CN106012090A - Preparation method of conductive graphene composite fibers - Google Patents
Preparation method of conductive graphene composite fibers Download PDFInfo
- Publication number
- CN106012090A CN106012090A CN201610469735.8A CN201610469735A CN106012090A CN 106012090 A CN106012090 A CN 106012090A CN 201610469735 A CN201610469735 A CN 201610469735A CN 106012090 A CN106012090 A CN 106012090A
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- Prior art keywords
- graphene
- solution
- preparation
- graphene oxide
- fibers
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Classifications
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
-
- 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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/003—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
Abstract
The invention belongs to the technical field of textiles and particularly relates to a preparation method of conductive graphene composite fibers. The preparation method comprises the following preparation steps: 1) hemp fibers are put into a pectinase solution and soaked at the normal temperature; then the treated hemp fibers are immersed in a chitosan water solution, soaked, dewatered and dried; 2) the prepared hemp fibers are immersed in a graphene dispersion liquid and put into an oven to be dried, and the conductive graphene composite fibers are obtained. The preparation method has the technical advantages as follows: 1) the graphene fibers are added for blending, the strength and the toughness of the hemp fibers are improved, the electrical resistivity of the conductive composite fibers is about 10-103 omega.m while the electrical resistivity of common fibers is 1,014 omega.m; 2) the dyeing effect of the composite fibers can be improved after the hemp fibers are modified with biological enzymes.
Description
Technical field
The invention belongs to textile technology field, be specifically related to the preparation method of a kind of graphene conductive composite fibre.
Background technology
Conductive fiber is always the study hotspot of functional fiber, generally refers to resistivity less than 108The fiber of Ω cm, has the functions such as conduction, electric heating and anti-electromagnetic radiation, generally concentrates the fields such as the antistatic clothes being applied in special occasions use or anti-electromalgnetic radiation clothes.
The main method of conductive fiber manufacture includes, one is conventional fibre surface-coated conductive compositions, and another kind is that conductive material mixes with fibrous raw material, makes conductive fiber by spinning technique.Fiber surface conductive coating method is by the conductive material containing metal, carbon black or metallic compound, it is coated on fiber surface and makes conductive fiber, also the conduction high polymers such as polyaniline can be adsorbed in fiber surface by situ aggregation method and obtain conductive fiber, filamentary conductive prepared by said method can highlight, but water-wash resistance and durability are not ideal enough.The main polymer of conducting particles (predominantly carbon black or metallic compound) with non-conductive composition is blended by co-blended spinning, composite conducting fiber is prepared by melted or wet spinning technology, in spinning process, conducting particles easily produces reunion, affects the conductive effect of composite fibre.
Graphene be a kind of by carbon atom with sp2Hybrid orbital composition hexangle type is the two-dimension nano materials of honeycomb lattice, has perfect big pi-conjugated system and the structure of the thinnest monolayer atomic thickness (0.34nm).The physical and chemical performance (heat conduction high-strength, high, high connductivity, Ultralight) of the nanostructured special due to it and excellence and show huge application potential at numerous areas such as biomedicine, energy storage, sensor and composites.
Being combined with flaxen fiber by Graphene, the research preparing electrically conductive composite fibre still rarely has report.
Summary of the invention
It is an object of the invention to provide the novel preparation method of a kind of graphene conductive composite fibre.
Realizing the optimal technical scheme that the object of the invention uses is: the preparation method of a kind of graphene conductive composite fibre, and the method includes following preparation process:
1) flaxen fiber is placed in soak at room temperature in pectinase solution；Then the flaxen fiber after processing continues to be immersed in immersion in chitosan aqueous solution, is dehydrated, dries；
2) flaxen fiber that step 1) prepares is immersed in graphene dispersing solution, is subsequently placed in baking oven drying, obtains graphene conductive composite fibre；
Wherein, described graphene dispersing solution is carboxylated Graphene and N, the mixture of N-dimethyl formyl, carboxylated Graphene and N, and the mass volume ratio of N-dimethyl formyl is 100mg:(50～100mL).
Preferably, the concentration of the pectinase solution described in step 1) is 10～50g/L, and soak time is 15～30 minutes；Described chitosan aqueous solution concentration is 10～20g/L, and soak time is 1～3 hour.
Preferably, described flaxen fiber is 1g:(5～20mL with the mass volume ratio of graphene dispersing solution), soak time is 1～3 hour.
It is furthermore preferred that described carboxylated graphene fiber is prepared by following steps:
1) adding graphene oxide in deionized water, the mass volume ratio of graphene oxide and deionized water is 1mg:(1～3mL), ultrasonic disperse 0.5～after 2 hours, obtain finely dispersed graphene oxide water solution；
2) finely dispersed graphene oxide water solution is mixed with monoxone, described monoxone is 50:1 with the mass ratio of graphene oxide, then under the conditions of low whipping speed is 50～200 revs/min, mixed solution is heated to 60～80 DEG C, keep its reaction 0.5～3 hour, it is cooled to room temperature, with membrane filtration, obtains carboxylated graphene oxide after drying；
3) by carboxylated graphene oxide ultrasonic disperse in N, N-dimethyl formyl.
