CN108642884A - The preparation method and its resulting materials of a kind of painted graphite alkene fiber and application - Google Patents
The preparation method and its resulting materials of a kind of painted graphite alkene fiber and application Download PDFInfo
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- CN108642884A CN108642884A CN201810478931.0A CN201810478931A CN108642884A CN 108642884 A CN108642884 A CN 108642884A CN 201810478931 A CN201810478931 A CN 201810478931A CN 108642884 A CN108642884 A CN 108642884A
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- Prior art keywords
- fiber
- graphite alkene
- graphene
- graphene oxide
- preparation
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Classifications
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- 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
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
-
- 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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention discloses a kind of preparation method of painted graphite alkene fiber and its resulting materials and applications, and this approach includes the following steps：(1) graphene oxide dispersion is centrifuged, obtains graphene oxide spinning solution；(2) graphene oxide spinning solution is injected into the coagulating bath of rotation, wet graphene oxide fiber is obtained after standing；(3) graphene oxide fiber impregnation is restored in reducing agent solution, obtains graphene fiber；(4) graphene fiber is impregnated in white polymer waterborne polyurethane solutions, is cured, repeated this step, obtain white graphite alkene fiber；(5) graphene fiber of white is impregnated in the aqueous polyurethane solution of pigment, is cured, repeat this step to get to the painted graphite alkene fiber.Compared with prior art, equipment needed for the method for the present invention is simple, at low cost, and technique is controllable, and obtained painted graphite alkene fiber has preferable intensity and electric conductivity, suitable for the wearable product of weaving.
Description
Technical field
The present invention relates to a kind of preparation method of painted graphite alkene fiber and its resulting materials and applications, belong to graphite fibre
Preparing technical field.
Background technology
Graphene is as a kind of novel two-dimentional carbon nanomaterial, the stringent two-dimensional structure of cellular carbon atom arrangement
And abundant excellent physical characteristic (higher carrier mobility, the specific surface area of super large, excellent mechanical performance and chemistry
Stability), once it is found that having started huge research boom in physics and materialogy field rapidly.Using wet spinning
Spinning derives the intrinsic property of graphene into the one-dimensional graphene fiber of macroscopic view.However due to graphite inside graphene fiber
A large amount of stackings of alkene piece and the big conjugation of graphene, graphene fiber show the black with metallic luster.
At present to the research in terms of the few colors to graphene fiber of research of graphene fiber function, graphene is original
Black in conductive fiber application aspect, using there is great limitation especially in terms of intelligent conductive spinning product color.And it is colored
Graphene fiber in terms of research can make up the single deficiency of graphene fiber color, greatly improve it in textile
On application value.
Invention content
Goal of the invention：In view of the above technical problems, it is an object of the invention to propose a kind of system of painted graphite alkene fiber
Painted graphite alkene fiber obtained by Preparation Method and this method.
Technical solution：The present invention adopts the following technical scheme that：
A kind of preparation method of painted graphite alkene fiber, includes the following steps：
(1) graphene oxide dispersion is centrifuged, obtains graphene oxide spinning solution；
(2) graphene oxide spinning solution is injected into the coagulating bath of rotation, it is fine that wet graphene oxide is obtained after standing
Dimension spontaneously dries, obtains graphene oxide fiber；
(3) the graphene oxide fiber impregnation that step (2) obtains is restored in reducing agent solution, is then cooled down, taken out,
After being impregnated in the mixed solution of second alcohol and water, is spontaneously dried after fiber is taken out, obtain graphene fiber；
(4) graphene fiber is impregnated in white polymer waterborne polyurethane solutions, is cured, repeated this step, obtain
White graphite alkene fiber；
(5) graphene fiber of white is impregnated in the aqueous polyurethane solution of pigment, is cured, repeat this step, i.e.,
Obtain the painted graphite alkene fiber.
As preferred：
90min is centrifuged under the rotating speed that the condition centrifuged described in step (1) is 11000rpm, obtains graphene oxide spinning
Liquid.
Coagulating bath described in step (2), solute are the calcium chloride of mass fraction 5%, and solvent is that volume ratio is 1:1 to 3:
The mixed solution of 1 second alcohol and water.
