CN110511609A - Aqueous self limiting temperature fever ink of a kind of graphene and preparation method thereof and the application in heating film - Google Patents

Aqueous self limiting temperature fever ink of a kind of graphene and preparation method thereof and the application in heating film Download PDF

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Publication number
CN110511609A
CN110511609A CN201910915858.3A CN201910915858A CN110511609A CN 110511609 A CN110511609 A CN 110511609A CN 201910915858 A CN201910915858 A CN 201910915858A CN 110511609 A CN110511609 A CN 110511609A
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graphene
limiting temperature
self limiting
agent
aqueous
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计晓荣
于永杰
陈昊
程瑾宁
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Jiangsu Kangshengteke High Polymer Conductive Material Co Ltd
WEIHAI YUNSHAN TECHNOLOGY Co Ltd
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Jiangsu Kangshengteke High Polymer Conductive Material Co Ltd
WEIHAI YUNSHAN TECHNOLOGY Co Ltd
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Priority to CN201910915858.3A priority Critical patent/CN110511609A/en
Publication of CN110511609A publication Critical patent/CN110511609A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B32B15/09—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/14—Printing or colouring
    • B32B38/145—Printing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • 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
    • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • 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
    • C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
    • 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
    • C09D11/108—Hydrocarbon resins

Abstract

The present invention relates to graphene applied technical fields, specifically a kind of aqueous self limiting temperature fever ink of graphene and preparation method thereof and the application in heating film, it is characterized in that the aqueous self limiting temperature fever ink of the graphene is by deionized water, graphene slurry, carbon black, PTC functional material, organic additive, lotion composition, the aqueous self limiting temperature fever ink of the graphene of preparation is applied in heating film, the present invention uses modified graphene, it is increased in the middle stability of solvent and lotion, stable conductive path is formed with carbon black again, to there is good adhesive force on insulating substrate PET film, and the addition of PTC functional material, so that Electric radiant Heating Film has self limiting temperature, it is remarkably improved the safety of Electric radiant Heating Film.Preparation process of the present invention is relatively simple, highly effective, has many advantages, such as that component is reasonable, simple process, stability are high, adhesive force is strong, highly-safe.

Description

Aqueous self limiting temperature fever ink of a kind of graphene and preparation method thereof and in heating film In application
Technical field
The present invention relates to graphene applied technical field, specifically a kind of component rationally, simple process, stability Aqueous self limiting temperature fever ink of the graphene high, adhesive force is strong, highly-safe and preparation method thereof and answering in heating film With.
Background technique
It is well known that persistently improve the air quality of area surroundings to accelerate propulsion of the country to cleaning heating policy, Demand of the people to highly effective and safe heating product is more more and more intense, and the appearance of graphene heating product makes up to a certain extent The vacancy in this market, and the preparation of graphene heating product be unable to do without the research and development and preparation of graphene fever ink.
Currently, Chinese patent notification number CN107446408A discloses a kind of PTC graphene fever ink and its preparation side Method, the patent application reduce the security risk of graphene heating film, improve the stability of graphene heating film, but the patent Using oleaginous system, there is certain environmental pollution, and execution conditions are more stringent, is unfavorable for environmental protection.
Chinese patent notification number CN105925052A discloses a kind of preparation method of modified graphene fever ink, this is specially Using ink resin as carrier modified graphene, electrical-conductive nanometer silver and fever nanometer chromium is added, in chemical bond force and molecule in benefit application Between be prepared under the action of power, which is difficult to ensure the stability of ink, is easy to influence electricity in the actual use process Power stability, electric conductivity and the safety of hotting mask, and oily matter not tractable is asked there is also pollution environment, the later period Topic.