The technological merit of the present invention is:1) present invention is by adding graphene fiber blending, improves intensity and the toughness of flaxen fiber so that the resistivity of electrically conductive composite fibre about 10～103Ω m, and the resistivity of conventional fibre about 1014Ω·m.2) flaxen fiber of the present invention is after enzyme modified processes, and can improve the Color of composite fibre.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment
1
1) 1g hemp being placed in 50mL concentration is soak at room temperature 30 minutes in 10g/L pectinase solution；Then it is to soak 1 hour in 20g/L chitosan aqueous solution that the hemp after processing continues to be immersed in 50mL concentration, is dehydrated, dries；
2) prepared cotton fiber is immersed in 5mL graphene dispersing solution 1 hour, is subsequently placed in baking oven drying, obtains graphene conductive composite fibre.This graphene dispersing solution is carboxylated Graphene and N, the mixture of N-dimethyl formyl, carboxylated Graphene and N, and the mass volume ratio of N-dimethyl formyl is 100mg:50mL.
Embodiment
2
1) 1g hemp being placed in 50mL concentration is soak at room temperature 15 minutes in 50g/L pectinase solution；Then it is to soak 3 hours in 10g/L chitosan aqueous solution that the hemp after processing continues to be immersed in 50mL concentration, is dehydrated, dries；
2) prepared cotton fiber is immersed in 20mL graphene dispersing solution 2 hours, is subsequently placed in baking oven drying, obtains graphene conductive composite fibre.This graphene dispersing solution is carboxylated Graphene and N, the mixture of N-dimethyl formyl, carboxylated Graphene and N, and the mass volume ratio of N-dimethyl formyl is 100mg:80mL.
Embodiment
3
1) 1g hemp being placed in 50mL concentration is soak at room temperature 20 minutes in 30g/L pectinase solution；Then it is to soak 2 hours in 15g/L chitosan aqueous solution that the hemp after processing continues to be immersed in 50mL concentration, is dehydrated, dries；
2) prepared cotton fiber is immersed in 10mL graphene dispersing solution 3 hours, is subsequently placed in baking oven drying, obtains graphene conductive composite fibre.This graphene dispersing solution is carboxylated Graphene and N, the mixture of N-dimethyl formyl, carboxylated Graphene and N, and the mass volume ratio of N-dimethyl formyl is 100mg:100mL.
Embodiment
4
Graphene fiber in embodiment 1～3 can prepare as follows.
1) being added in 100mL deionized water by 100mg graphene oxide, ultrasonic disperse, after 0.5 hour, obtains finely dispersed graphene oxide water solution；
2) in finely dispersed graphene oxide water solution, add the mixing of 5g monoxone, under the conditions of then low whipping speed is 50 revs/min, mixed solution is heated to 80 DEG C, keep its reaction 0.5 hour, it is cooled to room temperature, with membrane filtration, obtains carboxylated graphene oxide after drying；
3) take 100mg carboxylated graphene oxide ultrasonic disperse and obtain spinning solution in 50mL N, N-dimethyl formyl, prepare graphene fiber finally by wet spinning.
Embodiment
5
Graphene fiber in embodiment 1～3 also can prepare as follows.
1) being added in 200mL deionized water by 100mg graphene oxide, ultrasonic disperse, after 1 hour, obtains finely dispersed graphene oxide water solution；
2) in finely dispersed graphene oxide water solution, add the mixing of 5g monoxone, under the conditions of then low whipping speed is 100 revs/min, mixed solution is heated to 60 DEG C, keep its reaction 3 hours, it is cooled to room temperature, with membrane filtration, obtains carboxylated graphene oxide after drying；
3) take 100mg carboxylated graphene oxide ultrasonic disperse and obtain spinning solution in 80mL N, N-dimethyl formyl, prepare graphene fiber finally by wet spinning.
Embodiment
6
Graphene fiber in embodiment 1～3 prepares also by following steps.
1) being added in 300mL deionized water by 100mg graphene oxide, ultrasonic disperse, after 2 hours, obtains finely dispersed graphene oxide water solution；
2) in finely dispersed graphene oxide water solution, add the mixing of 5g monoxone, under the conditions of then low whipping speed is 200 revs/min, mixed solution is heated to 70 DEG C, keep its reaction 2 hours, it is cooled to room temperature, with membrane filtration, obtains carboxylated graphene oxide after drying；
3) take 100mg carboxylated graphene oxide ultrasonic disperse and obtain spinning solution in 100mL N, N-dimethyl formyl, prepare graphene fiber finally by wet spinning.
