CN109666339A - Electric heating ink and preparation method thereof - Google Patents

Electric heating ink and preparation method thereof Download PDF

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Publication number
CN109666339A
CN109666339A CN201910141372.9A CN201910141372A CN109666339A CN 109666339 A CN109666339 A CN 109666339A CN 201910141372 A CN201910141372 A CN 201910141372A CN 109666339 A CN109666339 A CN 109666339A
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China
Prior art keywords
electric heating
weight
ink
parts
heating ink
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CN201910141372.9A
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Inventor
张佑专
张建军
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New Austrian Graphene Technology Co Ltd
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New Austrian Graphene Technology Co Ltd
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Priority to CN201910141372.9A priority Critical patent/CN109666339A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/033Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/102Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/102Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • C09D11/104Polyesters
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/106Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09D11/107Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof

Abstract

The present invention provides electric heating ink and preparation method thereof.Electric heating ink includes: the three-dimensional grapheme of 2~25 parts by weight;The resin of 3~25 parts by weight;The conductive auxiliary agent of 2~25 parts by weight;The oiliness organic solvent of 30~93 parts by weight.Thus, three-dimensional grapheme can both form effective conductive network in two-dimensional surface, and three-dimensional grapheme can also further increase the contact dimension of conductive material as conductive material in three-dimensional space, and then the electric conductivity of electric heating ink is improved, the further dosage for reducing conductive auxiliary agent;And skeleton can also be played the role of in electric heating ink and the ink film layer obtained by the electric heating oil ink print, stability of ink film layer during electrification heat-producing is helped to improve, and then extend the service life of ink film layer;The dosage of the resin of cementation can have additionally been reduced, and then can reduce or avoid ink film layer to occur the risk that resin resets the decaying of bring power during heating repeatedly, heating up cooling.

Description

Electric heating ink and preparation method thereof
Technical field
The present invention relates to technical field of ink, specifically, being related to electric heating ink and preparation method thereof.
Background technique
An important class of the carbon system ink as electric heating ink, has applied many years, main conductive filler is The materials such as carbon black, graphite and carbon fiber, since 2000, with novel-sections such as the nano-scale carbon materials such as carbon nanotube and graphene Material is found in succession, the range of choice of the conductive filler further increased, and above-mentioned new material has stronger building conductive The ability of network, is also widely applied.
It, can also be conductive using being promoted although the introducing of these novel nano carbon materials can not only obtain better electric conductivity The intensity of layer, but these nano-carbon materials, since manufacturing process is complex, the cost is relatively high, therefore the use in ink Amount cannot be too big, and there is also amount of resins risks such as big, ink film layer power attenuation.
Research accordingly, with respect to electric heating ink needs to be goed deep into.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention One purpose is to propose a kind of electric heating ink, electric heating ink preparation process is simple, easy to operate, at low cost, amount of resin is few, The electric conductivity of the ink film layer obtained after or the ink good to the wetability of substrate printing film forming, electric radiation transformation efficiency compared with Good or service life is longer.
In one aspect of the invention, the present invention provides a kind of electric heating ink.According to an embodiment of the invention, the electricity Hot oil ink includes: the three-dimensional grapheme of 2~25 parts by weight;The resin of 3~25 parts by weight;The conductive auxiliary agent of 2~25 parts by weight;30 The oiliness organic solvent of~93 parts by weight.Three-dimensional grapheme can both form effective conductive network in two-dimensional surface as a result, Three-dimensional grapheme can also further increase the contact dimension of conductive material, Jin Erti as conductive material in three-dimensional space The electric conductivity of high electric heating ink, the further dosage for reducing conductive auxiliary agent;And it can also be in electric heating ink and by the electric heating Play the role of skeleton in the ink film layer that ink prints, it is steady during electrification heat-producing to help to improve ink film layer It is qualitative, and then extend the service life of ink film layer;In addition, as previously mentioned, three-dimensional grapheme can be in the ink film layer In play the role of skeleton, in this way, the dosage of the resin of cementation can have been reduced, and then can reduce or avoid ink film There is the risk that resin resets the decaying of bring power during heating repeatedly, heating up cooling in layer.
