CN108587446A - A kind of production method of polyaniline appendix graphite ene coatings - Google Patents
A kind of production method of polyaniline appendix graphite ene coatings Download PDFInfo
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- CN108587446A CN108587446A CN201810288047.0A CN201810288047A CN108587446A CN 108587446 A CN108587446 A CN 108587446A CN 201810288047 A CN201810288047 A CN 201810288047A CN 108587446 A CN108587446 A CN 108587446A
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- polyaniline
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/02—Polyamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention belongs to material chemistry technical fields, are related to a kind of production method of polyaniline appendix graphite ene coatings.The present invention is uniformly modified polyaniline on graphene oxide using in-situ polymerization mode, then KI reduction-oxidation graphite, while product I2It is absorbed by polyaniline molecule, obtains the uniform modification for realizing polyaniline in the highly conductive graphene surface of reduction, and played the role of collaboration and increase conductivity.Obtained coating conductivity is high, strong adhesive force.Prepares coating uses water-based slurry, meets environment protection requirement.Coating can be used for the fields such as antistatic, electromagnetic shielding and conducting wire.
Description
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of production method of polyaniline appendix graphite ene coatings.
Background technology
Conductive coating is to be coated on insulating substrate to play conducting electric current or the coating with antistatic effect.Graphene
Electric conductivity has excellent mechanical performance and thermal stability better than conductive materials such as silver powder, copper powders, is that excellent conduction applies
Layer base material, its shortcoming is that bad dispersibility in solution, poor with polymer-polymer miscibility, coating is easily peelable.Polyaniline is commonly to lead
The compound conductive material for preparing of polyaniline and graphene is had many reports, but polyaniline and the more difficult reality of graphene by electric macromolecule
It is existing compatible, tend to the problems such as uneven split-phase, conductivity and disbonding occur after forming coating.Polyaniline and graphene
It is still technical a major challenge to combine closely.
Invention content
In view of the shortcomings of the prior art, the purpose of the present invention is to provide a kind of making sides of polyaniline appendix graphite ene coatings
Method, which is characterized in that include the following steps：
(1) aniline monomer and graphite oxide are added in acidic aqueous solution, ultrasonic disperse obtains puce colloidal sol (colloidal sol
A it), then by oxidant is dissolved in acidic aqueous solution, and is slowly dropped in Sol A and obtains mixed sols.
(2) mixed sols that step (1) obtains is put into constant temperature in heat-preserving equipment to be stirred to react, obtains black precipitate；
(3) it is distributed in potassium iodide aqueous solution after washing the black precipitate that step (2) obtains, thickener, room temperature is added
It is stirred under~60 DEG C of ultrasonic environments and obtains within 8~12 hours stable blue conductive dispersions slurry；
(4) slurry for rotary coating or blade coating are air-dried at material surface, room temperature~70 DEG C and polyaniline appendix graphene can be obtained
Conductive coating.
The addition of the graphite oxide is 0.2~1.5gL-1；The ultrasonic disperse time is 1~2h.Aniline monomer is most
A concentration of 0.1~0.5molL in colloidal sol afterwards-1；Acidic aqueous solution pH is less than 2.
The oxidant includes one kind or combinations thereof in ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, ferric trichloride, oxygen
The molar ratio of agent and aniline monomer is 1: 1~3: 1.
The reaction time that the constant temperature is stirred to react be 12~24 hours, temperature be room temperature~60 DEG C, washing be spend from
Sub- water and ethyl alcohol alternately wash, and use centrifuge precipitation or pumping and filtering device to be filtered each time after washing, filtration product exists again
Disperse in deionized water or ethyl alcohol, repeated filtration is 6~7 until filtrate pH value.
The concentration equivalent that the black precipitate is added in potassium iodide aqueous solution is 10~40g/L, iodate potassium concn 10~
20g/L, thickener are water-soluble resin, including water soluble acrylic resin, water soluble alkyd resin, water soluble polyurethane resin
In one kind or combinations thereof, a concentration of 15~45g/L in potassium iodide aqueous solution is added.