Summary of the invention
Present invention aim to address above-mentioned the deficiencies in the prior art, a kind of safety and environmental protection, simple process, stability are provided Aqueous self limiting temperature fever ink of the graphene high, adhesive force is strong, highly-safe and preparation method thereof and answering in heating film With.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of aqueous self limiting temperature fever ink of graphene, it is characterised in that the aqueous self limiting temperature fever ink of the graphene is by deionization Water, graphene slurry, carbon black, PTC functional material, organic additive, lotion composition, the parts by weight of above-mentioned constituent are respectively as follows: 15-40 parts of deionized water, graphene starch 15-35 parts, 0.5-1.5 parts of carbon black, 5-15 parts of PTC functional material, organic additive 2-6 Part, 30-65 parts of lotion.
Lotion described above is styrene-acrylic emulsion, self-cross linking type made of acrylate and styrene and extraordinary monomer copolymerization Pure C system acrylic emulsion or ester modified one of the PU dispersion of aqueous aliphatic poly carbon acetic acid.
PTC functional material described above is aqueous polyethylene wax emulsion, aqueous polyacrylamide wax emulsion, aqueous high density are poly- One of ethylene wax emulsion, aqueous low-density polyethylene wax lotion mix a variety of in any proportion.
Organic additive described above is made of dispersing agent, levelling agent, wetting agent, defoaming agent and thickener, and above-mentioned group At ingredient according to the material composition ratio of mass fraction are as follows: dispersing agent 10%-25%, levelling agent 15%-20%, wetting agent 15%-25%, disappear Infusion 20%-25% and thickener 20%-25%；
Dispersing agent described above is one of polycarboxylic acids, sodium polycarboxylate or polycarboxylic acids amine, and the levelling agent changes for polyurethane Property polyethers association type levelling agent or acrylic acid levelling agent, the wetting agent is aliphatic ester, polyoxyethylene pheynylalkylamine or poly- One of oxy alkylene alkyl ether, the defoaming agent are one of amides, metal soap or silica-based defoaming agent, institute Stating thickener is polyurethane-modified polyethers thickener or polyurethane-modified polyethers association thickener.
A kind of preparation method of the aqueous self limiting temperature fever ink of graphene, it is characterised in that the technique of the preparation method walks It is rapid as follows:
(1) weighs the aqueous self limiting temperature fever ink each component of graphene, and 15-40 parts of deionized water, graphene starch 15-35 parts, charcoal 0.5-1.5 parts black, 5-15 parts of PTC functional material, 2-6 parts of organic additive, 30-65 parts of lotion, wherein organic additive is by dividing Powder, levelling agent, wetting agent, defoaming agent and thickener composition, above-mentioned constituent according to mass fraction material composition ratio are as follows: Dispersing agent 10%-25%, levelling agent 15%-20%, wetting agent 15%-25%, defoaming agent 20%-25% and thickener 20%-25%；
(2) lotion and deionized water are added in reaction kettle after mixing 20min by, put into graphene and carbon black stirring 30min adds PTC functional material, and reaction kettle successively then is added in dispersing agent, levelling agent, wetting agent and defoaming agent and is stirred It is taken out after mixing 30min, is placed in sand mill and is ground to granularity less than 25 μm, be eventually adding thickener, stirred evenly up to graphite The aqueous self limiting temperature fever ink of alkene.
Application of the aqueous self limiting temperature fever ink of a kind of graphene in heating film, it is characterised in that the heating film is by graphite The aqueous self limiting temperature fever ink of alkene, conductive silver paste, PET film, PET strip glue film and copper foil composition
The preparation method step of heating film described above are as follows: thickener is added into the aqueous self limiting temperature fever ink of graphene, 6000 ~ 20000cP of the aqueous self limiting temperature slurry viscosity of graphene is adjusted, then 20 ~ 60min of uniform stirring, it is added in spreader, Coated on the PET film for being printed with conductive silver paste, 100 ~ 400 μm of PET film thickness and then 80 ~ 130 DEG C of 10 ~ 25min of drying glue Attached copper foil, it is hot-forming with PET strip glue film.
The present invention is due to the aqueous self limiting temperature fever ink of the graphene prepared using above-mentioned constituent and process, tool Have the advantages that component is reasonable, simple process, stability are high, adhesive force is strong, highly-safe.