The method restored in reducing agent solution described in step (3) is：It is immersed in 80-90 DEG C of HI solution and restores
10-12 hours.
White polymer waterborne polyurethane solutions described in step (4) are the mixed of titanium dioxide and polymer waterborne polyurethane
Close solution.
Dip time 5-10s described in step (4), condition of cure are：Cure 30-60s at 130 DEG C.
In the aqueous polyurethane solution of pigment described in step (5), pigment is pigment red 112, pigment yellow 83 and pigment blue
15:One kind in 3, mass fraction 2%.
Dip time 5-10s described in step (5), condition of cure are：Cure 30-60s at 130 DEG C.
Painted graphite alkene fiber obtained by preparation method of the present invention, the graphene fiber have three layers structure, packet
Core layer graphene fiber, the white polymer waterborne layer of polyurethane outside graphene fiber layer are included, it is outermost color aqueous poly-
Urethane layer.With preferable intensity and electric conductivity, suitable for the wearable product of weaving.
The present invention prepares the graphene fiber with nucleocapsid mechanism by the way of dip-coating.This shell structure is being played to core
While core graphite alkene fiber protective effect, graphene fiber lovely luster, the appearance of various colors are also assigned, graphene is promoted
Application prospect of the fiber on the conductive wearable textile of intelligence.
Technique effect：Compared with prior art, equipment needed for the method for the present invention is simple, at low cost, and technique is controllable, and made
The painted graphite alkene fiber obtained has preferable intensity and electric conductivity, suitable for the wearable product of weaving.
Description of the drawings
Fig. 1 is the pictorial diagram of painted graphite alkene fiber prepared by the present invention；
Fig. 2 is painted graphite alkene fibre structure schematic diagram prepared by the present invention；
Fig. 3 is the cross-sectional scans electron microscope of painted graphite alkene fiber prepared by the present invention；
Fig. 4 is the linear VA characteristic curve figure of painted graphite alkene fiber prepared by the present invention；
Fig. 5 is the electric conductivity test chart of the sandwich layer and shell of painted graphite alkene fiber prepared by the present invention；
Fig. 6 is that painted graphite alkene fiber prepared by the present invention changes in different bending angles and the electric conductivity under bending number
Figure.
Specific implementation mode
Technical solutions according to the invention are further described in detail below by specific embodiment, but it is necessary to
It points out that following embodiment is served only for the description to invention content, does not constitute limiting the scope of the invention.
Embodiment 1：
(1) graphene oxide dispersion is centrifuged into 60min under the rotating speed of 11000rpm, obtains graphene oxide spinning
Liquid；
(2) graphene oxide spinning solution is injected into the bore of 0.7mm in the coagulating bath of rotation with syringe, is stood
Wet graphene oxide fiber is obtained after 30min, is spontaneously dried at ambient temperature in the form of single, is obtained graphene oxide
Fiber；The coagulating bath, solute are the calcium chloride of mass fraction 5%, and solvent is that volume ratio is 1:The mixing of 1 second alcohol and water
Solution；
(3) the graphene oxide fiber impregnation for obtaining step (2) restores 12 hours in 90 DEG C of HI solution, then cold
But in solvent be volume ratio it is 1 to taking out after room temperature:1h is impregnated in the mixed solution of 1 second alcohol and water, after fiber is taken out certainly
It is so dry, obtain graphene fiber；
(4) graphene fiber is impregnated into 5s in white polymer waterborne polyurethane solutions, cures 30s at 130 DEG C, weight
Multiple this step 8 time, obtains white graphite alkene fiber；
(5) graphene fiber of white is immersed in the aqueous polyurethane for the pigment red 112 that mass fraction is 2% and is impregnated
5s cures 60s at 130 DEG C, repeats this step 2 time, obtains red graphene fiber.
By above step, the red graphene fiber with nucleocapsid, fibre length 1-12cm, electric conductivity are obtained
More than 15000S/m, tensile strength is more than 500MPa.
