CN109295699A - A method of improving graphene finish fabric electric conductivity, conductivity uniformity and durability - Google Patents
A method of improving graphene finish fabric electric conductivity, conductivity uniformity and durability Download PDFInfo
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- CN109295699A CN109295699A CN201811155977.5A CN201811155977A CN109295699A CN 109295699 A CN109295699 A CN 109295699A CN 201811155977 A CN201811155977 A CN 201811155977A CN 109295699 A CN109295699 A CN 109295699A
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- graphene oxide
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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
- 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
Abstract
The invention discloses a kind of raising graphene finish fabric electric conductivity, the method of conductivity uniformity and durability, graphene oxide is set to be adsorbed in fabric surface using infusion process, then directly reducing agent is added under the conditions of Ultrasonic Heating in impregnation liquid in not drain, make the graphene oxide in fabric surface and treatment fluid while being transformed into redox graphene, the partial oxidation of graphite alkene in reduction process in solution is adsorbed onto again fabric surface because of the π-π on fabric between redox graphene simultaneously, the removing that ultrasonication promotes graphene oxide improves durability, promote graphene oxide in the more uniform uniformity for improving conduction of the distribution of fabric surface simultaneously.The preparation of durability and uniformity conductive fabric and the recycling of residual oxidization graphene are realized by means of the present invention, which can be used for the wearable clothing fabric of intelligence, can also be used for the multiple fields such as flexible electronic device, health care, smart motion.
Description
Technical field
The invention belongs to dyeing and finishing technique fields, and in particular to a kind of raising graphene finish fabric electric conductivity, it is conductive uniformly
The method of property and durability.
Background technique
Intelligence weaving dress ornament is collection sensing, servo, communication, memory, adaptive, selfreparing, the confession function such as energy and study
The fiber assembly device of energy can be perceived external drive and be made a response by program, in the micron-scale the surface and centre of fiber
Nanometer or submicrometer structure are had to realize its function.Wearable device based on fibrous material is based on fibrous material
Flexible electronic, photon technology, the intelligent textile technology that external drive can be perceived by program and changed.It arranges to assign by conduction and spin
The wearable characteristic of fabric is the hot spot of Recent study, and wherein the wearable textile of graphene compliant conductive is even more and is widely noticed.
In graphene conductive arrangement, graphene directly affects the conductivity uniformity of fabric in the deposition uniformity of fabric surface, and
The conductivity uniformity of fabric directly affects the wearable intelligent characteristic of fabric, therefore the conductivity uniformity of graphene conductive textile
It is the subject under discussion for being worth paying special attention to.
104328653 B of patent of invention CN discloses a kind of graphene oxide derivative for multifunctional finish of textiles
Method, by by fabric oxide impregnation Graphene derivative aqueous solution, then will be restored after fabric drying, make fabric surface
One layer of redox graphene derivative is covered, is then repeated the above steps, the conduction, uvioresistant, water repellent of excellent effect are obtained
Multifunctional fabric.Document (the good of Cao's machine is based on the preparation of graphene oxide compliant conductive fibrous material and performance [D] Southern Yangtze University,
2017.) disclose it is a kind of processing is impregnated and padded to silk using graphene oxide, by repeatedly impregnating or padding processing
The fabric of adsorption and oxidation graphene is dried afterwards, then the fabric of the adsorption and oxidation graphene of drying is impregnated into containing sodium hydrosulfite
Graphene oxide is restored in solution, the method that fabric electric conductivity can be assigned.It has no and fabric is impregnated at present in graphene oxide
Conduction increases ultrasound to improve fabric electric conductivity, conductivity uniformity and durability during arranging, and has impregnated straight without drain
It connects in graphene oxide raffinate to the graphene oxide in fabric surface and raffinate while restoring, make the graphite oxide in raffinate
Alkene second adsorption is to fabric surface, and the graphene oxide recoverable in raffinate, the method for reducing wastewater treatment burden.
