CN104313872B - A kind of preparation method of graphene/polyaniline covalent bond compliant conductive fabric - Google Patents
A kind of preparation method of graphene/polyaniline covalent bond compliant conductive fabric Download PDFInfo
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- CN104313872B CN104313872B CN201410554346.6A CN201410554346A CN104313872B CN 104313872 B CN104313872 B CN 104313872B CN 201410554346 A CN201410554346 A CN 201410554346A CN 104313872 B CN104313872 B CN 104313872B
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Abstract
The preparation method that the invention discloses a kind of graphene/polyaniline covalent bond compliant conductive fabric, belongs to technical field of textile chemistry. The present invention reduces after being first applied on fabric by the product of graphene oxide or derivatives thereof Yu p-phenylenediamine, make above-mentioned fabrics adsorption of aniline monomer again, then make aniline monomer in-situ polymerization on fabric become polyaniline and be combined with Graphene formation covalent bond. The method obtains Graphene and the covalently bound conductive layer of polyaniline at fabric face, improves the stability of conductive layer, it is thus achieved that the conductive fabric of excellent effect. The method is applicable to conventional fabric such as the natural fibers such as cotton, Pilus Caprae seu Ovis, silkworm silk, the synthetic fibers such as terylene, chinlon, acrylon, and the conduction of the blending of above-mentioned fabrics or intertexture arranges, prepared function fabric can be applicable to the fields such as health care, intelligence sensor, dislocation generation, military affairs.
Description
Technical field
The invention belongs to technical field of textile chemistry, relate to a kind of method adopting Graphene or derivatives thereof and conductive polymer polymer covalent bond certainly to prepare compliant conductive fabric.
Background technology
Conductive fabric is as a kind of functional fabric, and it is with a wide range of applications in fields such as flexible electronic device, intellectual material, novel solar batteries. Blending and coating are the methods of the textile material of exploitation conduction the earliest, both approaches processing is simple, conduction is uniform, but finish fabric flexible not, the conductive fabric that particularly prepared by coating, in taking process, run into stronger stretching or folding can make coating cracking. Therefore, form fexible film and conductive polymer polymer with Graphene at fabric face and cause the attention of people at the conduction method for sorting that fabric face carries out being polymerized.
Graphene is to exist with the cellular many hexagonal structures form of monolayer, and owing to carbon atom is connected by stable covalent bond, therefore Graphene has superpower electric conductivity. But simple graphene conductive fabric, it is necessary to after making to cover equably on fabric the Graphene of q.s, fabric just has good electric conductivity and conduction uniformity; Simple polyaniline conductive fabric, there is also thermostability less stable, and electric conductivity is not as strong problem. The present invention first will prepare the homogeneous solution system of graphene oxide or derivatives thereof, it is therefore an objective in order to prevent the gathering of Graphene in subsequent reactions process; Be subsequently adding p-phenylenediamine so as to graphene oxide generation covalent reaction, fabric is impregnated the aqueous solution of p-phenylenediamine grafted graphene oxide or derivatives thereof again, makes fabric carry out after fully adsorbing p-phenylenediamine grafted graphene oxide or derivatives thereof drying, reducing; Finally adopt the method carrying out in-situ polymerization aniline or derivatives thereof on fabric, prepare Graphene and the covalently bound compliant conductive fabric of polyaniline. Being combined owing to Graphene defines covalent bond with polyaniline, the fabric washability prepared is good, electric conductivity is high.
Summary of the invention
The method that it is an object of the invention to adopt self assembly, is applied on fabric by Graphene and derivant thereof, conductive polymer polymer, makes fabric obtain high conduction performance.
The present invention adopts the following technical scheme that
1 adopt p-phenylenediamine grafted graphene oxide, then to fabric dipping and reduction treatment, and with conductive polymer polymer monomer covalent bond, prepare washable graphene/polyaniline covalent bond compliant conductive fabric.