The present invention is uniformly modified polyaniline on graphene oxide using in-situ polymerization mode, then KI oxygen reduction fossils
Ink, while product I2It is absorbed by polyaniline molecule, obtains uniformly repairing for the highly conductive graphene surface for realizing polyaniline in reduction
Decorations, and play the role of collaboration and increase conductivity.Obtained coating conductivity is high, strong adhesive force.Prepares coating uses water base slurry
Material, meets environment protection requirement.Coating can be used for the fields such as antistatic, electromagnetic shielding and conducting wire.
Present disclosure and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this
The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention
The revealed content of embodiment should be not limited to by enclosing, and should be included in the combination of all the elements embodied in different piece, with
And various replacements and modification without departing substantially from the present invention, and covered by claims of the present invention.
Description of the drawings
Fig. 1 is the SEM photograph using (embodiment 1) synthesized polyaniline appendix graphene coating surface of the invention.
Specific implementation mode
Embodiment 1
(1) 0.01mol aniline monomers and 0.02g graphite oxides are added in 50mL acidic aqueous solutions, ultrasonic disperse 2h is obtained
It is dissolved in 50mL acidic aqueous solutions, and is slowly dropped to molten to puce colloidal sol (Sol A), then by 0.03mol ammonium persulfates
Mixed sols is obtained in glue A.
(2) mixed sols that step (1) obtains is put into constant temperature in 60 DEG C of heat-preserving equipments to be stirred to react 24 hours, is obtained black
Color precipitates；
(3) the black precipitate deionized water and ethyl alcohol obtained step (2) is alternately washed, each time after washing using centrifugation
Machine precipitates or pumping and filtering device is filtered, and filtration product is disperseed in deionized water or ethyl alcohol again, repeatedly filters until filtrate
PH value is 7, is distributed in potassium iodide aqueous solution after washing, and water soluble acrylic resin is added, is stirred under room temperature ultrasonic environment
Obtain within 12 hours stable blue conductive dispersions slurry；Black precipitate, potassium iodide, the concentration of water soluble acrylic resin difference
For：10g/L、12g/L、15g/L.
(4) it by slurry for rotary coating or blade coating in material surface, air-dries the painting of polyaniline appendix graphene conductive can be obtained at room temperature
Layer.
As shown in Figure 1, coating is fine and close, surfacing in conventional graphite alkene conductive coating coating surface SEM photograph does not occur
Lamella warpage.
The conductivity of gained coating：748Scm-1；Adhesive force：5B.
Embodiment 2
(1) 0.05mo aniline monomers and 0.15g graphite oxides are added in 50mL acidic aqueous solutions, ultrasonic disperse 2h is obtained
Puce colloidal sol (Sol A), then 0.05mol potassium peroxydisulfates are dissolved in 50mL acidic aqueous solutions, and it is slowly dropped to Sol A
In obtain mixed sols.
(2) by mixed sols that step (1) obtains, constant temperature is stirred to react 16 hours at room temperature, obtains black precipitate；
(3) the black precipitate deionized water and ethyl alcohol obtained step (2) is alternately washed, each time after washing using centrifugation
Machine precipitates or pumping and filtering device is filtered, and filtration product is disperseed in deionized water or ethyl alcohol again, repeatedly filters until filtrate
PH value is 7, is distributed in potassium iodide aqueous solution after washing, and water soluble acrylic resin is added, is stirred under the ultrasonic environment of 60 DEG C of room
It mixes and obtains within 8 hours stable blue conductive dispersions slurry；Black precipitate, potassium iodide, the concentration of water soluble acrylic resin point
It is not：12g/L、17g/L、20g/L.
(4) slurry for rotary coating or blade coating are air-dried at material surface, 70 DEG C and the painting of polyaniline appendix graphene conductive can be obtained
Layer.
The conductivity of gained coating：804Scm-1；Adhesive force：5B.
