CN109537083A - A kind of preparation method and applications of graphene/polyaniline nano-composite fiber film - Google Patents
A kind of preparation method and applications of graphene/polyaniline nano-composite fiber film Download PDFInfo
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- CN109537083A CN109537083A CN201811517468.2A CN201811517468A CN109537083A CN 109537083 A CN109537083 A CN 109537083A CN 201811517468 A CN201811517468 A CN 201811517468A CN 109537083 A CN109537083 A CN 109537083A
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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- Mechanical Engineering (AREA)
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- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of preparation method and applications of graphene/polyaniline nano-composite fiber film, its step includes: that graphene is dissolved in polyvinyl alcohol water solution, high speed shear obtains graphene solution, dodecyl benzene sulfonic acid is added to graphene solution ice bath stirring, and aniline stirring 30min is added, ammonium persulfate solution is added dropwise to mixed solution high-speed stirred 4h, obtain polyaniline/graphene composite electrostatic spinning liquid, through electrostatic spinning and be dried in vacuo polyaniline graphene composite cellulosic membrane, preparation method are easy to operate, low in cost；Gained graphene/polyaniline composite nano-fiber membrane is high for wearable electronic product electro-chemical activity as electrode material for super capacitor, specific volume is high, stability is good, also has a vast market foreground as energy storage material for intelligent textile.
Description
Technical field
The invention belongs to inorganic-organic composite material technical field, in particular to a kind of graphene/polyaniline is nano combined
The preparation method and applications of tunica fibrosa.
Background technique
Conductive fiber film is due to passing through the superfine nano of electrostatic spinning technique preparation with good flexibility and electric conductivity
Fiber or nano fibrous membrane because its excellent performance in various fields all has good development and application potential, as sensor,
The fields such as biological skeleton, electronic device, enhancing composite material, protective garment, filtering material, biomedical material.
Intrinsic conduction polymer (ICPs), including polyaniline, polythiophene and polypyrrole are that have to be similar to semiconductor and gold
The organic material of the electrical properties of inorganic material such as category.Due to low manufacturing cost, low-density, good machinability, height
The characteristics of mechanical flexibility, so that they become the substitute of high desnity metal and oxide.As most polymers,
ICPs has good ductility, similar thermal expansion coefficient and mechanical property, makes the development for stablizing conductive plastics composite material
It is possibly realized, may be used as the flexible transparent electrode of electrochromic device and solar battery.Polyaniline is as conducting polymer
Existing extensive research, it is cheap, electric conductivity is excellent, be one of most stable of thermodynamic material in ICPs, be have it is good
The intrinsic conduction polymer of good application prospect.However, the poor dissolubility and stability of polyaniline limits it commercialized
It uses.
Graphene (Graphene) is a kind of new material of laminated structure being made of single layer of carbon atom, between carbon atom
It is interconnected to hexagonal lattice structure by chemical bond, Mechanics of Machinery intensity is high, thermal conductivity is good, carrier mobility is high, ratio
Surface area is big, has a extensive future in the fields such as electronic device, sensor, energy storage device and reinforcement and filled composite materials.
The conductive carbon materials such as graphite and graphene have high Mechanics of Machinery intensity and good electric conductivity, but as with electric double layer electricity
Hold feature carbon material, specific capacitance is not high, and graphene dispersion performance in nonpolar solvent is poor, limits graphene-based multiple
The application of condensation material.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of graphene/polyaniline nano-composite fiber film and its answer
With using polyaniline and graphene as raw material, first doped induction and emulsion polymerizing preparation aniline/graphene/polyvinyl alcohol are multiple
Spinning solution is closed, polyaniline/graphene/polyethylene glycol fiber films with high-specific surface area are made by electrostatic spinning, pass through two
Person's synergistic effect, improves the electric conductivity and stability of polyaniline, and make up the small problem of carbon material capacitance, while helping to lead
Application of the electric polymer nanofiber in wearable electronic product and intelligent textile.