Detailed description of the invention
Fig. 1 is by the heating film of the aqueous self limiting temperature ink preparation of graphene in 1-5 of the embodiment of the present invention in high/low temperature alternation The curve graph that resistance varies with temperature is measured in moisture-heat test-box.
Specific embodiment
The present invention is further described below:
A kind of aqueous self limiting temperature fever ink of graphene, it is characterised in that the aqueous self limiting temperature fever ink of the graphene is by deionization Water, graphene slurry, carbon black, PTC functional material, organic additive, lotion composition, the parts by weight of above-mentioned constituent are respectively as follows: 15-40 parts of deionized water, graphene starch 15-35 parts, 0.5-1.5 parts of carbon black, 5-15 parts of PTC functional material, organic additive 2-6 Part, 30-65 parts of lotion, the lotion are styrene-acrylic emulsion made of acrylate and styrene and extraordinary monomer copolymerization, are selfed Connection type pure C system acrylic emulsion or ester modified one of the PU dispersion of aqueous aliphatic poly carbon acetic acid, described is organic Additive is made of dispersing agent, levelling agent, wetting agent, defoaming agent and thickener, above-mentioned constituent according to mass fraction object Matter ratio of components are as follows: dispersing agent 10%-25%, levelling agent 15%-20%, wetting agent 15%-25%, defoaming agent 20%-25% and thickener 20%-25%, the dispersing agent are one of polycarboxylic acids, sodium polycarboxylate or polycarboxylic acids amine, and the levelling agent changes for polyurethane Property polyethers association type levelling agent or acrylic acid levelling agent, the wetting agent is aliphatic ester, polyoxyethylene pheynylalkylamine or poly- One of oxy alkylene alkyl ether, the defoaming agent are one of amides, metal soap or silica-based defoaming agent, institute Stating thickener is polyurethane-modified polyethers thickener or polyurethane-modified polyethers association thickener, the PTC function Material is aqueous polyethylene wax emulsion, aqueous polyacrylamide wax emulsion, aqueous high density polyethylene waxes lotion, aqueous low density polyethylene One of alkene wax emulsion mixes a variety of in any proportion, and the processing step of the preparation method is as follows: (1) weighs graphite The aqueous self limiting temperature fever ink each component of alkene, 15-40 parts of deionized water, graphene starch 15-35 parts, 0.5-1.5 parts of carbon black, PTC 5-15 parts of functional material, 2-6 parts of organic additive, 30-65 parts of lotion, wherein organic additive is by dispersing agent, levelling agent, wetting Agent, defoaming agent and thickener composition, above-mentioned constituent according to mass fraction material composition ratio are as follows: dispersing agent 10%-25%, stream Flat agent 15%-20%, wetting agent 15%-25%, defoaming agent 20%-25% and thickener 20%-25%；(2) adds lotion and deionized water It is added to after 20min is mixed in reaction kettle, puts into graphene and carbon black stirs 30min, add PTC functional material, then Reaction kettle successively is added in dispersing agent, levelling agent, wetting agent and defoaming agent and is taken out after stirring 30min, is placed in sand mill and grinds Granularity is milled to less than 25 μm, is eventually adding thickener, is stirred evenly up to the aqueous self limiting temperature fever ink of graphene.
Application of the aqueous self limiting temperature fever ink of a kind of graphene in heating film, it is characterised in that the heating film is by graphite The aqueous self limiting temperature fever ink of alkene, conductive silver paste, PET film, PET strip glue film and copper foil composition.The preparation side of the heating film Method step are as follows: thickener is added into the aqueous self limiting temperature fever ink of graphene, adjusts the aqueous self limiting temperature slurry viscosity of graphene 6000 ~ 20000cP, then 20 ~ 60min of uniform stirring, it is added in spreader, coated in the PET for being printed with conductive silver paste On film, then 80 ~ 130 DEG C of 10 ~ 25min of drying, adherency copper foil are hot-forming with PET strip glue film for 100 ~ 400 μm of PET film thickness.
