CN107936686A - A kind of compound carbon-based water-based electric heating ink of graphene and preparation method thereof - Google Patents
A kind of compound carbon-based water-based electric heating ink of graphene and preparation method thereof Download PDFInfo
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- CN107936686A CN107936686A CN201711273359.6A CN201711273359A CN107936686A CN 107936686 A CN107936686 A CN 107936686A CN 201711273359 A CN201711273359 A CN 201711273359A CN 107936686 A CN107936686 A CN 107936686A
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
We's invention is related to a kind of compound carbon-based water-based electric heating ink of graphene, is made of the component of following mass fractions：Water-base resin adhesive：40 60%；Electric heating filler：15 30%；Functionalization graphene：1 15%；Water：10 30%；Auxiliary agent：3 15%.The ink of the present invention utilizes the high compatibility of special groups and resin in functionalization graphene, improve the stable and uniform of system, so as to improve the problem of water-based ink peels off force difference, bending performance is bad, while abundant conductive radiator functional group makes electric radiation rate bring up to more than 75%.The ink of the present invention belongs to full carbon system ink, exists without metal, safety and environmental protection, electric heating property are stable, not oxidizable, preparation method is simple, are easy to mass production.
Description
Technical field
The present invention relates to the preparing technical field of electric heating ink, more particularly, to a kind of compound carbon-based water-based electric heating of graphene
Ink and preparation method thereof.
Background technology
Under the big Policy Background of country, " coal changes electricity " comes into substantial period, so replacing coal with eco-friendly power source
It is development trend to carry out heating, and wherein electric energy is preferred.The hot-water heating that Far red infrared radiation electrothermal membrane substitutes at this stage is used for heating, has
There is energy conservation and environmental protection, the advantages such as simple, various informative, health-care physical therapy are installed.The common Far red infrared radiation electrothermal membrane of in the market be by
Electric heating ink, metal current-carrying bar are through printing, processing, hot pressing is made between insulating substrate film.Wherein form conductive exothermal coating
Electric heating ink be this kind of product key problem in technology.
Existing electric heating ink is formed with organic solvent and noble metal electric heating particulate mostly, expensive, and pollution is big,
And other metal powders in addition to silver powder are easy to aoxidize and reduce electric heating.Although and the organic electric heating ink of pure carbon powder into
This is cheap, but there are environmental pollution is big, electric stability is poor, the low problem of electric radiation rate, greatly limit it in heating
Formal application.
105001716 A of patent CN 103468057 A and patent CN discloses a kind of Graphene conductive ink, but its body
It is for solvent-borne type, environment can be polluted in preparation process.Also there is a collection of water-based electric heating ink at this stage, but its is attached
Put forth effort the effect for not reaching solvent-based ink, the problem of poor adhesive force, poor in flexibility occur.Such as 105694594 A of patent CN
Process can used as unique conductive heater main body using chemical-treated graphene with 105906832 A of patent CN
It is middle graphitization again occur, cause electrical power to decay.104693897 A of patent CN employ functionalization graphene composite material
The carbon composite of graphene, has essential distinction with the functionalization graphene of this patent.Patent CN201710211519 uses stone
Black alkene, carbon pipe and carbon black set up three-dimensional structure, solve the problems, such as graphitization again, the electrical property decay of graphene, but its only with
Common graphene, and preparation time reaches more than 40h, also needs heating to react, it is actual in adhesive force, electric radiation rate etc.
Specific data are not provided on application performance yet.Because the oxygen content size of graphene, contained by functional group species directly affect it
The conductive radiator of material.
The content of the invention
Exist it is an object of the invention to provide a kind of without metal, make its safety and environmental protection, electric heating property stabilization, be not easy oxygen
Compound carbon-based water-based electric heating ink of graphene of change and preparation method thereof.
The technical solution adopted by the present invention to solve the technical problems is：A kind of compound carbon-based water-based electric heating oil of graphene
Ink, is made of the component of following mass fractions：
Water-base resin adhesive：40-60%；
Electric heating filler：15-30%；
Functionalization graphene：1-15%；
Water：10-30%；
Auxiliary agent：3-15%.
Specifically, the functionalization graphene performance indicator requirement be：At least containing amino, carboxyl, nitro, fluorination work(
One kind in rolling into a ball, oxygen content is below 3%, and piece layer number is at 1-5 layers, and piece footpath is at 1-5 μm.
Specifically, the water-base resin adhesive is selected from water-based acrylic resin, aqueous polyester resin, water-based fluorocarbon tree
One or more of compoundings in fat, water-based silicones.
Specifically, it is fine in 1-20 μm of carbon black, conductive black, carbon nanotubes, carbon to be selected from particle size range for the electric heating filler
One or more of compoundings of dimension.