Above-mentioned purpose of the invention is achieved through the following technical solutions:
The preparation method of graphene/polyaniline nano-composite fiber film, specifically, comprising the following steps:
(1) granule of polyvinyl alcohol is added to the water, under stirring conditions in 90~95 DEG C of heating meltings, obtains polyethylene
Alcoholic solution；Graphene is added to above-mentioned poly-vinyl alcohol solution and 10~30min of high speed shear again, obtaining solid content is 0.25wt%
Graphene/polyvinyl alcohol liquid；Wherein, the mass concentration of the poly-vinyl alcohol solution is 4.0%~4.5%；
(2) graphene described in step (1)/polyvinyl alcohol liquid is transferred to conical flask, is placed in ice bath circulation
In pump, dodecyl benzene sulfonic acid, aniline and ammonium persulfate solution are sequentially added in 0 DEG C under stirring conditions and carries out emulsion polymerization
3~5h is reacted, until reaction solution at blackish green, obtains polyaniline/graphene/polyvinyl alcohol multiple emulsion；Emulsion breaking calculates polyphenyl
Amine/graphene solid content；Multiple emulsion is added in poly-vinyl alcohol solution, configures polyaniline/graphene of different solid contents, contains admittedly
Amount is the polyvinyl alcohol spinning solution of 10wt%；Wherein,
The rate of addition of the ammonium persulfate solution is 6 drops/5s；
In the polyaniline/graphene/polyvinyl alcohol composite spinning liquid, the mixture of the polyaniline and the graphene
Mass concentration be 0.2%~1%；
The molar ratio of the dodecyl benzene sulfonic acid, ammonium persulfate and aniline is 0.8:0.8:1；
(3) composite spinning liquid described in step (2) is added to electrostatic spinning apparatus through electrostatic spinning and vacuum drying, is obtained
Graphene/polyaniline composite nano-fiber membrane；Wherein, the technological parameter of the electrostatic spinning include: spinning voltage be 15~
35kV, temperature are 20~40 DEG C, and relative humidity is 30%~70%, and spinning distance is 20cm, the flow velocity of spinning head spinning solution
For 0.5mL/h.
Preferably, in step (1), the mass concentration of the poly-vinyl alcohol solution is 10%；The graphene is added to institute
State poly-vinyl alcohol solution high speed shear 20min.
Preferably, in step (2), in the polyaniline/graphene/polyvinyl alcohol composite spinning liquid, the polyaniline and
The mass concentration of the mixture of the graphene is 0.4%~0.8%.
It is highly preferred that in step (2), in the polyaniline/graphene/polyvinyl alcohol composite spinning liquid, the polyaniline
Mass concentration with the mixture of the graphene is 0.6%.
Second aspect, graphene/polyaniline composite nano-fiber membrane are fine by above-mentioned graphene/polyaniline composite Nano
The preparation method for tieing up film is made.
The third aspect, above-mentioned graphene/polyaniline composite nano-fiber membrane is as capacitor electrode material for wearable
Electronic product.
Fourth aspect, above-mentioned graphene/polyaniline composite nano-fiber membrane are used for intelligent textile as energy storage material.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention uses polyvinyl alcohol, because its good film forming greatly improves the content of composite cellulosic membrane polyaniline,
The composite cellulosic membrane large specific surface area of preparation, further increases the electric conductivity of composite cellulosic membrane.
(2) preparation method of the present invention is easy to operate, low in cost, graphene/polyaniline composite nano-fiber membrane obtained
As electrode material for super capacitor is high for wearable electronic product electro-chemical activity, specific volume is high, stability is good；As energy storage
Material also has a vast market foreground for intelligent textile.
Detailed description of the invention
Fig. 1 is the process flow chart that the present invention prepares graphene/polyaniline composite nano-fiber membrane.
Fig. 2 is the cyclic voltammetry curve of 1 gained graphene polyaniline composite nanofiber membrane of embodiment.