The beneficial effects of the present invention are: lotion described in ingredient: selection is water-based emulsion, working condition more ring It protects, the graphene and carbon black: the two is used in conjunction with each other, and makes the conductive effect of system more preferably, the PTC function material Material: increasing the functionality of slurry, and the slurry of preparation has ptc characteristics, the dispersing agent: divides graphene and carbon black preferably Be dispersed in system, the defoaming agent: the ink for producing preparation can defoam faster, the levelling agent: so that ink exists When film forming more uniformly, naturally, the wetting agent: reduce surface tension, increase the adhesive force with substrate, improve ink Film forming, the present invention has good adhesive force, and the addition of PTC functional material on insulating substrate PET film, so that electric heating Film has self limiting temperature, is remarkably improved the safety of Electric radiant Heating Film.Preparation process of the present invention is relatively simple, highly effective.
Embodiment 1
A kind of aqueous self limiting temperature fever ink of graphene, score meter, including following component by weight: 15 parts of deionized water, graphite Alkene starches 15 parts, 1.5 parts of carbon black, 5 parts of aqueous polyethylene wax emulsion, 6 parts of organic additive and acrylate and styrene and special type 65 parts of styrene-acrylic emulsion made of monomer copolymerization；
Wherein, organic additive by following mass fraction material composition: dispersing agent polycarboxylic acids 10%, polyurethane-modified polyethers Association type levelling agent 20%, wetting agent aliphatic ester 25%, amides defoaming agent 25% and polyurethane-modified polyethers thickener 20%.
The preparation method of the present embodiment graphene aqueous self limiting temperature fever ink and self limiting temperature heating film the following steps are included:
Prepare the aqueous self limiting temperature fever ink of graphene
The aqueous self limiting temperature fever ink each component of graphene is weighed by weight, and lotion and deionized water are added in reaction kettle After 20min is mixed, puts into graphene and carbon black and stir 30min, add PTC functional material, then successively by dispersing agent, Levelling agent, wetting agent and defoaming agent are added reaction kettle and take out after stirring 30min, are placed in sand mill and are ground to granularity less than 25 μm, it is eventually adding thickener, stirs evenly to obtain the final product.
Prepare the aqueous self limiting temperature heating film of graphene
Present embodiments provide a kind of heating film using the above-mentioned resulting aqueous self limiting temperature ink preparation of graphene, the fever Film includes that appropriate polyurethane-modified polyethers thickener is added, and the viscosity of the aqueous self limiting temperature slurry of graphene is adjusted to need Degree, then uniform stirring 20min is added in spreader, is printed on 110 μm of PET film for being printed on conductive silver paste, Then 80 DEG C of drying 20 adhere to copper foil, hot-forming with 100 μm of PET strip glue film.
Embodiment 2
A kind of aqueous self limiting temperature fever ink of graphene, score meter, including following component by weight: 25 parts of deionized water, graphite 25 parts of alkene slurry, 1 part of carbon black, 10 parts of aqueous low-density polyethylene wax lotion, 4 parts of organic additive and aqueous aliphatic poly carbon acetic acid 50 parts of ester modified PU dispersion；
Wherein, organic additive by following mass fraction material composition: dispersing agent sodium polycarboxylate 20%, levelling agent acrylic acid 15%, wetting agent polyoxyethylene pheynylalkylamine 20%, metal soap defoaming agent 22% and polyurethane-modified polyethers association thickener 23%。
The preparation method of the present embodiment graphene aqueous self limiting temperature fever ink and self limiting temperature heating film the following steps are included:
Prepare the aqueous self limiting temperature fever ink of graphene
The aqueous self limiting temperature fever ink each component of graphene is weighed by weight, and lotion and deionized water are added in reaction kettle After 20min is mixed, puts into graphene and carbon black and stir 30min, add PTC functional material, then successively by dispersing agent, Levelling agent, wetting agent and defoaming agent are added reaction kettle and take out after stirring 30min, are placed in sand mill and are ground to granularity less than 25 μm, it is eventually adding thickener, stirs evenly to obtain the final product.