Specifically, the auxiliary agent includes defoamer, thickener, dispersant, wetting agent, levelling agent, adhesive promoter.
The preparation method of the above-mentioned compound carbon-based water-based electric heating ink of graphene, step are as follows：By water-base resin adhesive, electricity
Hot filler, water, the auxiliary agent in addition to thickener are added in agitator tank in mass fraction ratio, are transferred into and are ground after fully dispersed 1-3h
Grinding machine, after grinding 3-5h reaches 10-20 μm of fineness, viscosity is adjusted to 2000- according to different printing mode thickener
8000mPas obtains the compound carbon-based water-based electric heating ink of graphene.
Specifically, the mode of printing is silk-screen printing or intaglio printing, and silk-screen printing adjusts viscosity to 5000-
8000mPa·s；Intaglio printing adjusts viscosity to 2000-3000mPas.
Specifically, the base material that the mode of printing uses is PET film, PI plates, cotton, fiber, non-woven fabrics or paper.
The invention has the advantages that：The ink of the present invention utilizes special groups and resin in functionalization graphene
High compatibility, improves the stable and uniform of system, so that the problem of water-based ink peels off force difference, bending performance is bad is improved,
Abundant conductive radiator functional group makes electric radiation rate bring up to more than 75% at the same time.The ink of the present invention belongs to full carbon system oil
Ink, exists, safety and environmental protection, electric heating property are stable, not oxidizable, preparation method is simple, are easy to mass production without metal.
Embodiment
It is the specific embodiment of the present invention below, technical scheme is described further, but the present invention
Protection domain is not limited to these embodiments.It is every to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute
Protection domain within.
Experimental method used in following embodiments is conventional method, and reagent used and equipment can be from business ways
Footpath obtains.
Functionalization graphene used in following embodiments is the graphene using independent research, by functional modification
The satisfactory functionalization graphene obtained afterwards：At least contain containing one kind in amino, carboxyl, nitro, fluorination functional group, oxygen
Amount below 3%, piece layer number at 1-5 layers, piece footpath is at 1-2 μm.
In following embodiments in the performance test of ink：
Printing adaptability is tested using base gravure ink proof press and silk-screen printing.
Peeling force be according to《The water-based film gravure compound oil inks of GBT 26394-2011》It is measured.
Bending performance according to《GBT 7287-2008 infrared radiation heater test methods》Tested.
Electric radiation rate according to《JGT 286-2010 low-temp radiating electrothermal membranes》It is measured.
Naked film temperature is that ink is printed onto PET film, after drying, adds copper foil electrode, after connecting 220V voltages, 10min
Test to obtain with infrared radiation thermometer afterwards.
Embodiment 1
52% water-base resin adhesive (aqueous polyester resin：Water-based fluorocarbon resin=2:1)；20% electric heating filler is (conductive
Carbon black：Carbon nanotubes=19:1)；15% functionalization graphene (amino graphene, carboxyl graphene=3:1)；10% water；2%
In addition to thickener auxiliary agent (0.5% dispersant, 0.5% wetting agent, 0.2% levelling agent, 0.3% adhesive promoter, 0.5%
Defoamer).Above raw material is added in agitator tank successively, is sufficiently stirred the laggard grinders of 2h, circular grinding 3h reaches 15 μm
After fineness, viscosity-adjusting agent to 3000mPas is obtained the compound carbon-based water-based electric heating ink of graphene by the thickener for adding 1%.
Embodiment 2
40% water-base resin adhesive (aqueous polyester resin：Water-based fluorocarbon resin=2:1)；20% electric heating filler is (conductive
Carbon black：Carbon nanotubes=19:1)；2% functionalization graphene (amino graphene, nitro graphene=3:1)；30% water；5% removes
Auxiliary agent (2% dispersant, 0.5% wetting agent, 0.5% levelling agent, 1% adhesive promoter, 1% defoamer) outside thickener.
Above raw material is added in agitator tank successively, the laggard grinders of 1h is sufficiently stirred, after circular grinding 5h reaches 10 μm of fineness, adds
Add 3% thickener that viscosity-adjusting agent to 5000mPas is obtained the compound carbon-based water-based electric heating ink of graphene.
Embodiment 3
60% water-base resin adhesive (aqueous polyester resin：Water-based acrylic resin=2:1)；20% electric heating filler (is led
Electric carbon black：Carbon nanotubes=19:1)；2% functionalization graphene (amino graphene, fluorinated graphene=3:1)；14% water；2%
Auxiliary agent (0.5% dispersant, 0.5% wetting agent, 0.5% levelling agent, 0.5% defoamer) in addition to thickener.By above raw material
It is added to successively in agitator tank, is sufficiently stirred the laggard grinders of 3h, after circular grinding 3h reaches 20 μm of fineness, adds 2% increasing
Viscosity-adjusting agent to 8000mPas is obtained the compound carbon-based water-based electric heating ink of graphene by thick dose.