Fig. 3 is the cyclic voltammetry curve of 2 gained graphene polyaniline composite nanofiber membrane of embodiment.
Fig. 4 is the cyclic voltammetry curve of 3 gained graphene polyaniline composite nanofiber membrane of embodiment.
Fig. 5 is the cyclic voltammetry curve of 4 gained graphene polyaniline composite nanofiber membrane of embodiment.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
Referring to Fig. 1, the preparation method of graphene/polyaniline nano-composite fiber film, specifically:
(1) granule of polyvinyl alcohol is added to the water, under stirring conditions in 90~95 DEG C of heating meltings, obtains polyethylene
Alcoholic solution；Graphene is added to above-mentioned poly-vinyl alcohol solution and 10~30min of high speed shear again, obtaining solid content is 0.25wt%
Graphene/polyvinyl alcohol liquid；Wherein, the mass concentration of poly-vinyl alcohol solution is 4.0%~4.5%；
(2) graphene/polyvinyl alcohol liquid in step (1) is transferred to conical flask, is placed in ice bath circulating pump,
Dodecyl benzene sulfonic acid, aniline and ammonium persulfate solution are sequentially added in 0 DEG C under stirring conditions and carries out emulsion polymerization 3
~5h, until reaction solution at blackish green, obtains polyaniline/graphene/polyvinyl alcohol multiple emulsion.By emulsion breaking, calculate polyaniline/
Graphene solid content.Multiple emulsion is added in poly-vinyl alcohol solution, polyaniline/graphene of different solid contents is configured, contains admittedly
Amount is the polyvinyl alcohol spinning solution of 10wt%.Wherein, the rate of addition of ammonium persulfate solution be 6 drops/5s, polyaniline/graphene/
In polyvinyl alcohol composite spinning liquid, the mass concentration of the mixture of polyaniline and graphene is 0.2%~1%, detergent alkylate
The molar ratio of sulfonic acid, ammonium persulfate and aniline is 0.8:0.8:1；
(3) composite spinning liquid in step (2) is added to electrostatic spinning apparatus through electrostatic spinning and vacuum drying, obtains graphite
Alkene/polyaniline composite nanofiber membrane；Wherein, it is 15~35kV that the technological parameter of electrostatic spinning, which includes: spinning voltage, and temperature is
20~40 DEG C, relative humidity is 30%~70%, and spinning distance is 20cm, and the flow velocity of spinning head spinning solution is 0.5mL/h.
Embodiment 1
The pva powder that molecular weight is Mw=1799g/mol is added in aqueous solution, concentration 4.3%, 95 DEG C are stirred
Dissolution is mixed, poly-vinyl alcohol solution is obtained；The graphene that solid content is 0.25% is added in poly-vinyl alcohol solution, high speed shear
20min；Mixed solution is transferred in conical flask, ice bath-refrigerating cycle pump is placed in, detergent alkylate sulphur is added in 0 DEG C of stirring
Acid, mixing speed are stirred until homogeneous for 1200r/min, and aniline monomer is added, and mixing speed rises to 2000r/min stirring 30min；
Configured 10mL ammonium persulfate solution is added dropwise in mixed solution with 6 drops/5s, stirs 4h, is stood.Lotion is carried out brokenly
Cream calculates polyaniline/graphene solid content.Multiple emulsion is added in poly-vinyl alcohol solution, polyaniline/graphene is configured
The spinning solution that solid content is 0.2wt%, polyvinyl alcohol solid content is 10wt%.Above-mentioned spinning solution is added in electrostatic spinning apparatus
Electrostatic spinning is carried out, graphene polyaniline composite nanofiber membrane is dried in vacuo to obtain；Electrospinning conditions are as follows: spinning voltage is
17kV, temperature are 25 DEG C, relative humidity 30%, and spinning distance is 20cm, and the flow velocity of spinning head spinning solution is 0.5mL/h,
Its cyclic voltammetry curve is as shown in Figure 2.