Prepare the aqueous self limiting temperature heating film of graphene
Present embodiments provide a kind of heating film using the above-mentioned resulting aqueous self limiting temperature ink preparation of graphene, the fever Film includes that appropriate polyurethane-modified polyethers association thickener is added, and the viscosity of the aqueous self limiting temperature slurry of graphene is adjusted To the degree of needs, then uniform stirring 40min, is added in spreader, is printed on and has been printed on 150 μm of conductive silver paste On PET film, then 100 DEG C of drying adhere to copper foil, hot-forming with 150 μm of PET strip glue film.
Embodiment 3
A kind of aqueous self limiting temperature fever ink of graphene, score meter, including following component by weight: 35 parts of deionized water, graphite Alkene starches 35 parts, 0.5 part of carbon black, aqueous polyethylene wax emulsion and aqueous low-density polyethylene wax lotion is 15 parts each, organic additive 2 Part, self-cross linking type pure C system acrylic emulsion and ester modified each 30 parts of PU dispersion of aqueous aliphatic poly carbon acetic acid.
Wherein, organic additive by following mass fraction material composition: dispersing agent polycarboxylic acids amine 25%, levelling agent propylene Acid 15%, wetting agent polyoxy alkenyl alkyl ethers 15%, silica 20% and polyurethane-modified polyethers thickener 25%.
The preparation method of the present embodiment graphene aqueous self limiting temperature fever ink and self limiting temperature heating film the following steps are included:
Prepare the aqueous self limiting temperature fever ink of graphene
The aqueous fever ink each component of graphene is weighed by weight, and lotion and deionized water are added to mixing in reaction kettle and stirred After mixing 20min, put into graphene and carbon black and stir 30min, add PTC functional material, then successively by dispersing agent levelling agent, Wetting agent and defoaming agent are added reaction kettle and take out after stirring 30min, are placed in sand mill and are ground to granularity less than 25 μm, finally Thickener is added, stirs evenly to obtain the final product.
Prepare the aqueous self limiting temperature heating film of graphene
Present embodiments provide a kind of heating film using the above-mentioned resulting aqueous self limiting temperature ink preparation of graphene, the fever Film includes that appropriate polyurethane-modified polyethers thickener is added, and the viscosity of the aqueous self limiting temperature slurry of graphene is adjusted to need Degree, then uniform stirring 60min is added in spreader, is printed on 200 μm of PET film for being printed on conductive silver paste, Then 120 DEG C of drying adhere to copper foil, hot-forming with 150 μm of PET strip glue film.
Embodiment 4
A kind of aqueous self limiting temperature fever ink of graphene, score meter, including following component by weight: 18 parts of deionized water, graphite 23 parts of alkene slurry, 0.6 part of carbon black, 30 parts of aqueous polyethylene wax emulsion, 2 parts of organic additive, aqueous aliphatic poly carbon acetate change 40 parts of PU dispersion of property.
Wherein, organic additive by following mass fraction material composition: dispersing agent polycarboxylic acids amine 25%, levelling agent propylene Acid 15%, wetting agent polyoxy alkenyl alkyl ethers 15%, silica 20% and polyurethane-modified polyethers thickener 25%.
The preparation method of the present embodiment graphene aqueous self limiting temperature fever ink and self limiting temperature heating film the following steps are included:
Prepare the aqueous self limiting temperature fever ink of graphene
The aqueous fever ink each component of graphene is weighed by weight, and lotion and deionized water are added to mixing in reaction kettle and stirred After mixing 20min, puts into graphene and carbon black stirs 30min, PTC functional material is added, then successively by dispersing agent, levelling Agent, wetting agent and defoaming agent are added reaction kettle and take out after stirring 30min, are placed in sand mill and are ground to granularity less than 25 μm, It is eventually adding thickener, stirs evenly to obtain the final product.