Embodiment 4
52% water-base resin adhesive (water-based silicones：Water-based fluorocarbon resin=2:1)；15% electric heating filler (conductive charcoal
It is black：Carbon fiber=4:1)；6% functionalization graphene (amino graphene, carboxyl graphene=2:1)；12% water；14% except thickening
Auxiliary agent (2% dispersant, 2% wetting agent, 2% levelling agent, 3% adhesive promoter, 5% defoamer) outside agent.Will be former above
Material is added in agitator tank successively, is sufficiently stirred the laggard grinders of 2h, after circular grinding 3h reaches 15 μm of fineness, adds 1%
Viscosity-adjusting agent to 2000mPas is obtained the compound carbon-based water-based electric heating ink of graphene by thickener.
Embodiment 5
52% water-base resin adhesive (water-based fluorocarbon resin：Water-based acrylic resin=2:1)；30% electric heating filler (charcoal
It is black：Conductive black：Carbon nanotubes=9:20:1)；1% functionalization graphene (carboxyl graphene, fluorinated graphene=2:1)；
10% water；6% in addition to thickener auxiliary agent (3% dispersant, 0.5% wetting agent, 0.5% levelling agent, 1% adhesive promoter,
1% defoamer).Above raw material is added in agitator tank successively, is sufficiently stirred the laggard grinders of 2h, circular grinding 3h reaches 10
After μm fineness, viscosity-adjusting agent to 5000mPas is obtained the compound carbon-based water-based electric heating ink of graphene by the thickener for adding 1%.
Comparative example 1
52% water-base resin adhesive (aqueous polyurethane：Water-based acrylic resin=2:1)；22% electric heating filler is (conductive
Carbon black：Carbon nanotubes=10:1)；18% water；7% auxiliary agent (3% dispersant, 0.5% wetting agent, 0.5% stream in addition to thickener
Flat agent, 1% adhesive promoter, 2% defoamer).Above raw material is added in agitator tank successively, is sufficiently stirred that 2h is laggard to be ground
Grinding machine, after circular grinding 3h reaches 15 μm of fineness, viscosity-adjusting agent is obtained graphene by the thickener for adding 1% to 3000mPas
Compound carbon-based water-based electric heating ink.
Comparative example 2
52% water-based acrylic resin adhesive；21% electric heating filler (conductive black：Carbon nanotubes=10:1)；1% work(
Can graphite alkene (amino graphene, carboxyl graphene=3:1)；18% water；7% in addition to thickener auxiliary agent (3% dispersant,
0.5% wetting agent, 0.5% levelling agent, 1% adhesive promoter, 2% defoamer).Above raw material is added to agitator tank successively
In, the laggard grinders of 2h are sufficiently stirred, after circular grinding 3h reaches 15 μm of fineness, the thickener for adding 1% arrives viscosity-adjusting agent
3000mPas obtains the compound carbon-based water-based electric heating ink of graphene.
Performance test
Take above-described embodiment obtain ink, ink is printed onto in PET film, respectively to printing adaptability, peeling force,
Bending performance, electric radiation rate, naked film temperature are tested.Test result see the table below：
As can be seen from the above table, the ink performance prepared in the embodiment of the present invention is considerably beyond comparative example ink.
Claims (8)
1. a kind of compound carbon-based water-based electric heating ink of graphene, it is characterised in that be made of the component of following mass fractions：
Water-base resin adhesive：40-60%；
Electric heating filler：15-30%；
Functionalization graphene：1-15%；
Water：10-30%；
Auxiliary agent：3-15%.
2. the compound carbon-based water-based electric heating ink of graphene as claimed in claim 1, it is characterised in that the functionalization graphene
Performance indicator requirement be：At least containing one kind in amino, carboxyl, nitro, fluorination functional group, oxygen content is below 3%, piece
Layer number is at 1-5 layers, and piece footpath is at 1-5 μm.
3. the compound carbon-based water-based electric heating ink of graphene as claimed in claim 1, it is characterised in that the water-base resin bonding
One or more of in water-based acrylic resin, aqueous polyester resin, water-based fluorocarbon resin, water-based silicones of agent answer
Match somebody with somebody.
4. the compound carbon-based water-based electric heating ink of graphene as claimed in claim 1, it is characterised in that the electric heating filler is selected from
Particle size range is in 1-20 μm of carbon black, conductive black, carbon nanotubes, one or more of compoundings of carbon fiber.