P-phenylenediamine grafted graphene oxide described in 2 adopts following processing step:
(1) by the anion surfactant of 0.01��0.5 mass parts, the sulphuric acid of 0.05��0.4 mass parts, join in the graphene oxide or derivatives thereof of 0.05��1 mass parts, at 20��60 DEG C, ultrasonic reaction 0.5��2h under 300-1000W power, obtain the homogeneous mixture solotion of graphene oxide or derivatives thereof and anion surfactant;
(2) by the p-phenylenediamine of 0.1��2 mass parts, the thionyl chloride of 0.01��1 mass parts, add in the solution of (1) gained, under the protection of nitrogen, react 1��6h in 40��80 DEG C, obtain p-phenylenediamine grafted graphene oxide or derivatives thereof;
Described graphene oxide or derivatives thereof is at least one in graphene oxide, carboxylated graphene oxide, sulfonic group graphene oxide;
Described anion surfactant is at least one in alkylsulfonate, alkylbenzenesulfonate, alkyl carboxylate, alkylbenzene carboxylates, alkylnaphthalene sulfonate, alkylnaphthalene carboxylate, alkyl-anthraquinone sulfonate, alkyl-anthraquinone carboxylate.
Fabric dipping and reduction treatment described in 3 adopt following processing step:
Fabric is impregnated in the solution of p-phenylenediamine grafted graphene oxide or derivatives thereof gained, dipping temperature 20��50 DEG C, dip time 0.5��2h, again by fabric in 50��80 DEG C of drying 0.5��5h, then reduce drying fabric in the reductant solution of 1��10g/L, reduction temperature 50��100 DEG C, recovery time 0.5��6h, finally washing, drying, obtain covering the fabric of p-phenylenediamine grafting redox graphene or derivatives thereof;
Described reducing agent is at least one in sodium dithionite, sodium sulfite, glucose, chitosan, vitamin C, hydrazine hydrate, sodium borohydride.
Following processing step is adopted with conductive polymer polymer monomer covalent bond described in 4:
The fabric of gained is impregnated into containing in 0.02��1mol/L conductive polymer polymer monomer and 0.02��1mol/L acid solution, dipping temperature 0��40 DEG C, dip time 0.5��24h, being subsequently adding initiator makes polymer monomer aggregate into conductive polymer polymer, obtains graphene/polyaniline covalent bond compliant conductive fabric;
Described conductive polymer polymer monomer is at least one in aniline, p-aminobenzene sulfonic acid, metanilic acid.
The invention has the beneficial effects as follows: Graphene and high score conducting polymer are applied to fabric face in covalently bound mode, technical scheme is simple, be easy to operation, to equipment without particular/special requirement, utilize conventional equipment for dyeing and finishing just can carry out large-scale production, have broad application prospects.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
A kind of preparation method of graphene/polyaniline covalent bond compliant conductive fabric, its process is as follows:
(1) homogeneous mixture solotion of graphene oxide and anionic surfactant is prepared: by the anion surfactant of 0.2 mass parts, the sulphuric acid of 0.1 mass parts, join in the graphene oxide of 0.4 mass parts, at 40 DEG C, ultrasonic reaction 1h under 800W power, obtain the homogeneous mixture solotion of graphene oxide or derivatives thereof and anion surfactant;
(2) p-phenylenediamine grafted graphene oxide or derivatives thereof: by the p-phenylenediamine of 0.12 mass parts, the thionyl chloride of 0.06 mass parts, add in the solution of (1) gained, under the protection of nitrogen, react 4h in 50 DEG C, obtain p-phenylenediamine grafted graphene oxide or derivatives thereof;
(3) fabric of p-phenylenediamine grafting redox graphene is prepared: be impregnated into by fabric in the solution of (2) gained, dipping temperature 30 DEG C, dip time 1h, again by fabric in 60 DEG C of drying 3h, then reduce drying fabric in the hydrogensulfite solution of 5g/L, reduction temperature 90 DEG C, recovery time 0.5h, finally washing, drying, obtain covering the fabric of p-phenylenediamine grafting redox graphene;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: be impregnated into by the fabric of (3) gained containing in 0.2mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 20 DEG C, dip time 12h, being subsequently adding 0.2mol/L initiator ammonium persulfate makes aniline in-situ polymerization become polyaniline, obtain graphene/polyaniline covalent bond compliant conductive fabric, and there is good washable and electric conductivity.