Summary of the invention
It is poor the technical problem to be solved by the present invention is to be directed to the uniformity of current graphene oxide dip finishing fabric,
The graphene oxide that has impregnated remains problem to be treated, after providing a kind of fabric ultrasonic immersing processing graphene oxide solution
The method of not drain ultrasound reduction directly in graphene oxide solution, realizes in the graphene oxide and solution of fabric surface
Graphene oxide restore simultaneously, and the graphene oxide in solution can also second adsorption to fabric surface improve leading for fabric
Electrically, whole ultrasonic treatment improves the conductivity uniformity and conduction durability of fabric.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: 0.2~10g/L graphene oxide water solution is prepared, in 0~30 DEG C of ultrasound
Under the conditions of 10~60min of stir process, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 0~30 DEG C of sonic oscillation handle 20~120min, then be warming up to 70~100 DEG C with the rate of 0.5~3 DEG C/min, then
Put into the reducing agent of 2~10g/L, 10~90min of isothermal holding, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Contain the hydrophilic radicals such as carboxyl, hydroxyl, epoxy group and carbonyl in the step (1) in graphene oxide molecule,
And the preparation process of graphene oxide uses ultrasound, the single layer rate of graphene oxide can be improved in ultrasound.
Ultrasonic purpose is to make graphene oxide sufficiently dissolution dispersion in aqueous solution in the step (2).
The hydrophilic radical of graphene oxide can be with the hydroxyl, amino or carboxyl isopolarity base of fabric in the step (3)
Group is with the combination of hydrogen bond, Van der Waals force or ionic bond, so that graphene oxide be made more securely to be bonded to fabric surface.
Reducing agent is one of sodium hydrosulfite, rongalite, thiourea dioxide, hydrazine hydrate or a variety of in the step (3).
Graphene oxide dipping is adsorbed onto the reduction of fabric surface and graphene oxide in same place in the step (3)
It is carried out in reason bath.
Also promote while fabric surface graphene oxide restores in the step (3) graphene oxide in solution also
It is former.
In the step (3) in solution in graphene oxide reduction process again understand some redox graphene due to
Strong π-π the active force between graphene macromolecular and be adsorbed onto fabric surface, further improve the electric conductivity of fabric.
The absorption, reduction of graphene oxide carry out under ultrasound condition in the step (3), and ultrasound condition not only promotes
The removing of graphene oxide, improves the durability of fabric conduction, and promotes graphene oxide and redox graphene
In the distribution of fabric surface, finally redox graphene is made to be evenly distributed in fabric surface, to improve fabric conduction
Uniformity.
In the step (4) redox graphene filtered, wash after recycled, reduce wastewater treatment difficulty,
Cost is saved.
Technical principle of the invention: by preparing graphene oxide water solution, adsorb graphene oxide using infusion process
In fabric surface, make graphene oxide and fabric with ionic bond, hydrogen bond or Van der Waals force in conjunction with, then not drain is directly impregnating
Reducing agent is added under the conditions of Ultrasonic Heating in treatment fluid, make the graphene oxide in fabric surface and treatment fluid while being transformed into
Redox graphene, at the same the partial oxidation of graphite alkene in reduction process in solution because with redox graphene on fabric it
Between π-π and be adsorbed onto fabric surface again, the removing that ultrasonication not only promotes graphene oxide improves durable
Property, and promote graphene oxide in the more uniform uniformity for improving conduction of the distribution of fabric surface, not drain also original place
Reason not only restored the graphene oxide of fabric surface, but also the graphene oxide in solution is promoted to recycle.