According to an embodiment of the invention, the electric heating ink further includes at least one of: first point of 0~1 parts by weight Powder;Second dispersing agent of 0~10 parts by weight;The auxiliary agent of 0~1 parts by weight.
According to an embodiment of the invention, the resin is selected from polyester resin, epoxy resin, polyurethane resin and acrylic acid tree At least one of rouge;The conductive auxiliary agent is selected from least one of carbon nanotube, carbon black, acetylene black and graphite;The oil Property organic solvent is in cyclohexanone, ethyl acetate, dibasic acid ester mixed liquor, propylene glycol methyl ether acetate and ethyl carbitol It is at least one.
According to an embodiment of the invention, first dispersing agent is selected from polyvinylpyrrolidone (PVP), cetyl three Methyl bromide ammonium (CATB), neopelex (SDBS), lauryl sodium sulfate (SDS) etc.;State the choosing of the second dispersing agent From sodium carboxymethylcellulose (CMC), ethyl cellulose (EC), polyacrylic acid (PAA), polyethylene glycol (PEG) etc.;;The auxiliary agent Selected from wetting dispersing agent, defoaming agent, levelling agent, coalescing agent and at least one of adhesion promoter and substrate wetting agents.
According to an embodiment of the invention, the solid content of the electric heating ink is 7%~45%.
According to an embodiment of the invention, 4500~64500cps of viscosity of the electric heating ink.
According to an embodiment of the invention, the fineness of the electric heating ink is less than or equal to 50 microns.
In the other side of this hair invention, the present invention provides a kind of methods for preparing electric heating ink noted earlier.Root According to the embodiment of the present invention, the method for preparing electric heating ink includes: to dissolve resin in a part of oiliness organic solvent, To obtain the first mixed liquor;First mixed liquor is uniformly mixed with three-dimensional grapheme, to obtain the second mixed liquor;It will The mixing of oiliness organic solvent described in second mixed liquor, conductive auxiliary agent and another part, to obtain the electric heating ink.By This, above-mentioned preparation method simple operations, easy to industrialized production, preparation cost is low, and in the above preparation method, three-dimensional stone Black alkene can both form effective conductive network in two-dimensional surface, and three-dimensional grapheme, can also be in three-dimensional as conductive material The contact dimension of conductive material is further increased in space, and then improves the electric conductivity of obtained electric heating ink, it is further to drop The dosage of low conductive auxiliary agent;And bone can also be played in electric heating ink and the ink film layer obtained by the electric heating oil ink print The effect of frame helps to improve stability of ink film layer during electrification heat-producing, and then extends the use longevity of ink film layer Life;In addition, as previously mentioned, three-dimensional grapheme can play the role of skeleton in ink film layer, in this way, bonding can have been reduced The dosage of the resin of effect, and then can reduce or avoid ink film layer tree during heating repeatedly, heating up cooling Rouge resets the risk of bring power decaying.
According to an embodiment of the invention, being carried out at grinding after second mixed liquor and the conductive auxiliary agent are mixed Reason, and oiliness organic solvent described in another part is added during the milled processed, to obtain the electric heating ink.
According to an embodiment of the invention, the step of preparing second mixed liquor includes: by first mixed liquor, described Three-dimensional grapheme is uniformly mixed at least one of the first dispersing agent and the second dispersing agent;Optional, in the milled processed Further include the steps that auxiliary agent is added later.
Specific embodiment
The embodiment of the present invention is described below in detail.The embodiments described below is exemplary, and is only used for explaining this hair It is bright, and be not considered as limiting the invention.Particular technique or condition are not specified in embodiment, according to text in the art It offers described technology or conditions or is carried out according to product description.Reagents or instruments used without specified manufacturer, For can be with conventional products that are commercially available.