Embodiment 2
A kind of preparation method of graphene/polyaniline covalent bond compliant conductive fabric, its process is as follows:
(1) homogeneous mixture solotion of carboxylated graphene oxide and anionic surfactant is prepared: by the anion surfactant of 0.1 mass parts, the sulphuric acid of 0.2 mass parts, join in the carboxylated graphene oxide of 0.3 mass parts, at 30 DEG C, ultrasonic reaction 2h under 500W power, obtain the homogeneous mixture solotion of carboxylated graphene oxide or derivatives thereof and anion surfactant;
(2) p-phenylenediamine carboxyl grafting graphene oxide: by the p-phenylenediamine of 0.08 mass parts, the thionyl chloride of 0.04 mass parts, add in the solution of (1) gained, under the protection of nitrogen, react 3h in 70 DEG C, obtain p-phenylenediamine carboxyl grafting graphene oxide or derivatives thereof;
(3) fabric of the p-phenylenediamine grafting carboxylated graphene oxide of reduction is prepared: be impregnated into by fabric in the solution of (2) gained, dipping temperature 20 DEG C, dip time 1.5h, again by fabric in 60 DEG C of drying 3h, then reduce drying fabric in the hydrazine hydrate solution of 4g/L, reduction temperature 80 DEG C, recovery time 2h, finally washing, drying, obtain covering the fabric of the p-phenylenediamine grafting carboxylated graphene oxide of reduction;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: be impregnated into by the fabric of (3) gained containing in 0.5mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 30 DEG C, dip time 6h, being subsequently adding 0.5mol/L initiator ammonium persulfate makes aniline in-situ polymerization become polyaniline, obtain graphene/polyaniline covalent bond compliant conductive fabric, and there is good washable and electric conductivity.
Embodiment 3
A kind of preparation method of graphene/polyaniline covalent bond compliant conductive fabric, its process is as follows:
(1) homogeneous mixture solotion of sulfonic group graphene oxide and anionic surfactant is prepared: by the anion surfactant of 0.15 mass parts, the sulphuric acid of 0.15 mass parts, join in the sulfonic group graphene oxide of 0.4 mass parts, at 40 DEG C, ultrasonic reaction 1.5h under 800W power, obtain the homogeneous mixture solotion of sulfonic group graphene oxide or derivatives thereof and anion surfactant;
(2) p-phenylenediamine grafting sulfonic groups graphene oxide: by the p-phenylenediamine of 0.13 mass parts, the thionyl chloride of 0.06 mass parts, add in the solution of (1) gained, under the protection of nitrogen, react 8h in 60 DEG C, obtain p-phenylenediamine grafting sulfonic groups graphene oxide or derivatives thereof;
(3) fabric of p-phenylenediamine grafting reduction sulfonic group graphene oxide is prepared: be impregnated into by fabric in the solution of (2) gained, dipping temperature 250 DEG C, dip time 2.5h, again by fabric in 50 DEG C of drying 6h, then reduce drying fabric in the hydrogensulfite solution of 6g/L, reduction temperature 90 DEG C, recovery time 0.5h, finally washing, drying, obtain covering the fabric of p-phenylenediamine grafting reduction sulfonic group graphene oxide or derivatives thereof;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: be impregnated into by the fabric of (3) gained containing in 0.35mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 10 DEG C, dip time 18h, being subsequently adding 0.35mol/L initiator ammonium persulfate makes aniline in-situ polymerization become polyaniline, obtain graphene/polyaniline covalent bond compliant conductive fabric, and there is good washable and electric conductivity.
Embodiment 4
A kind of preparation method of graphene/polyaniline covalent bond compliant conductive fabric, its process is as follows:
(1) homogeneous mixture solotion of graphene oxide and anionic surfactant is prepared: by the anion surfactant of 0.12 mass parts, the sulphuric acid of 0.05 mass parts, join in the graphene oxide of 0.5 mass parts, at 20 DEG C, ultrasonic reaction 2h under 600W power, obtain the homogeneous mixture solotion of sulfonic group graphene oxide or derivatives thereof and anion surfactant;
(2) p-phenylenediamine grafted graphene oxide: by the p-phenylenediamine of 0.15 mass parts, the thionyl chloride of 0.08 mass parts, add in the solution of (1) gained, under the protection of nitrogen, react 12h in 40 DEG C, obtain p-phenylenediamine grafted graphene oxide or derivatives thereof;
(1) fabric of p-phenylenediamine grafting redox graphene is prepared: be impregnated into by fabric in the solution of (2) gained, dipping temperature 20 DEG C, dip time 1h, again by fabric in 70 DEG C of drying 2h, then reduce drying fabric in the hydrazine hydrate solution of 4g/L, reduction temperature 95 DEG C, recovery time 1h, finally washing, drying, obtain covering the fabric of p-phenylenediamine grafting redox graphene or derivatives thereof;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: be impregnated into by the fabric of (3) gained containing in 0.15mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 20 DEG C, dip time 8h, being subsequently adding 0.15mol/L initiator ammonium persulfate makes aniline in-situ polymerization become polyaniline, obtain graphene/polyaniline covalent bond compliant conductive fabric, and there is good washable and electric conductivity.
