal layer be 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 Structure, the crystallinity influence very little of external strata acid amides, but the sandwich construction 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.
Brief description of the drawings
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.
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 scope.
A kind of preparation method of graphene-graphene oxide composite nylon fiber, comprises the following steps:
1) graphene oxide and polyamide are prepared into the mass fraction of graphene oxide in graphene oxide master batch, master batch For 20%, by polyamide granules and master batch in mass ratio 10:1-10:3 in blending bucket be well mixed after input extruder carry out Melt spinning;
2) tow oils through oil nozzle after melt sprays through spinning pack, and finish is the white oil of mass fraction 15% in finish case In the aqueous solution, finish be added with reducing agent, mass fraction of the reducing agent in finish be 5-15%, reducing agent be sodium borohydride, One kind in sodium citrate;
3) it is again obtained graphene-oxygen after 100-140 DEG C of hot-rolling progress hot gas spring through excess temperature that tow oils through oil nozzle Graphite alkene composite nylon fiber, it is coiled through device package is wrapped.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.

Claims (4)

1. the preparation method of a kind of graphene-graphene oxide composite nylon fiber, it is characterised in that comprise the following steps:
1) graphene oxide and polyamide are prepared into graphene oxide master batch, polyamide granules is well mixed with the master batch Input extruder carries out melt spinning afterwards;
2) tow is oiled through oil nozzle after melt sprays through spinning pack, and reducing agent is added with finish;
3) after oiling, graphene-graphene oxide composite nylon fiber is made after hot-rolling carries out hot gas spring in tow.
2. the preparation method of graphene according to claim 1-graphene oxide composite nylon fiber, it is characterised in that The step 1) described in mass fraction of the graphene oxide in the master batch be 20%, the polyamide granules and the mother Grain is 10 in mass ratio:1-10:3.
3. the preparation method of graphene according to claim 1-graphene oxide composite nylon fiber, it is characterised in that The step 2) described in finish be mass fraction 15% the white oil aqueous solution, mass fraction of the reducing agent in finish be 5-15%, the reducing agent is one kind in sodium borohydride, sodium citrate.
4. the preparation method of graphene according to claim 1-graphene oxide composite nylon fiber, it is characterised in that The step 3) described in hot-rolling temperature be 100-140 DEG C.
CN201710419099.2A 2017-06-06 2017-06-06 A kind of preparation method of graphene-graphene oxide composite nylon fiber Active CN107164817B (en)

Priority Applications (1)

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

Applications Claiming Priority (1)

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
CN107164817A true CN107164817A (en) 2017-09-15
CN107164817B CN107164817B (en) 2019-03-26

Family

ID=59824401

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710419099.2A Active CN107164817B (en) 2017-06-06 2017-06-06 A kind of preparation method of graphene-graphene oxide composite nylon fiber

Country Status (1)

Country Link
CN (1) CN107164817B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102690426A (en) * 2012-06-08 2012-09-26 浙江大学 Method for preparing graphene/polymer composite material based on infrared irradiation
WO2012169804A2 (en) * 2011-06-07 2012-12-13 단국대학교 산학협력단 Method for manufacturing a graphene-treated fiber
CN102828267A (en) * 2012-09-10 2012-12-19 浙江大学 Preparation method of conductive high-strength graphene-reinforced polymer fiber
US20130272950A1 (en) * 2012-04-16 2013-10-17 Electronics And Telecommunications Research Institute Method of manufacturing a graphene fiber
CN103541043A (en) * 2013-08-01 2014-01-29 华为技术有限公司 Preparation method of electric graphene composite fiber
CN103603088A (en) * 2013-10-22 2014-02-26 浙江大学 Conductive fiber with scabbard type structure and preparation method thereof
CN105088415A (en) * 2015-06-15 2015-11-25 中国科学技术大学 Graphene oxide solution for wet spinning and preparation method thereof, graphene fiber and preparation method of graphene fiber
CN106676664A (en) * 2016-08-31 2017-05-17 浙江金旗新材料科技有限公司 Flame-retardant and wear-resistant type chinlon 6 pre-oriented yarn

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012169804A2 (en) * 2011-06-07 2012-12-13 단국대학교 산학협력단 Method for manufacturing a graphene-treated fiber
US20130272950A1 (en) * 2012-04-16 2013-10-17 Electronics And Telecommunications Research Institute Method of manufacturing a graphene fiber
CN102690426A (en) * 2012-06-08 2012-09-26 浙江大学 Method for preparing graphene/polymer composite material based on infrared irradiation
CN102828267A (en) * 2012-09-10 2012-12-19 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
CN103603088A (en) * 2013-10-22 2014-02-26 浙江大学 Conductive fiber with scabbard type structure and preparation method thereof
CN105088415A (en) * 2015-06-15 2015-11-25 中国科学技术大学 Graphene oxide solution for wet spinning and preparation method thereof, graphene fiber and preparation method of graphene fiber
CN106676664A (en) * 2016-08-31 2017-05-17 浙江金旗新材料科技有限公司 Flame-retardant and wear-resistant type chinlon 6 pre-oriented yarn

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Also Published As

Publication number Publication date
CN107164817B (en) 2019-03-26

Similar Documents

Publication Publication Date Title
CN111235671A (en) Modified graphene anti-ultraviolet polyamide fiber and preparation method thereof
WO2017066937A1 (en) Method for preparing graphene-polyester nanocomposite fiber
CN110205702A (en) A kind of modified white graphite alkene terylene composite fibre and preparation method thereof
CN107164817B (en) A kind of preparation method of graphene-graphene oxide composite nylon fiber
CN104141177B (en) Antistatic wool top and its manufacture method
CN103774272B (en) A kind of ultra-thin light-weight fabric ultraviolet resistant nylon 6 fiber and preparation method thereof
CN101967699A (en) Preparation method of high-performance carbon nanotube fiber
WO2011111559A1 (en) Carbon-fiber chopped strand and manufacturing method of the same
CN1818161A (en) Health-care fibre and production thereof
CN106003934B (en) A kind of anti-electrostatic nano fibrous nonwoven material and preparation method
CN107459782A (en) A kind of processing technology of nano modification PET bottle reworked material production strap
CN113611438B (en) Crushing method of carbon nanotube fiber bundle and conductive slurry
CN102425015A (en) Method for preparing fibers with performance of sheep wool and imitated wool fabric
CN109797455A (en) Modified ES composite fibre of one Plant Extracts and preparation method thereof
CN109576805A (en) A kind of corrugated imitates bristle brush silk and its processing method
CN103981589A (en) Production process of far-infrared polyamide fiber
CN105440280A (en) Preparation method and application of anti-radiation nylon 6 resin
CN113417026B (en) Graphene high-thermal-insulation fiber and preparation method thereof
CN102011210A (en) Flat far infrared ECDP magnetic fiber and preparation method thereof
Zan et al. Double layer metal selenides growing on Ni-plated carbon fibers toward high efficiency electromagnetic wave absorption
CN101275310A (en) Production technology for polylactic acid anti-bacterial fiber having skin-core structure
CN102296375A (en) Bamboo charcoal health-care polypropylene magnetic fiber and preparation method thereof
TW202016375A (en) Manufacturing method of nanometer filament capable of preventing nanometer shell powder from blocking the extrusion of polyester
TWI314595B (en)
CN103407169A (en) Textured yarn long-fiber reinforced thermoplastic plastic granules and production method thereof

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
CB02 Change of applicant information

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.

CB02 Change of applicant information
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

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.

TR01 Transfer of patent right