Prepare the aqueous self limiting temperature heating film of graphene
Present embodiments provide a kind of heating film using the above-mentioned resulting aqueous self limiting temperature ink preparation of graphene, the fever Film includes that appropriate polyurethane-modified polyethers thickener is added, and the viscosity of the aqueous self limiting temperature slurry of graphene is adjusted to need Degree, then uniform stirring 60min is added in spreader, is printed on 120 μm of PET film for being printed on conductive silver paste, Then 120 DEG C of drying 10min adhere to copper foil, hot-forming with 180 μm of PET strip glue film.
Embodiment 5
A kind of aqueous self limiting temperature fever ink of graphene, score meter, including following component by weight: 20 parts of deionized water, graphite Alkene starches 26 parts, 1 part of carbon black, 10 parts of aqueous polyethylene wax emulsion, 10 parts of aqueous polyacrylamide wax emulsion, 2 parts of organic additive, propylene The acid esters PU dispersion ester modified with styrene-acrylic emulsion made of styrene and extraordinary monomer copolymerization and aqueous aliphatic poly carbon acetic acid Each 32 parts
Wherein, organic additive by following mass fraction material composition: dispersing agent polycarboxylic acids amine 25%, levelling agent acrylic acid 15%, wetting agent polyoxy alkenyl alkyl ethers 15%, silica 20% and polyurethane-modified polyethers thickener 25%.
The preparation method of the present embodiment graphene aqueous self limiting temperature fever ink and self limiting temperature heating film the following steps are included:
Prepare the aqueous self limiting temperature fever ink of graphene
The aqueous fever ink each component of graphene is weighed by weight, and lotion and deionized water are added to mixing in reaction kettle and stirred After mixing 20min, puts into graphene and carbon black stirs 30min, PTC functional material is added, then successively by dispersing agent, levelling Agent, wetting agent and defoaming agent are added reaction kettle and take out after stirring 30min, are placed in sand mill and are ground to granularity less than 25 μm, It is eventually adding thickener, stirs evenly to obtain the final product.
Prepare the aqueous self limiting temperature heating film of graphene
Present embodiments provide a kind of heating film using the above-mentioned resulting aqueous self limiting temperature ink preparation of graphene, the fever Film includes that appropriate polyurethane-modified polyethers thickener is added, and the viscosity of the aqueous self limiting temperature slurry of graphene is adjusted to need Degree, then uniform stirring 55min is added in spreader, is printed on 225 μm of PET film for being printed on conductive silver paste, Then 95 DEG C of drying 13min adhere to copper foil, hot-forming with 135 μm of PET strip glue film.
In the present invention, to the heating film prepared in embodiment 1-5 by the aqueous self limiting temperature ink of graphene in high/low temperature alternation The curve (such as Fig. 1) that resistance varies with temperature is measured in moisture-heat test-box.
Following test result is obtained from figure: the heating film of the aqueous self limiting temperature fever ink preparation of graphene has from limit Temperature characteristics realize self limiting temperature function, and when electric heating film temperature constantly increases, resistance is also being continuously improved, and the power of Electric radiant Heating Film will It reducing, the heat of generation will reduce, and improve the safety of Electric radiant Heating Film to a certain extent, reduce security risk, and its Aqueous material, not can cause environmental pollution, and meet energy-saving and emission-reduction reality.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (8)

  1. The ink 1. a kind of aqueous self limiting temperature of graphene is generated heat, it is characterised in that the aqueous self limiting temperature fever ink of the graphene by go from Sub- water, graphene slurry, carbon black, PTC functional material, organic additive, lotion composition, the parts by weight difference of above-mentioned constituent Are as follows: 15-40 parts of deionized water, graphene starch 15-35 parts, 0.5-1.5 parts of carbon black, 5-15 parts of PTC functional material, organic additive 2-6 parts, 30-65 parts of lotion.
  2. The ink 2. a kind of aqueous self limiting temperature of graphene according to claim 1 is generated heat, it is characterised in that the lotion is Styrene-acrylic emulsion made of acrylate is copolymerized with styrene and extraordinary monomer, self-cross linking type pure C system acrylic emulsion or aqueous Ester modified one of the PU dispersion of aliphatic poly carbon acetic acid.