Beneficial effects of the present invention: not drain directly exists after fabric ultrasonic immersing processing graphene oxide solution in the present invention
The method of ultrasound reduction in graphene oxide solution, reduces the process of the fabric drying of oxide impregnation graphene, saves
The energy realizes the graphene oxide in the graphene oxide and solution of fabric surface while restoring, and the oxidation stone in solution
Black alkene can also second adsorption the electric conductivity of fabric is improved to fabric surface, and whole ultrasonic treatment improves the conduction of fabric
Even property and conductive durability, can also finally be such that the graphene oxide in raffinate recycles, and reduce wastewater treatment burden.The present invention
Technical solution simple process it is feasible, to raw material, auxiliary agent, fabric without particular/special requirement, set using conventional dyeing apparatus and ultrasound
It is standby to achieve that large-scale production, it has broad application prospects.Realize that durability and uniformity are conductive by means of the present invention
The preparation of fabric and the recycling of residual oxidization graphene, the fabric can be used for the wearable clothing fabric of intelligence, can also be used for flexibility
The multiple fields such as electronic device, health care, smart motion.
Specific embodiment
Combined with specific embodiments below, the present invention will be further described.It should be understood that following embodiment is merely to illustrate this
The person skilled in the art of the range of invention and is not intended to limit the present invention, the field can make one according to the content of foregoing invention
A little nonessential modifications and adaptations.
A kind of raising graphene finish fabric electric conductivity of the invention, the method for conductivity uniformity and durability, step is such as
Under:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: 0.2~10g/L graphene oxide water solution is prepared, in 0~30 DEG C of ultrasound
Under the conditions of 10~60min of stir process, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 0~30 DEG C of sonic oscillation handle 20~120min, then be warming up to 70~100 DEG C with the rate of 0.5~3 DEG C/min, then
Put into the reducing agent of 2~10g/L, 10~90min of isothermal holding, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 1
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 5g/L graphene oxide water solution, stirred under 0 DEG C of ultrasound condition
10min is handled, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 20 DEG C of sonic oscillations handle 40min, then be warming up to 100 DEG C with the rate of 3 DEG C/min, then put into 10g/L reducing agent and protect
Dangerous powder, isothermal holding 10min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 2
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 0.2g/L graphene oxide water solution, stirred under 0 DEG C of ultrasound condition
Processing 10min is mixed, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 0 DEG C of sonic oscillation handle 20min, then be warming up to 70 DEG C with the rate of 0.5 DEG C/min, it is white then to put into 2g/L reducing agent carving
Powder, isothermal holding 90min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 3
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 10g/L graphene oxide water solution, stirred under 30 DEG C of ultrasound conditions
Processing 60min is mixed, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 30 DEG C of sonic oscillations handle 120min, then be warming up to 100 DEG C with the rate of 3 DEG C/min, then put into 10g/L reducing agent two
Aminoiminomethanesulfonic acid, isothermal holding 10min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 4
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 2g/L graphene oxide water solution, stirred under 10 DEG C of ultrasound conditions
30min is handled, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 20 DEG C of sonic oscillations handle 30min, then be warming up to 80 DEG C with the rate of 2 DEG C/min, then put into the hydration of 4g/L reducing agent
Hydrazine, isothermal holding 50min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 5
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 6g/L graphene oxide water solution, stirred under 20 DEG C of ultrasound conditions
50min is handled, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 10 DEG C of sonic oscillations handle 60min, then be warming up to 90 DEG C with the rate of 2 DEG C/min, then put into 6g/L reducing agent (3g/L
Sodium hydrosulfite, 3g/L rongalite), isothermal holding 60min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 6
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 1g/L graphene oxide water solution, stirred under 20 DEG C of ultrasound conditions
20min is handled, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 20 DEG C of sonic oscillations handle 80min, then be warming up to 70 DEG C with the rate of 0.5 DEG C/min, then put into 3g/L reducing agent carving
White powder, isothermal holding 40min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 7
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 0.8g/L graphene oxide water solution, stirred under 10 DEG C of ultrasound conditions
Processing 20min is mixed, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 20 DEG C of sonic oscillations handle 80min, then be warming up to 90 DEG C with the rate of 2 DEG C/min, then put into 5g/L reducing agent (2g/L
Sodium hydrosulfite, 3g/L hydrazine hydrate), isothermal holding 90min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Embodiment 8
A method of graphene finish fabric electric conductivity, conductivity uniformity and durability being improved, steps are as follows:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide (GO),
The graphene oxide precipitating of 4000~10000r/min is left and taken in centrifugation, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: preparing 1g/L graphene oxide water solution, stirred under 5 DEG C of ultrasound conditions
40min is handled, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by (2)
In in 2 DEG C of sonic oscillations handle 40min, then be warming up to 95 DEG C with the rate of 1.5 DEG C/min, then put into the sodium hydrosulfite of 2g/L,
Isothermal holding 40min, sufficiently washing, drying that processing terminate；
(4) in solution redox graphene recycling: after fabric is taken out, solid suspension in solution filtered,
The redox graphene of high-quality can be obtained in washing, freeze-drying.