In one aspect of the invention, the present invention provides a kind of electric heating ink.According to an embodiment of the invention, the electricity Hot oil ink includes: the three-dimensional grapheme of 2~25 parts by weight;The resin of 3~25 parts by weight;The conductive auxiliary agent of 2~25 parts by weight;30 The oiliness organic solvent of~93 parts by weight.Three-dimensional grapheme can both form effective conductive network in two-dimensional surface as a result, Three-dimensional grapheme can also further increase the contact dimension of conductive material, Jin Erti as conductive material in three-dimensional space The electric conductivity of high electric heating ink, the further dosage for reducing conductive auxiliary agent;And it can also be in electric heating ink and by the electric heating Play the role of skeleton in the ink film layer that ink prints, it is steady during electrification heat-producing to help to improve ink film layer It is qualitative, and then extend the service life of ink film layer;In addition, as previously mentioned, three-dimensional grapheme can be in the ink film layer In play the role of skeleton, in this way, the dosage of the resin of cementation can have been reduced, and then can reduce or avoid ink film There is the risk of resin rearrangement reaction bring power decaying during heating repeatedly, heating up cooling in layer.
According to an embodiment of the invention, the number of plies of three-dimensional grapheme is there is no limit requirement, those skilled in the art can root According to actual demand flexible choice, in some embodiments of the invention, the number of plies of three-dimensional grapheme is less than 10 layers, such as 9 layers, 7 Layer, 6 layers, 5 layers, 4 layers, 3 layers, 2 layers or one layer.According to an embodiment of the invention, the preparation method of three-dimensional grapheme does not also limit System requires, and those skilled in the art can be using any method for preparing three-dimensional grapheme in the prior art.
According to an embodiment of the invention, in order to improve the caking property in electric heating ink between each component, resin is selected from polyester At least one of resin, epoxy resin, polyurethane resin and acrylic resin.Electric heating oil not only can be effectively promoted as a result, Caking property in ink between each component, it can also be ensured that prepare ink film layer with mechanical properties such as preferable hardness.
According to an embodiment of the invention, in order to be effectively improved the electric conductivity of electric heating ink, conductive auxiliary agent be selected from carbon nanotube, At least one of carbon black, acetylene black and graphite.Not only material source is extensive as a result, but also can be very good to promote electric heating oil The electric conductivity of ink, and then improve the electric radiation transformation efficiency of ink film layer.Wherein, not only electric conductivity is preferable for carbon nanotube, and And the intensity of ink film layer can also be promoted, but since carbon nanotube preparation process is more many and diverse, higher cost, in terms of cost Consider, the dosage of carbon nanotube should not be excessive, (uses two-dimensional graphene) in the prior art, adds a small amount of carbon nanotube not The electric conductivity of electric heating ink can be promoted well.In the present invention, as previously mentioned, the three-dimensional grapheme of three-dimensional grapheme both can be with Effective conductive network is formed in two-dimensional surface, three-dimensional grapheme, can also be in three-dimensional space into one as conductive material Step increases the contact dimension of conductive material, and then improves the electric conductivity of electric heating ink, so adding in technical solution of the present invention On a small quantity (such as 2 parts by weight, 3 parts by weight, 4 parts by weight, 5 parts by weight, 6 parts by weight, 7 parts by weight, 8 parts by weight or 9 parts by weight) Carbon nanotube can effectively promote the electric conductivity of electric heating ink, and then meet the use demand of electric heating ink, improve ink film The electric radiation conversion ratio of layer.