Embodiment 3
(1) 0.02mol aniline monomers and 0.1g graphite oxides are added in 50mL acidic aqueous solutions, ultrasonic disperse 2h is obtained
Puce colloidal sol (Sol A), then 0.04mol sodium peroxydisulfates are dissolved in 50mL acidic aqueous solutions, and it is slowly dropped to Sol A
In obtain mixed sols.
(2) by mixed sols that step (1) obtains, constant temperature is stirred to react 12 hours at room temperature, obtains black precipitate；
(3) the black precipitate deionized water and ethyl alcohol obtained step (2) is alternately washed, each time after washing using centrifugation
Machine precipitates or pumping and filtering device is filtered, and filtration product is disperseed in deionized water or ethyl alcohol again, repeatedly filters until filtrate
PH value is 7, is distributed in potassium iodide aqueous solution after washing, and water soluble alkyd resin is added, 10 are stirred under room temperature ultrasonic environment
Hour obtains stable blue conductive dispersions slurry；Black precipitate, potassium iodide, the concentration of water soluble alkyd resin are respectively：
10g/L、10g/L、30g/L。
(4) slurry for rotary coating or blade coating are air-dried at material surface, 50 DEG C and the painting of polyaniline appendix graphene conductive can be obtained
Layer.
The conductivity of gained coating：522Scm-1；Adhesive force：4B.
Embodiment 4
(1) 0.03mol aniline monomers and 0.1g graphite oxides are added in 50mL acidic aqueous solutions, ultrasonic disperse 2h is obtained
Puce colloidal sol (Sol A), then 0.05mol ferric trichlorides are dissolved in 50mL acidic aqueous solutions, and it is slowly dropped to Sol A
In obtain mixed sols.
(2) mixed sols that step (1) obtains is put into constant temperature in 50 DEG C of heat-preserving equipments to be stirred to react 18 hours, is obtained black
Color precipitates；
(3) the black precipitate deionized water and ethyl alcohol obtained step (2) is alternately washed, each time after washing using centrifugation
Machine precipitates or pumping and filtering device is filtered, and filtration product is disperseed in deionized water or ethyl alcohol again, repeatedly filters until filtrate
PH value is 7, is distributed in potassium iodide aqueous solution after washing, and water soluble polyurethane resin is added, is stirred under room temperature ultrasonic environment
Obtain within 12 hours stable blue conductive dispersions slurry；Black precipitate, potassium iodide, the concentration of water soluble polyurethane resin difference
For：40g/L、20g/L、15g/L.
(4) slurry for rotary coating or blade coating are air-dried at material surface, 50 DEG C and the painting of polyaniline appendix graphene conductive can be obtained
Layer.The conductivity of gained coating：267Scm-1；Adhesive force：5B.
Claims (6)
1. a kind of production method of polyaniline appendix graphite ene coatings, which is characterized in that include the following steps：
(1) aniline monomer and graphite oxide being added in acidic aqueous solution, ultrasonic disperse obtains puce colloidal sol (Sol A), then
Oxidant is dissolved in acidic aqueous solution, and is slowly dropped in Sol A and obtains mixed sols.
(2) mixed sols that step (1) obtains is put into constant temperature in heat-preserving equipment to be stirred to react, obtains black precipitate；
(3) it is distributed in potassium iodide aqueous solution after washing the black precipitate that step (2) obtains, thickener, room temperature~60 is added
It is stirred under DEG C ultrasonic environment and obtains within 8~12 hours stable blue conductive dispersions slurry；
(4) slurry for rotary coating or blade coating are air-dried at material surface, room temperature~70 DEG C and polyaniline appendix graphene conductive can be obtained
Coating.
2. a kind of production method of polyaniline appendix graphite ene coatings according to claim 1, it is characterised in that：The oxygen
The addition of graphite is 0.2~1.5gL-1；The ultrasonic disperse time is 1~2h.Aniline monomer is a concentration of in last colloidal sol
0.1~0.5molL-1；Acidic aqueous solution pH is less than 2.
