CN104313872A - Preparation method of graphene/polyaniline covalent binding conductive fabric - Google Patents
Preparation method of graphene/polyaniline covalent binding conductive fabric Download PDFInfo
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- CN104313872A CN104313872A CN201410554346.6A CN201410554346A CN104313872A CN 104313872 A CN104313872 A CN 104313872A CN 201410554346 A CN201410554346 A CN 201410554346A CN 104313872 A CN104313872 A CN 104313872A
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Abstract
The invention discloses a preparation method of a graphene/polyaniline covalent binding conductive fabric, which belongs to the technical field of textile chemistry. The preparation method comprises the steps of applying oxidized graphene or oxidized graphene derivative and a reaction product of p-phenylenediamine onto the fabric to be reduced, enabling the fabric to adsorb the polyaniline monomer, enabling the in-situ polymerization of the polyaniline monomer on the fabric to form polyaniline, and enabling the polyaniline to form covalent key combination with the graphene. According to the method, a conductive layer formed by covalently combining the graphene and polyaniline can be acquired on the surface of the fabric, so that the stability of the conductive layer is improved, and the conductive fabric with excellent effect can be acquired. The method is applicable to conventional fabrics such as natural fibers including cotton, wool, silk and the like, synthesized fibers including terylene, chinlon, acrylic fibers and the like and blending of fabric or conductive arrangement of intertexture, and the prepared functional fabric can be applied to the fields of medical healthcare, intelligent sensors, mobile power generation, military and the like.
Description
Technical field
The invention belongs to technical field of textile chemistry, relate to a kind of Graphene or derivatives thereof and conductive polymer polymer covalent bond of adopting from the method preparing 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 develop the method for conduction textile material the earliest, these two kinds method processing is simple, conduction is even, but the flexibility of finish fabric is inadequate, the particularly conductive fabric prepared of coating, runs into stronger stretching or foldingly can make coating cracking taking in process.Therefore, the attention of people is caused at fabric face formation fexible film and conductive polymer polymer at the conduction method for sorting that fabric face carries out being polymerized with Graphene.
Graphene exists with the cellular many hexagonal structures form of individual layer, and because carbon atom is connected by stable covalent bond, therefore Graphene has superpower electric conductivity.But simple graphene conductive fabric, after must making fabric covers equably the Graphene of q.s, fabric just has good electric conductivity and conduction uniformity; , also there is heat resistance less stable in simple polyaniline conductive fabric, electric conductivity is not very strong problem.The present invention first will prepare the homogeneous solution system of graphene oxide or derivatives thereof, and object is the gathering in order to prevent Graphene in subsequent reactions process; Then add p-phenylenediamine (PPD) to make it and graphene oxide generation covalent reaction, again by the aqueous solution of textile impregnation p-phenylenediamine (PPD) grafted graphene oxide or derivatives thereof, carry out drying, reducing after making fabric fully adsorb p-phenylenediamine (PPD) grafted graphene oxide or derivatives thereof; Finally adopt the method for carrying out in-situ polymerization aniline or derivatives thereof on fabric, obtained Graphene and the covalently bound compliant conductive fabric of polyaniline.Because Graphene and polyaniline define covalent bonds, obtained fabric washability is good, electric conductivity is high.
Summary of the invention
The object of the invention is to adopt the method for self assembly, Graphene and derivative thereof, conductive polymer polymer are applied on fabric, make fabric obtain high conduction performance.
The present invention adopts following technical scheme:
1 adopts p-phenylenediamine (PPD) grafted graphene oxide, then to textile impregnation and reduction treatment, and with conductive polymer polymer monomer covalent bond, prepare washable graphene/polyaniline covalent bond compliant conductive fabric.