Since existing substrate is usually polyethylene terephthalate (PET) material or epoxide resin material, and above-mentioned material Material is lipophile material, i.e. hydrophobicity is preferable, and those skilled in the art use hydrophilic solvent at present, so just need Hydrophily processing is carried out to substrate in advance, printing process is relatively complicated as a result, and it is also possible to leads to the regional area of substrate Hydrophily processing is bad, and then causes the electric heating ink at the region poor to the wetability of substrate, and then influences ink film layer Total quality.For this purpose, in order to improve electric heating ink to the wetability of substrate, according to an embodiment of the invention, oiliness is organic molten Agent in cyclohexanone, ethyl acetate, dibasic acid ester mixed liquor, propylene glycol methyl ether acetate and ethyl carbitol at least one Kind.Oiliness organic solvent is selected as a result, without being surface-treated to substrate, and can be effectively improved electric heating ink to substrate Wetability, and then be convenient for electric heating ink printing.
According to an embodiment of the invention, electric heating ink is also in order to improve the uniformity of each component dispersion in electric heating ink Including at least one of: the first dispersing agent of 0~1 parts by weight;Second dispersing agent of 0~10 parts by weight;0~1 parts by weight Auxiliary agent.The addition of first dispersing agent and/or the second dispersing agent as a result, can be effectively improved each component dispersion in electric heating ink Uniformity, and then promoted electric heating ink performance uniformity, and then by the electric heating ink prepare ink film layer different location The electric conductivity at place is more uniform;The addition of auxiliary agent can promote electric heating ink to the wetability of substrate, film forming or in substrate On the performances such as adhesive force.
According to an embodiment of the invention, first dispersing agent is selected from polyvinylpyrrolidone (PVP), cetyl three At least one of methyl bromide ammonium (CATB), neopelex (SDBS) and lauryl sodium sulfate (SDS);It is described Second dispersing agent is selected from sodium carboxymethylcellulose (CMC), ethyl cellulose (EC), polyacrylic acid (PAA) and polyethylene glycol (PEG) At least one of;.Each component dispersibility is preferable in electric heating ink as a result, and to three-dimensional grapheme, resin, conductive auxiliary agent Equal materials are free from side effects.
According to an embodiment of the invention, auxiliary agent is selected from wetting dispersing agent, defoaming agent, levelling agent, coalescing agent and adhesive force At least one of promotor and substrate wetting agents.Those skilled in the art flexible choice can fit according to actual needs as a result, When auxiliary agent, wetability of the Lai Gaishan electric heating ink to substrate, film forming.Or property such as adhesive force on base material after printing Energy.
According to an embodiment of the invention, 4500~64500cps of viscosity of electric heating ink, such as 4500cps, 5000cps, 6000cps、7000cps、7500cps、8500cps、9500cps、10500cps、11500cps、12500cps、15500cps、 18500cps、20500cps、25500cps、30500cps、35500cps、40500cps、45500cps、50500cps、 55500cps,60500cps,61500cps,62500cps,63500cps,64500cps.Those skilled in the art can be with as a result, The viscosity of electric heating ink is flexibly set according to actual conditions such as different printing technologies and print speed printing speed, for example can use silk screen Printing or coating process;In addition, can choose the relatively low electric heating ink of viscosity, if print speed printing speed if print speed printing speed is very fast It is relatively slow, then it can choose the relatively high electric heating ink of viscosity.
According to an embodiment of the invention, the solid content of electric heating ink be 7%~45%, such as 7%, 10%, 13%, 15%, 18%, 20%, 23%, 25%, 27%, 30%, 33%, 35%, 37%, 40%, 42%, 44% or 45%.As a result, Those skilled in the art can prepare the electric heating ink of suitable solid content, in other words, ability according to the viscosity of required electric heating ink Field technique personnel can adjust the viscosity of electric heating ink by the solid content of electric heating ink, wherein solid content is bigger, electric heating ink Viscosity it is bigger.