  3. The ink 3. the aqueous self limiting temperature of a kind of graphene according to claim 1 is generated heat, it is characterised in that the PTC function Material is aqueous polyethylene wax emulsion, aqueous polyacrylamide wax emulsion, aqueous high density polyethylene waxes lotion, aqueous low density polyethylene One of alkene wax emulsion mixes a variety of in any proportion.
  4. The ink 4. a kind of aqueous self limiting temperature of graphene according to claim 1 is generated heat, it is characterised in that described organic to add Add agent to be made of dispersing agent, levelling agent, wetting agent, defoaming agent and thickener, above-mentioned constituent according to mass fraction substance Ratio of components are as follows: dispersing agent 10%-25%, levelling agent 15%-20%, wetting agent 15%-25%, defoaming agent 20%-25% and thickener 20%- 25%。
  5. The ink 5. a kind of aqueous self limiting temperature of graphene according to claim 4 is generated heat, it is characterised in that the dispersing agent is One of polycarboxylic acids, sodium polycarboxylate or polycarboxylic acids amine, the levelling agent be polyurethane-modified polyethers association type levelling agent or Acrylic acid levelling agent, the wetting agent are one of aliphatic ester, polyoxyethylene pheynylalkylamine or polyoxy alkenyl alkyl ethers, institute Stating defoaming agent is one of amides, metal soap or silica-based defoaming agent, and the thickener is polyurethane-modified poly- Ethers thickener or polyurethane-modified polyethers association thickener.
  6. 6. a kind of preparation method of the aqueous self limiting temperature fever ink of graphene, it is characterised in that the processing step of the preparation method It is as follows:
    (1) weighs the aqueous self limiting temperature fever ink each component of graphene, and 15-40 parts of deionized water, graphene starch 15-35 parts, charcoal 0.5-1.5 parts black, 5-15 parts of PTC functional material, 2-6 parts of organic additive, 30-65 parts of lotion, wherein organic additive is by dividing Powder, levelling agent, wetting agent, defoaming agent and thickener composition, above-mentioned constituent according to mass fraction material composition ratio are as follows: Dispersing agent 10%-25%, levelling agent 15%-20%, wetting agent 15%-25%, defoaming agent 20%-25% and thickener 20%-25%；
    (2) lotion and deionized water are added in reaction kettle after mixing 20min by, put into graphene and carbon black stirring 30min adds PTC functional material, and reaction kettle successively then is added in dispersing agent, levelling agent, wetting agent and defoaming agent and is stirred It is taken out after mixing 30min, is placed in sand mill and is ground to granularity less than 25 μm, be eventually adding thickener, stirred evenly up to graphite The aqueous self limiting temperature fever ink of alkene.
  7. 7. a kind of application of aqueous self limiting temperature fever ink of graphene in heating film, it is characterised in that the heating film is by graphene Aqueous self limiting temperature fever ink, conductive silver paste, PET film, PET strip glue film and copper foil composition.
  8. 8. a kind of application of the aqueous self limiting temperature fever ink of graphene according to claim 1 in heating film, feature It is the preparation method step of the heating film are as follows: thickener is added into the aqueous self limiting temperature fever ink of graphene, adjusts Graphene 6000 ~ 20000cP of aqueous self limiting temperature slurry viscosity, then 20 ~ 60min of uniform stirring, it is added in spreader, coating On the PET film for being printed with conductive silver paste, 100 ~ 400 μm of PET film thickness and then 80 ~ 130 DEG C of 10 ~ 25min of drying adhere to copper Foil, it is hot-forming with PET strip glue film.