Described in 2, p-phenylenediamine (PPD) grafted graphene oxide adopts following processing step:
(1) by the anion surfactant of 0.01 ~ 0.5 parts by mass, the sulfuric acid of 0.05 ~ 0.4 parts by mass, join in the graphene oxide or derivatives thereof of 0.05 ~ 1 parts by mass, 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 (PPD) of 0.1 ~ 2 parts by mass, the thionyl chloride of 0.01 ~ 1 parts by mass, adds in the solution of (1) gained, and under 40 ~ 80 DEG C of protections at nitrogen, reaction 1 ~ 6h, obtains p-phenylenediamine (PPD) 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, Fluhyzon carboxylate, alkyl-anthraquinone sulfonate, alkyl-anthraquinone carboxylate.
Textile impregnation described in 3 and reduction treatment adopt following processing step:
By textile impregnation in the solution of p-phenylenediamine (PPD) 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 oven dry fabric is reduced in the reductant solution of 1 ~ 10g/L, reduction temperature 50 ~ 100 DEG C, recovery time 0.5 ~ 6h, finally wash, dry, obtain the fabric covering p-phenylenediamine (PPD) grafting redox graphene or derivatives thereof;
Described reductant is at least one in sodium dithionite, sodium hydrogensulfite, glucose, shitosan, vitamin C, hydrazine hydrate, sodium borohydride.
Following processing step is adopted with conductive polymer polymer monomer covalent bond described in 4:
By the textile impregnation of gained to 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, then adding initator 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, sulfanilic 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 of the present invention is simple, convenient 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 thereto.
Embodiment 1
A preparation method for 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 parts by mass, the sulfuric acid of 0.1 parts by mass, join in the graphene oxide of 0.4 parts by mass, 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 (PPD) grafted graphene oxide or derivatives thereof: by the p-phenylenediamine (PPD) of 0.12 parts by mass, the thionyl chloride of 0.06 parts by mass, add in the solution of (1) gained, under 50 DEG C of protections at nitrogen, react 4h, obtain p-phenylenediamine (PPD) grafted graphene oxide or derivatives thereof;
(3) fabric of p-phenylenediamine (PPD) grafting redox graphene is prepared: by textile impregnation 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 oven dry fabric is reduced in the hydrogensulfite solution of 5g/L, reduction temperature 90 DEG C, recovery time 0.5h, finally wash, dry, obtain the fabric covering p-phenylenediamine (PPD) grafting redox graphene;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: by the textile impregnation of (3) gained to containing in 0.2mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 20 DEG C, dip time 12h, then 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 preparation method for 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 parts by mass, the sulfuric acid of 0.2 parts by mass, join in the carboxylated graphene oxide of 0.3 parts by mass, 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 (PPD) carboxyl grafting graphene oxide: by the p-phenylenediamine (PPD) of 0.08 parts by mass, the thionyl chloride of 0.04 parts by mass, add in the solution of (1) gained, under 70 DEG C of protections at nitrogen, react 3h, obtain p-phenylenediamine (PPD) carboxyl grafting graphene oxide or derivatives thereof;
(3) prepare p-phenylenediamine (PPD) grafting and reduce the fabric of carboxylated graphene oxide: by textile impregnation 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 oven dry fabric is reduced in the hydrazine hydrate solution of 4g/L, reduction temperature 80 DEG C, recovery time 2h, finally wash, dry, obtain covering p-phenylenediamine (PPD) grafting and reduce the fabric of carboxylated graphene oxide;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: by the textile impregnation of (3) gained to containing in 0.5mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 30 DEG C, dip time 6h, then 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 preparation method for 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 parts by mass, the sulfuric acid of 0.15 parts by mass, join in the sulfonic group graphene oxide of 0.4 parts by mass, 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 (PPD) grafting sulfonic groups graphene oxide: by the p-phenylenediamine (PPD) of 0.13 parts by mass, the thionyl chloride of 0.06 parts by mass, add in the solution of (1) gained, under 60 DEG C of protections at nitrogen, react 8h, obtain p-phenylenediamine (PPD) grafting sulfonic groups graphene oxide or derivatives thereof;