3. a kind of production method of polyaniline appendix graphite ene coatings according to claim 1, it is characterised in that：The oxygen
Agent includes one kind or combinations thereof in ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, ferric trichloride, oxidant and aniline monomer
Molar ratio be 1: 1~3: 1.
4. a kind of production method of polyaniline appendix graphite ene coatings according to claim 1, it is characterised in that：The constant temperature
The reaction time being stirred to react is 12~24 hours, and temperature is room temperature~60 DEG C, and washing is alternately washed with deionized water and ethyl alcohol
It washs, uses centrifuge precipitation or pumping and filtering device to be filtered each time after washing, filtration product is again in deionized water or ethyl alcohol
Dispersion, repeated filtration are 6~7 until filtrate pH value.
5. a kind of production method of polyaniline appendix graphite ene coatings according to claim 1, it is characterised in that：The black
The concentration equivalent that precipitation is added in potassium iodide aqueous solution is 10~40g/L, and iodate 10~20g/L of potassium concn, thickener is water-soluble
One kind or combinations thereof in property resin, including water soluble acrylic resin, water soluble alkyd resin, water soluble polyurethane resin,
A concentration of 15~45g/L in potassium iodide aqueous solution is added.
6. poly- made by a kind of production method of the polyaniline appendix graphite ene coatings as described in Claims 1 to 5 any one
Aniline appendix graphite ene coatings.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810288047.0A CN108587446A (en) | 2018-03-26 | 2018-03-26 | A kind of production method of polyaniline appendix graphite ene coatings |
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| CN201810288047.0A CN108587446A (en) | 2018-03-26 | 2018-03-26 | A kind of production method of polyaniline appendix graphite ene coatings |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781459A (en) * | 2010-02-04 | 2010-07-21 | 南京理工大学 | Graphene/polyaniline conductive composite material and preparation method thereof |
| CN103803531A (en) * | 2012-11-14 | 2014-05-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing poly 1,5-diamino-anthraquinone modified graphene nanometer composite material |
| CN105199134A (en) * | 2015-10-12 | 2015-12-30 | 湖北工业大学 | Polyaniline-modified graphene conductive composite film and preparation method thereof |
| CN105273186A (en) * | 2015-11-19 | 2016-01-27 | 浙江大学 | Preparation method of graphene oxide-polyaniline composite electromagnetic shielding material |
| US20160027938A1 (en) * | 2014-07-23 | 2016-01-28 | The Regents Of The University Of Michigan | Tetradymite Layer Assisted Heteroepitaxial Growth And Applications |
| CN107722264A (en) * | 2017-11-23 | 2018-02-23 | 清远初曲智能科技有限公司 | A kind of colloidal sol polyaniline composite graphite alkene conductive material and preparation method thereof |
-
2018
- 2018-03-26 CN CN201810288047.0A patent/CN108587446A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781459A (en) * | 2010-02-04 | 2010-07-21 | 南京理工大学 | Graphene/polyaniline conductive composite material and preparation method thereof |
| CN103803531A (en) * | 2012-11-14 | 2014-05-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing poly 1,5-diamino-anthraquinone modified graphene nanometer composite material |
| US20160027938A1 (en) * | 2014-07-23 | 2016-01-28 | The Regents Of The University Of Michigan | Tetradymite Layer Assisted Heteroepitaxial Growth And Applications |
| CN105199134A (en) * | 2015-10-12 | 2015-12-30 | 湖北工业大学 | Polyaniline-modified graphene conductive composite film and preparation method thereof |
| CN105273186A (en) * | 2015-11-19 | 2016-01-27 | 浙江大学 | Preparation method of graphene oxide-polyaniline composite electromagnetic shielding material |
| CN107722264A (en) * | 2017-11-23 | 2018-02-23 | 清远初曲智能科技有限公司 | A kind of colloidal sol polyaniline composite graphite alkene conductive material and preparation method thereof |
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Application publication date: 20180928 |