The implementation result of the present invention
It after embodiment 1-4 processes, is tested by fabric respectively as follows, and test result is in Table 1.
Fabric face resistance (Suzhou Electronics Co., Ltd. of Tontru) on SZT-2A four-point probe is upper to be measured.
As shown in Table 1, the resistance value of finish fabric is decreased obviously. As can be seen here, technical scheme provided by the present invention can give the electric conductivity that polyester-cotton fabric is excellent.
The test result of fabric implemented by table 1
Claims (3)
1. the preparation method of a graphene/polyaniline covalent bond compliant conductive fabric, it is characterized in that adopting p-phenylenediamine grafted graphene oxide, then to fabric dipping and reduction treatment, and with conductive polymer polymer monomer covalent bond, preparing washable graphene/polyaniline covalent bond compliant conductive fabric, it specifically adopts following processing step:
(1) by the anion surfactant of 0.01��0.5 mass parts, the sulphuric acid of 0.05��0.4 mass parts, join in the graphene oxide or derivatives thereof of 0.05��1 mass parts, at 20��60 DEG C, ultrasonic reaction 0.5��2h under 300-1000W power, obtain the homogeneous mixture solotion of graphene oxide or derivatives thereof and anion surfactant;
(2) by the p-phenylenediamine of 0.1��2 mass parts, the thionyl chloride of 0.01��1 mass parts, add in the solution of (1) gained, under the protection of nitrogen, react 1��6h in 40��80 DEG C, obtain p-phenylenediamine grafted graphene oxide or derivatives thereof;
Described graphene oxide or derivatives thereof is at least one in graphene oxide, carboxylated graphene oxide, sulfonic group graphene oxide;
Described anion surfactant is at least one in alkylsulfonate, alkylbenzenesulfonate, alkyl carboxylate, alkylbenzene carboxylates, alkylnaphthalene sulfonate, alkylnaphthalene carboxylate, alkyl-anthraquinone sulfonate, alkyl-anthraquinone carboxylate.
2., such as the preparation method that right wants a kind of graphene/polyaniline covalent bond compliant conductive fabric as described in 1, it is characterized in that described fabric dipping and reduction treatment adopt following processing step:
Fabric is impregnated in the solution of p-phenylenediamine grafted graphene oxide or derivatives thereof gained, dipping temperature 20��50 DEG C, dip time 0.5��2h, again by fabric in 50��80 DEG C of drying 0.5��5h, then reduce drying fabric in the reductant solution of 1��10g/L, reduction temperature 50��100 DEG C, recovery time 0.5��6h, finally washing, drying, obtain covering the fabric of p-phenylenediamine grafting redox graphene or derivatives thereof;
Described reducing agent is at least one in sodium dithionite, sodium sulfite, glucose, chitosan, vitamin C, hydrazine hydrate, sodium borohydride.
3., such as the preparation method that right wants a kind of graphene/polyaniline covalent bond compliant conductive fabric as described in 1, it is characterized in that described and conductive polymer polymer monomer covalent bond adopts following processing step:
The fabric of gained is impregnated into containing in 0.02��1mol/L conductive polymer polymer monomer and 0.02��1mol/L acid solution, dipping temperature 0��40 DEG C, dip time 0.5��24h, being subsequently adding initiator makes polymer monomer aggregate into conductive polymer polymer, obtains graphene/polyaniline covalent bond compliant conductive fabric;
Described conductive polymer polymer monomer is at least one in aniline, p-aminobenzene sulfonic acid, metanilic acid.
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