Implementation result of the invention
After Examples 1 to 8 is handled, fabric is tested as follows, test result is shown in Table 1.
1) fastness to washing measures
Experimental test is carried out according to GB/T3921-2008 " textile color stability fastness to soaping ".
2) conducting performance test
Fabric surface resistance measures in (Suzhou Electronics Co., Ltd. of Tontru) on SZT-2A four-point probe.
3) conductivity uniformity is tested
10 points are arbitrarily taken on the fabric, measure its sheet resistance value, with the average value of formula (1) gauging surface resistanceThen each point sheet resistance value is calculated to the standard deviation S of average value with formula (2)r。
Standard deviation SrNumerical value is smaller, indicates that conductivity uniformity is better.
The test result of the implementation fabric of table 1
Implement sample in table 1 and refer to the fabric sample obtained according to embodiment, comparative sample refer to do not apply be ultrasonically treated it is other
Process conditions obtained sample consistent with embodiment, as shown in Table 1, technical solution provided by the present invention can assign textile
Excellent electric conductivity, excellent conductivity uniformity and durability, electric conductivity, conductivity uniformity are after washing 50 times almost without change
Change.It can be seen that conductive fabric electric conductivity produced by the present invention is excellent, and there is outstanding conductivity uniformity and washability.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (5)
1. a kind of raising graphene finish fabric electric conductivity, the method for conductivity uniformity and durability, it is characterised in that step is such as
Under:
(1) it prepares graphene oxide: taking ultrasonic Hummers method, using graphite as raw material, prepare graphene oxide, centrifugation is left and taken
The graphene oxide of 4000~10000 r/min precipitates, and freeze-drying obtains evenly dispersed graphene oxide；
(2) it prepares graphene oxide water solution: 0.2~10 g/L graphene oxide water solution is prepared, in 0~30 DEG C of ultrasound condition
Lower 10~60 min of stir process, for use；
(3) graphene oxide is applied to fabric surface and restored: fabric is immersed into graphene oxide water solution obtained by step (2)
In in 0~30 DEG C of sonic oscillation handle 20~120min, then be warming up to 70~100 DEG C with the rate of 0.5~3 DEG C/min, then
Put into the reducing agent of 2~10g/L, 10~90min of isothermal holding, sufficiently washing, drying that processing terminate.
2. raising graphene finish fabric electric conductivity, the method for conductivity uniformity and durability according to claim 1,
It is characterized in that: containing carboxyl, hydroxyl, epoxy group and carbonyl, and graphene oxide in the step (1) in graphene oxide molecule
Preparation process use ultrasound.
3. raising graphene finish fabric electric conductivity, the method for conductivity uniformity and durability according to claim 1,
Be characterized in that: reducing agent is one of sodium hydrosulfite, rongalite, thiourea dioxide, hydrazine hydrate or a variety of in the step (3).
4. raising graphene finish fabric electric conductivity, the method for conductivity uniformity and durability according to claim 1,
Be characterized in that: graphene oxide dipping is adsorbed onto the reduction of fabric surface and graphene oxide same in the step (3)
It is carried out in processing bath.
5. raising graphene finish fabric electric conductivity, the method for conductivity uniformity and durability according to claim 1,
Be characterized in that: after taking out fabric in the step (3), the solid suspension in solution can be obtained through suction filtration, washing, freeze-drying
To the redox graphene of high-quality.
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Application publication date: 20190201 |
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