CN201910915858.3A 2019-09-26 2019-09-26 Aqueous self limiting temperature fever ink of a kind of graphene and preparation method thereof and the application in heating film Pending CN110511609A (en)

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CN111287003A (en) * 2020-03-30 2020-06-16 新材料与产业技术北京研究院 Water-based graphene PTC conductive dye, preparation method thereof and conductive fiber treated by dye
CN111607292A (en) * 2020-05-26 2020-09-01 湖南烯源新材科技有限公司 Novel PTC heating ink, preparation method thereof and application thereof in electrothermal film
CN111628248A (en) * 2020-05-26 2020-09-04 湖南烯源新材科技有限公司 Power battery self-temperature-limiting graphene heating film assembly and preparation method of heating film thereof
CN111849338A (en) * 2020-07-30 2020-10-30 佛山(华南)新材料研究院 Self-dispersion aqueous electric heating slurry and preparation method thereof
CN112593415A (en) * 2020-12-01 2021-04-02 肃宁县中原纺织有限责任公司 Water-based graphene flame-retardant PTC conductive paste, preparation method thereof and flexible conductive heating cloth
CN112999200A (en) * 2021-03-03 2021-06-22 张铿 Transdermal drug delivery layer
CN113004741A (en) * 2021-03-05 2021-06-22 苏州大学 Water-based intelligent far infrared functional ink, preparation method and application in heating film
CN113436805A (en) * 2021-04-29 2021-09-24 哈工大机器人集团(无锡)科创基地研究院 Preparation method and application of low-silver aqueous conductive silver paste
CN114181563A (en) * 2021-12-20 2022-03-15 深圳清华大学研究院 High-rate self-temperature-control graphene powder, self-temperature-control ink and graphene self-temperature-control heating coating
CN114231093A (en) * 2021-12-27 2022-03-25 东莞市博恩复合材料有限公司 PTC heat-conducting ink and preparation method thereof
WO2022120565A1 (en) * 2020-12-08 2022-06-16 苏州烯时代材料科技有限公司 Graphene heating ink, preparation method therefor, and application thereof

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CN111287003A (en) * 2020-03-30 2020-06-16 新材料与产业技术北京研究院 Water-based graphene PTC conductive dye, preparation method thereof and conductive fiber treated by dye
CN111287003B (en) * 2020-03-30 2022-09-09 新材料与产业技术北京研究院 Water-based graphene PTC conductive dye, preparation method thereof and conductive fiber treated by dye
CN111607292A (en) * 2020-05-26 2020-09-01 湖南烯源新材科技有限公司 Novel PTC heating ink, preparation method thereof and application thereof in electrothermal film
CN111628248A (en) * 2020-05-26 2020-09-04 湖南烯源新材科技有限公司 Power battery self-temperature-limiting graphene heating film assembly and preparation method of heating film thereof
CN111628248B (en) * 2020-05-26 2021-08-24 湖南烯源新材科技有限公司 Power battery self-temperature-limiting graphene heating film assembly and preparation method of heating film thereof
CN111849338A (en) * 2020-07-30 2020-10-30 佛山(华南)新材料研究院 Self-dispersion aqueous electric heating slurry and preparation method thereof
CN112593415A (en) * 2020-12-01 2021-04-02 肃宁县中原纺织有限责任公司 Water-based graphene flame-retardant PTC conductive paste, preparation method thereof and flexible conductive heating cloth
WO2022120565A1 (en) * 2020-12-08 2022-06-16 苏州烯时代材料科技有限公司 Graphene heating ink, preparation method therefor, and application thereof
CN112999200A (en) * 2021-03-03 2021-06-22 张铿 Transdermal drug delivery layer
CN112999200B (en) * 2021-03-03 2024-04-09 北京昊澄生物科技有限公司 Transdermal drug delivery layer
CN113004741A (en) * 2021-03-05 2021-06-22 苏州大学 Water-based intelligent far infrared functional ink, preparation method and application in heating film
CN113436805A (en) * 2021-04-29 2021-09-24 哈工大机器人集团(无锡)科创基地研究院 Preparation method and application of low-silver aqueous conductive silver paste
CN114181563A (en) * 2021-12-20 2022-03-15 深圳清华大学研究院 High-rate self-temperature-control graphene powder, self-temperature-control ink and graphene self-temperature-control heating coating
CN114231093A (en) * 2021-12-27 2022-03-25 东莞市博恩复合材料有限公司 PTC heat-conducting ink and preparation method thereof

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