Embodiment 2
The pva powder that molecular weight is Mw=1799g/mol is added in aqueous solution, concentration 4.3%, 95 DEG C are stirred
Dissolution is mixed, poly-vinyl alcohol solution is obtained；The graphene that solid content is 0.25% is added in poly-vinyl alcohol solution, high speed shear
20min；Mixed liquor is transferred in conical flask, ice bath-refrigerating cycle pump is placed in, detergent alkylate sulphur is added in 0 DEG C of stirring
Acid, mixing speed are stirred until homogeneous for 1200r/min, and aniline monomer is added, and revolving speed rises to 2000r/min stirring 30min；It will match
The 10ml ammonium persulfate solution set is added dropwise in mixed solution with 6 drops/5s, stirs 4h, is stood.Lotion is demulsified, is counted
Calculate polyaniline/graphene solid content.Multiple emulsion is added in poly-vinyl alcohol solution, configuration polyaniline/graphene, which is consolidated, to be contained
Amount be 0.2wt%, the spinning solution that polyvinyl alcohol solid content is 10wt%.Above-mentioned spinning solution is added in electrostatic spinning apparatus and carries out
Electrostatic spinning is dried in vacuo to obtain graphene polyaniline composite nanofiber membrane；Electrospinning conditions are as follows: spinning voltage 23kV,
Temperature is 25 DEG C, relative humidity 30%, and spinning distance is 20cm, and the flow velocity of spinning head spinning solution is 0.5mL/h, circulation
Volt-ampere curve is as shown in Figure 3.
Embodiment 3
The pva powder that molecular weight is Mw=1799g/mol is added in aqueous solution, concentration 4.3%, 95 DEG C are stirred
Dissolution is mixed, poly-vinyl alcohol solution is obtained, the graphene that solid content is 0.25% is added in poly-vinyl alcohol solution, high speed shear
20min, mixed solution are transferred to conical flask, are placed in ice bath-refrigerating cycle pump, and dodecyl benzene sulfonic acid is added in 0 DEG C of stirring,
Mixing speed is stirred until homogeneous for 1200r/min, and aniline monomer is added, and revolving speed is risen to 2000r/min stirring 30min；It will match
The 10ml ammonium persulfate solution set is added dropwise in mixed solution with 6 drops/5s, stirs 4h, is stood.Lotion is demulsified, is counted
Calculate polyaniline/graphene solid content.Multiple emulsion is added in poly-vinyl alcohol solution, configuration polyaniline/graphene, which is consolidated, to be contained
Amount be 0.2wt%, the spinning solution that polyvinyl alcohol solid content is 10wt%.Above-mentioned spinning solution is added in electrostatic spinning apparatus and carries out
Electrostatic spinning is dried in vacuo to obtain graphene polyaniline composite nanofiber membrane；Electrospinning conditions are as follows: spinning voltage 23kV,
Temperature is 25 DEG C, relative humidity 30%, and spinning distance is 20cm, and the flow velocity of spinning head spinning solution is 0.5mL/h, circulation
Volt-ampere curve is as shown in Figure 4.
Embodiment 4
The pva powder that molecular weight is Mw=1799g/mol is added in aqueous solution, concentration 10% is in temperature
Stirring and dissolving at T=95 DEG C, obtains poly-vinyl alcohol solution, is that 0.25% graphene is added to poly-vinyl alcohol solution by solid content
In, high speed shear 20min, mixed solution is transferred to conical flask, is placed in ice bath-refrigerating cycle pump, and 0 DEG C of stirring is added 12
Alkyl benzene sulphonate, mixing speed are stirred until homogeneous for 1200r/min, and aniline monomer is added, revolving speed is promoted to 2000r/min and is stirred
Mix 30min；Configured 10ml ammonium persulfate solution is added dropwise in mixed solution with 6 drops/5s, stirs 4h, is stood.By lotion into
Row demulsification, calculates polyaniline/graphene solid content.Multiple emulsion is added in poly-vinyl alcohol solution, polyaniline/graphite is configured
The spinning solution that the solid content of alkene is 1.0wt%, polyvinyl alcohol solid content is 10wt%.Above-mentioned spinning solution is added to electrostatic spinning
Electrostatic spinning is carried out in device, is dried in vacuo to obtain graphene polyaniline composite nanofiber membrane；Electrospinning conditions are as follows: spinning electricity
Pressure is 23kV, and temperature is 25 DEG C, and relative humidity 30%, spinning distance is 20cm, and the flow velocity of spinning head spinning solution is
0.5mL/h, cyclic voltammetry curve are as shown in Figure 5.