(3) fabric of p-phenylenediamine (PPD) grafting reduction sulfonic group graphene oxide is prepared: by textile impregnation 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 oven dry fabric is reduced in the hydrogensulfite solution of 6g/L, reduction temperature 90 DEG C, recovery time 0.5h, finally wash, dry, obtain the fabric covering p-phenylenediamine (PPD) grafting reduction sulfonic group graphene oxide or derivatives thereof;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: by the textile impregnation of (3) gained to containing in 0.35mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 10 DEG C, dip time 18h, then 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 preparation method for 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 parts by mass, the sulfuric acid of 0.05 parts by mass, join in the graphene oxide of 0.5 parts by mass, 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 (PPD) grafted graphene oxide: by the p-phenylenediamine (PPD) of 0.15 parts by mass, the thionyl chloride of 0.08 parts by mass, add in the solution of (1) gained, under 40 DEG C of protections at nitrogen, react 12h, obtain p-phenylenediamine (PPD) grafted graphene oxide or derivatives thereof;
(1) fabric of p-phenylenediamine (PPD) grafting redox graphene is prepared: by textile impregnation 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 oven dry fabric is reduced in the hydrazine hydrate solution of 4g/L, reduction temperature 95 DEG C, recovery time 1h, finally wash, dry, obtain the fabric covering p-phenylenediamine (PPD) grafting redox graphene or derivatives thereof;
(4) graphene/polyaniline covalent bond conductive fabric is prepared: by the textile impregnation of (3) gained to containing in 0.15mol/L aniline and 1mol/L hydrochloric acid solution, dipping temperature 20 DEG C, dip time 8h, then 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.
Implementation result of the present invention
Fabric after embodiment 1-4 process, is tested it 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 obviously declines.As can be seen here, technical scheme provided by the present invention can give polyester-cotton fabric excellent electric conductivity.
The test result of fabric implemented by table 1
Claims (4)
1. the preparation method of a graphene/polyaniline covalent bond compliant conductive fabric, it is characterized in that adopting p-phenylenediamine (PPD) grafted graphene oxide, then to textile impregnation and reduction treatment, and with conductive polymer polymer monomer covalent bond, prepare washable graphene/polyaniline covalent bond compliant conductive fabric.
2., as right wants the preparation method of a kind of graphene/polyaniline covalent bond compliant conductive fabric as described in 1, it is characterized in that described p-phenylenediamine (PPD) grafted graphene oxide adopts following processing step:
(1) by the anion surfactant of 0.01 ~ 0.5 parts by mass, the sulfuric acid of 0.05 ~ 0.4 parts by mass, join in the graphene oxide or derivatives thereof of 0.05 ~ 1 parts by mass, 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 (PPD) of 0.1 ~ 2 parts by mass, the thionyl chloride of 0.01 ~ 1 parts by mass, adds in the solution of (1) gained, and under 40 ~ 80 DEG C of protections at nitrogen, reaction 1 ~ 6h, obtains p-phenylenediamine (PPD) 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, Fluhyzon carboxylate, alkyl-anthraquinone sulfonate, alkyl-anthraquinone carboxylate.
3., as right wants the preparation method of a kind of graphene/polyaniline covalent bond compliant conductive fabric as described in 1, it is characterized in that described textile impregnation and reduction treatment adopt following processing step:
By textile impregnation in the solution of p-phenylenediamine (PPD) 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 oven dry fabric is reduced in the reductant solution of 1 ~ 10g/L, reduction temperature 50 ~ 100 DEG C, recovery time 0.5 ~ 6h, finally wash, dry, obtain the fabric covering p-phenylenediamine (PPD) grafting redox graphene or derivatives thereof;
Described reductant is at least one in sodium dithionite, sodium hydrogensulfite, glucose, shitosan, vitamin C, hydrazine hydrate, sodium borohydride.
4., as right wants the preparation method of 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:
By the textile impregnation of gained to 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, then adding initator 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, sulfanilic acid, metanilic acid.
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