Claims (4)
1. the preparation method of a graphene conductive composite fibre, it is characterised in that: include following preparation process:
(1) flaxen fiber is placed in soak at room temperature in pectinase solution；Then the flaxen fiber after processing continues to be immersed in immersion in chitosan aqueous solution, is dehydrated, dries；
(2) flaxen fiber that step (1) prepares is immersed in graphene dispersing solution, is subsequently placed in baking oven drying, obtains graphene conductive composite fibre；
Wherein, described graphene dispersing solution is carboxylated Graphene and N, the mixture of N-dimethyl formyl, carboxylated Graphene and N, and the mass volume ratio of N-dimethyl formyl is 100mg:(50～100mL).
The preparation method of graphene conductive composite fibre the most according to claim 1, it is characterised in that: the concentration of the pectinase solution described in step (1) is 10～50g/L, and soak time is 15～30 minutes；Described chitosan aqueous solution concentration is 10～20g/L, and soak time is 1～3 hour.
The preparation method of graphene conductive composite fibre the most according to claim 1, it is characterised in that: described flaxen fiber is 1g:(5～20mL with the mass volume ratio of graphene dispersing solution), soak time is 1～3 hour.
The preparation method of graphene conductive composite fibre the most according to claim 1, it is characterised in that: described carboxylated graphene fiber is prepared by following steps:
(1) adding graphene oxide in deionized water, the mass volume ratio of graphene oxide and deionized water is 1mg:(1～3mL), ultrasonic disperse 0.5～after 2 hours, obtain finely dispersed graphene oxide water solution；
(2) finely dispersed graphene oxide water solution is mixed with monoxone, described monoxone is 50:1 with the mass ratio of graphene oxide, then under the conditions of low whipping speed is 50～200 revs/min, mixed solution is heated to 60～80 DEG C, keep its reaction 0.5～3 hour, it is cooled to room temperature, with membrane filtration, obtains carboxylated graphene oxide after drying；
(3) by carboxylated graphene oxide ultrasonic disperse in N, N-dimethyl formyl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610469735.8A CN106012090A (en) | 2016-06-26 | 2016-06-26 | Preparation method of conductive graphene composite fibers |
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| CN201610469735.8A CN106012090A (en) | 2016-06-26 | 2016-06-26 | Preparation method of conductive graphene composite fibers |
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| CN106012090A true CN106012090A (en) | 2016-10-12 |
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| CN201610469735.8A Pending CN106012090A (en) | 2016-06-26 | 2016-06-26 | Preparation method of conductive graphene composite fibers |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109518496A (en) * | 2018-11-30 | 2019-03-26 | 河南健锋帽业有限公司 | A kind of colouring method of sodolin |
| WO2020064961A1 (en) * | 2018-09-27 | 2020-04-02 | Sanko Tekstil Isletmeleri San. Ve Tic. A.S. | A process for providing a textile with electrical conductivity properties |
| CN112176746A (en) * | 2020-09-30 | 2021-01-05 | 谷令纺织科技(常州)有限公司 | Preparation method of natural fiber graphene composite material |
| CN114541135A (en) * | 2022-02-23 | 2022-05-27 | 东华大学 | High-performance terahertz absorption composite fabric and preparation method thereof |
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| CN103820909A (en) * | 2014-02-18 | 2014-05-28 | 南京邮电大学 | Conductive yarn and production method thereof |
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- 2016-06-26 CN CN201610469735.8A patent/CN106012090A/en active Pending
Patent Citations (4)
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| CN103820909A (en) * | 2014-02-18 | 2014-05-28 | 南京邮电大学 | Conductive yarn and production method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020064961A1 (en) * | 2018-09-27 | 2020-04-02 | Sanko Tekstil Isletmeleri San. Ve Tic. A.S. | A process for providing a textile with electrical conductivity properties |
| CN112771225A (en) * | 2018-09-27 | 2021-05-07 | 尚科纺织企业工业及贸易公司 | Method for imparting conductivity to textiles |
| CN109518496A (en) * | 2018-11-30 | 2019-03-26 | 河南健锋帽业有限公司 | A kind of colouring method of sodolin |
| CN109518496B (en) * | 2018-11-30 | 2021-07-02 | 浙江九彩龙染织科技有限公司 | Dyeing method of linen fabric |
| CN112176746A (en) * | 2020-09-30 | 2021-01-05 | 谷令纺织科技(常州)有限公司 | Preparation method of natural fiber graphene composite material |
| CN112176746B (en) * | 2020-09-30 | 2022-05-06 | 常州森彩新材料科技有限公司 | Preparation method of natural fiber graphene composite material |
| CN114541135A (en) * | 2022-02-23 | 2022-05-27 | 东华大学 | High-performance terahertz absorption composite fabric and preparation method thereof |
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Application publication date: 20161012 |