5. the compound carbon-based water-based electric heating ink of graphene as claimed in claim 1, it is characterised in that the auxiliary agent includes defoaming
Agent, thickener, dispersant, wetting agent, levelling agent, adhesive promoter.
6. the preparation method of the compound carbon-based water-based electric heating ink of graphene as described in claim 1-5 is any, it is characterised in that
Step is as follows：Water-base resin adhesive, electric heating filler, water, the auxiliary agent in addition to thickener are added in mass fraction ratio and stirred
Mix in tank, grinder is transferred into after fully dispersed 1-3h, after grinding 3-5h reaches 10-20 μm of fineness, according to different printing mode
Viscosity, which is adjusted, with thickener obtains the compound carbon-based water-based electric heating ink of graphene to 2000-8000mPas.
7. the preparation method of the compound carbon-based water-based electric heating ink of graphene as claimed in claim 6, it is characterised in that the print
Brush mode is silk-screen printing or intaglio printing, and silk-screen printing adjusts viscosity to 5000-8000mPas；Intaglio printing adjusts viscosity
To 2000-3000mPas.
8. the preparation method of the compound carbon-based water-based electric heating ink of graphene as claimed in claim 6, it is characterised in that the print
The base material that brush mode uses is PET film, PI plates, cotton, fiber, non-woven fabrics or paper.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726509A (en) * | 2018-08-08 | 2018-11-02 | 内蒙古石墨烯材料研究院 | A kind of graphene Electric radiant Heating Film and its preparation method and application |
| CN109651891A (en) * | 2018-12-29 | 2019-04-19 | 宁波石墨烯创新中心有限公司 | A kind of graphene water-based composition, preparation method and graphene water-soluble conducting ink |
| CN110054949A (en) * | 2019-03-12 | 2019-07-26 | 北京爱上地科技有限公司 | The compound dye line slurry of aqueous CNTs- graphene, line with heating function and electrothermal cloth |
| CN111155301A (en) * | 2020-01-13 | 2020-05-15 | 苏州艾美医疗用品有限公司 | Graphene needle-punched non-woven fabric and preparation method thereof |
| CN111432508A (en) * | 2020-04-15 | 2020-07-17 | 威海无缝新材料有限公司 | Graphene fast heating film and preparation method thereof |
| CN111887539A (en) * | 2020-07-17 | 2020-11-06 | 武汉世帝牧文化传媒有限公司 | Heating insole |
| CN113563760A (en) * | 2021-07-22 | 2021-10-29 | 桂林清研皓隆新材料有限公司 | Electrothermal ink, preparation method thereof and electrothermal product |
| CN114133791A (en) * | 2021-12-20 | 2022-03-04 | 深圳清华大学研究院 | Conductive ink and super-hydrophobic graphene composite deicing flexible electrothermal film |
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| CN107384148A (en) * | 2017-07-24 | 2017-11-24 | 宁波墨西科技有限公司 | Graphene-based heat radiation coating and preparation method thereof |
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| CN103275552A (en) * | 2013-05-20 | 2013-09-04 | Kmt纳米科技（香港）有限公司 | Carbon electric heating printing ink and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726509A (en) * | 2018-08-08 | 2018-11-02 | 内蒙古石墨烯材料研究院 | A kind of graphene Electric radiant Heating Film and its preparation method and application |
| CN109651891A (en) * | 2018-12-29 | 2019-04-19 | 宁波石墨烯创新中心有限公司 | A kind of graphene water-based composition, preparation method and graphene water-soluble conducting ink |
| CN110054949A (en) * | 2019-03-12 | 2019-07-26 | 北京爱上地科技有限公司 | The compound dye line slurry of aqueous CNTs- graphene, line with heating function and electrothermal cloth |
| CN111155301A (en) * | 2020-01-13 | 2020-05-15 | 苏州艾美医疗用品有限公司 | Graphene needle-punched non-woven fabric and preparation method thereof |
| CN111432508A (en) * | 2020-04-15 | 2020-07-17 | 威海无缝新材料有限公司 | Graphene fast heating film and preparation method thereof |
| CN111887539A (en) * | 2020-07-17 | 2020-11-06 | 武汉世帝牧文化传媒有限公司 | Heating insole |
| CN113563760A (en) * | 2021-07-22 | 2021-10-29 | 桂林清研皓隆新材料有限公司 | Electrothermal ink, preparation method thereof and electrothermal product |
| CN114133791A (en) * | 2021-12-20 | 2022-03-04 | 深圳清华大学研究院 | Conductive ink and super-hydrophobic graphene composite deicing flexible electrothermal film |
| CN114133791B (en) * | 2021-12-20 | 2023-03-10 | 深圳清华大学研究院 | Conductive ink and super-hydrophobic graphene composite deicing flexible electrothermal film |
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