Claims (7)
1. the preparation method of graphene/polyaniline nano-composite fiber film, which comprises the following steps:
(1) granule of polyvinyl alcohol is added to the water, under stirring conditions in 90~95 DEG C of heating meltings, it is molten obtains polyvinyl alcohol
Liquid；Graphene is added to the stone for obtaining that solid content is 0.25wt% to above-mentioned poly-vinyl alcohol solution and 10~30min of high speed shear again
Black alkene/polyvinyl alcohol liquid；Wherein, the mass concentration of the poly-vinyl alcohol solution is 4.0%~4.5%；
(2) graphene described in step (1)/polyvinyl alcohol liquid is transferred to conical flask, is placed in ice bath circulating pump,
Dodecyl benzene sulfonic acid, aniline and ammonium persulfate solution are sequentially added in 0 DEG C under stirring conditions and carries out emulsion polymerization 3
~5h, until reaction solution at blackish green, obtains polyaniline/graphene/polyvinyl alcohol multiple emulsion；Simultaneously the poly- second is added in emulsion breaking
Polyvinyl alcohol spinning solution is obtained in enolate solution；Wherein,
The rate of addition of the ammonium persulfate solution is 6 drops/5s；
In the polyaniline/graphene/polyvinyl alcohol composite spinning liquid, the matter of the mixture of the polyaniline and the graphene
Measuring concentration is 0.2%~1%；
The molar ratio of the dodecyl benzene sulfonic acid, ammonium persulfate and aniline is 0.8:0.8:1；
(3) composite spinning liquid described in step (2) is added to electrostatic spinning apparatus through electrostatic spinning and vacuum drying, obtains graphite
Alkene/polyaniline composite nanofiber membrane；Wherein, it is 15~35kV, temperature that the technological parameter of the electrostatic spinning, which includes: spinning voltage,
Degree is 20~40 DEG C, and relative humidity is 30%~70%, and spinning distance is 20cm, and the flow velocity of spinning head spinning solution is 0.5mL/
h。
2. the preparation method of graphene/polyaniline nano-composite fiber film according to claim 1, which is characterized in that step
Suddenly in (1), the mass concentration of the poly-vinyl alcohol solution is 10%；The graphene is added to the poly-vinyl alcohol solution high speed
Shear 20min.
3. the preparation method of graphene/polyaniline nano-composite fiber film according to claim 1, which is characterized in that step
Suddenly in (2), in the polyaniline/graphene/polyvinyl alcohol composite spinning liquid, the mixture of the polyaniline and the graphene
Mass concentration be 0.4%~0.8%.
4. the preparation method of graphene/polyaniline nano-composite fiber film according to claim 1 or 3, which is characterized in that
In step (2), in the polyaniline/graphene/polyvinyl alcohol composite spinning liquid, the mixing of the polyaniline and the graphene
The mass concentration of object is 0.6%.
5. graphene/polyaniline composite nano-fiber membrane, which is characterized in that pass through the described in any item graphite of Claims 1 to 4
Alkene/polyaniline composite nanofiber membrane preparation method is made.
6. graphene/polyaniline composite nano-fiber membrane described in claim 5 is used for wearable electricity as capacitor electrode material
Sub- product.
7. graphene/polyaniline composite nano-fiber membrane described in claim 5 is used for intelligent textile as energy storage material.
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