Embodiment 2：
(1) graphene oxide dispersion is centrifuged into 90min under the rotating speed of 10000rpm, obtains graphene oxide spinning
Liquid；
(2) graphene oxide spinning solution is injected into the bore of 0.7mm in the coagulating bath of rotation with syringe, is stood
Wet graphene oxide fiber is obtained after 30min, is spontaneously dried at ambient temperature in the form of single, is obtained graphene oxide
Fiber；The coagulating bath, solute are the calcium chloride of mass fraction 5%, and solvent is that volume ratio is 2:The mixing of 1 second alcohol and water
Solution；
(3) the graphene oxide fiber impregnation for obtaining step (2) restores 12 hours in 80 DEG C of HI solution, then cold
But in solvent be volume ratio it is 2 to taking out after room temperature:1h is impregnated in the mixed solution of 1 second alcohol and water, after fiber is taken out certainly
It is so dry, obtain graphene fiber；
(4) graphene fiber is impregnated into 10s in white polymer waterborne polyurethane solutions, cures 50s at 130 DEG C,
This step 8 time is repeated, white graphite alkene fiber is obtained；
(5) graphene fiber of white is immersed in the aqueous polyurethane for the pigment yellow 83 that mass fraction is 2% and is impregnated
10s cures 50s at 130 DEG C, repeats this step 2 time, obtains yellow graphene fiber.
By above step, the yellow graphene fiber with nucleocapsid, fibre length 1-12cm, electric conductivity are obtained
More than 15000S/m, tensile strength is more than 500MPa.
Embodiment 3：
(1) graphene oxide dispersion is centrifuged into 90min under the rotating speed of 11000rpm, obtains graphene oxide spinning
Liquid；
(2) graphene oxide spinning solution is injected into the bore of 0.7mm in the coagulating bath of rotation with syringe, is stood
Wet graphene oxide fiber is obtained after 30min, is spontaneously dried at ambient temperature in the form of single, is obtained graphene oxide
Fiber；The coagulating bath, solute are the calcium chloride of mass fraction 5%, and solvent is that volume ratio is 3:The mixing of 1 second alcohol and water
Solution；
(3) the graphene oxide fiber impregnation for obtaining step (2) restores 10 hours in 90 DEG C of HI solution, then cold
But in solvent be volume ratio it is 1.5 to taking out after room temperature:1h is impregnated in the mixed solution of 1 second alcohol and water, after fiber is taken out
It spontaneously dries, obtains graphene fiber；
(4) graphene fiber is impregnated into 8s in white polymer waterborne polyurethane solutions, cures 50s at 130 DEG C, weight
Multiple this step 8 time, obtains white graphite alkene fiber；
(5) graphene fiber of white is immersed in the pigment blue 15 that mass fraction is 2%:It is soaked in 3 aqueous polyurethane
Stain 9s cures 40s at 130 DEG C, repeats this step 2 time, obtains blue graphene fiber.
By above step, the blue graphene fiber with nucleocapsid, fibre length 1-12cm, electric conductivity are obtained
More than 15000S/m, tensile strength is more than 500Mpa.
Gained painted graphite alkene product testing of the invention：
As shown in Figure 1, painted graphite alkene fiber has bright smooth surface.As shown in Figures 2 and 3, a kind of colored stone
Black alkene fiber, the fiber are the white macromolecule outside three-decker, including core layer graphene fiber, graphene fiber layer
Aqueous polyurethane layer, outermost color aqueous layer of polyurethane, length are 1-12 centimetres.The graphene fiber and shell of central core
Fiber formed coaxial configuration, can be used as the fibrous capacitor of parallel column or wound form.Painted graphite alkene fiber
Shell even compact so that the black of graphene fiber is completely covered, and provides protection for the graphene fiber of internal layer
Effect.
The VA characteristic curve of painted graphite alkene fiber prepared by this method is as shown in figure 4, the conductivity of fiber is
15600S/m；With reference to Fig. 5, the inner fiber of painted graphite alkene fiber prepared by this method is conductive, outer layer shell structure tool
There is insulating properties.
As shown in fig. 6, this figure is electric conductivity variation of the painted graphite alkene fiber under different bending angles and bending number
Figure.Fiber electric conductivity under different bending angles does not have significant change, and after 500 bendings test, fiber is conductive
Property is basically unchanged.
Claims (10)
1. a kind of preparation method of painted graphite alkene fiber, which is characterized in that include the following steps：
(1) graphene oxide dispersion is centrifuged, obtains graphene oxide spinning solution；
(2) graphene oxide spinning solution is injected into the coagulating bath of rotation, wet graphene oxide fiber is obtained after standing, from
It is so dry, obtain graphene oxide fiber；
(3) the graphene oxide fiber impregnation that step (2) obtains is restored in reducing agent solution, is then cooled down, taken out, in second
After being impregnated in the mixed solution of alcohol and water, is spontaneously dried after fiber is taken out, obtain graphene fiber；
(4) graphene fiber is impregnated in white polymer waterborne polyurethane solutions, is cured, repeated this step, obtain white
Graphene fiber；
(5) by white graphene fiber impregnated in the aqueous polyurethane solution of pigment, cure, repeat this step to get to
The painted graphite alkene fiber.
2. a kind of preparation method of painted graphite alkene fiber according to claim 1, which is characterized in that described in step (1)
90min is centrifuged under the rotating speed that the condition of centrifugation is 11000rpm, obtains graphene oxide spinning solution.
3. a kind of preparation method of painted graphite alkene fiber according to claim 1, which is characterized in that described in step (2)
Coagulating bath, solute are the calcium chloride of mass fraction 5%, and solvent is that volume ratio is 1:1 to 3:The mixing of 1 second alcohol and water is molten
Liquid.
4. a kind of preparation method of painted graphite alkene fiber according to claim 1, which is characterized in that described in step (3)
The method restored in reducing agent solution is：It is immersed in 80-90 DEG C of HI solution and restores 10-12 hours.
5. a kind of preparation method of painted graphite alkene fiber according to claim 1, which is characterized in that described in step (4)
White polymer waterborne polyurethane solutions are the mixed solution of titanium dioxide and aqueous polyurethane.
6. a kind of preparation method of painted graphite alkene fiber according to claim 1, which is characterized in that described in step (4)
Dip time 5-10s, condition of cure are：Cure 30-60s at 130 DEG C.
7. a kind of preparation method of painted graphite alkene fiber according to claim 1, which is characterized in that described in step (5)
In the aqueous polyurethane solution of color pigment, pigment is pigment red 112, pigment yellow 83 and pigment blue 15:One kind in 3, quality
Score is 2%.
8. a kind of preparation method of painted graphite alkene fiber according to claim 1, which is characterized in that described in step (5)
Dip time 5-10s, condition of cure are：Cure 30-60s at 130 DEG C.
9. the painted graphite alkene fiber obtained by any one of the claim 1-8 preparation methods, which is characterized in that the stone
Black alkene fiber haves three layers the white polymer waterborne polyurethane outside structure, including core layer graphene fiber, graphene fiber layer
Layer, outermost color aqueous layer of polyurethane.
10. application of the painted graphite alkene fiber described in claim 9 in the wearable product for preparing weaving.
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| CN201810478931.0A CN108642884A (en) | 2018-05-18 | 2018-05-18 | The preparation method and its resulting materials of a kind of painted graphite alkene fiber and application |
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| CN201810478931.0A CN108642884A (en) | 2018-05-18 | 2018-05-18 | The preparation method and its resulting materials of a kind of painted graphite alkene fiber and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112647159A (en) * | 2019-10-10 | 2021-04-13 | 中国科学技术大学 | Graphene-based micron rod with multi-capsule-hole structure and preparation method thereof |
| CN114369882A (en) * | 2022-02-24 | 2022-04-19 | 江苏省特种设备安全监督检验研究院 | Self-coloring graphene fiber and preparation method and application thereof |
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| CN106868885A (en) * | 2017-03-16 | 2017-06-20 | 江苏工程职业技术学院 | A kind of processing method of polyamide fibre Graphene white dipped gloves |
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| CN112647159A (en) * | 2019-10-10 | 2021-04-13 | 中国科学技术大学 | Graphene-based micron rod with multi-capsule-hole structure and preparation method thereof |
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Application publication date: 20181012 |