According to an embodiment of the invention, the fineness of electric heating ink is less than or equal in order to enable electric heating ink is convenient for printing 50 microns, for example be 50 microns, 45 microns, 40 microns, 35 microns, 30 microns, 25 microns or 20 microns.Electric heating ink as a result, Fineness it is good, particle is smaller, phenomena such as stifled version will not be caused in silk-screen printing, can cause to damage in offset lithography and gravure The phenomenon that printing plate and scraper, and also advantageously improve the intensity light for the ink film layer that preparation is obtained by the electric heating oil ink print Degree.
In the other side of this hair invention, the present invention provides a kind of methods for preparing electric heating ink noted earlier.Root According to the embodiment of the present invention, the method for preparing electric heating ink includes:
S100: resin is dissolved in a part of oiliness organic solvent, to obtain the first mixed liquor.
According to an embodiment of the invention, can assist to accelerate dissolution of the resin in oiliness organic solvent with machinery Stirring or magnetic agitation, in this way, process flow can be shortened.
S200: the first mixed liquor is uniformly mixed with three-dimensional grapheme, to obtain the second mixed liquor.
According to an embodiment of the invention, preparation the second mixed liquor the step of include: by the first mixed liquor, three-dimensional grapheme with At least one of first dispersing agent and the second dispersing agent are uniformly mixed, specifically, three-dimensional graphite is added into the first mixed liquor Alkene and at least one of the first dispersing agent and the second dispersing agent, and with high speed machine blender or high-shear emulsion machine into Row decentralized processing 0.5~1 hour.
S300: the second mixed liquor, conductive auxiliary agent and another part oiliness organic solvent are mixed, to obtain electric heating oil Ink.
According to an embodiment of the invention, the second mixed liquor and conductive auxiliary agent are mixed in order to promote the fineness of electric heating ink It is ground later, and another part oiliness organic solvent is added during milled processed, to obtain electric heating oil Ink.As a result, during the grinding process, further the materials such as three-dimensional grapheme, resin, conductive auxiliary agent can be ground, is obtained The smaller material of partial size, and then promote the fineness of electric heating ink.In some embodiments of the invention, above-mentioned steps specifically: Conductive auxiliary agent is added into the second mixed liquor, and continues to carry out decentralized processing with high speed machine blender or high-shear emulsion machine Mixed liquor is transferred in planetary ball mill or three-roll grinder or sand mill further milled processed 20 later by 0.5~1h ~45 minutes, and during milled processed be added another part oiliness organic solvent.
According to an embodiment of the invention, further including the steps that auxiliary agent is added after milled processed, stir evenly later, just Electric heating ink can be obtained.
According to an embodiment of the invention, above-mentioned preparation method simple operations, easy to industrialized production, preparation cost is low, and And in the above preparation method, three-dimensional grapheme can both form effective conductive network, three-dimensional grapheme in two-dimensional surface As conductive material, the contact dimension of conductive material can also be further increased in three-dimensional space, and then improves obtained electricity The electric conductivity of hot oil ink, the further dosage for reducing conductive auxiliary agent;And it can also be in electric heating ink and by the electric heating ink It prints in obtained ink film layer and plays the role of skeleton, help to improve stabilization of ink film layer during electrification heat-producing Property, and then extend the service life of ink film layer;In addition, as previously mentioned, three-dimensional grapheme can play bone in ink film layer The effect of frame in this way, the dosage of the resin of cementation can have been reduced, and then can reduce or avoid ink film layer repeatedly There is the risk that resin resets the decaying of bring power during heating, heating cooling.
According to an embodiment of the invention, the above-mentioned method for preparing electric heating ink can be used for preparing electric heating oil noted earlier Ink, wherein to the property of resin, three-dimensional grapheme, conductive auxiliary agent, the first dispersing agent, the second dispersing agent, auxiliary agent and electric heating ink Can the requirements such as parameter and front it is consistent, this is no longer going to repeat them.
Embodiment
Embodiment 1
2.5 weight of polyester resins are dissolved in 30 weight part of ethylacetate, use mechanical stirring;It is complete to resin After fully dissolved, 2 weight three-dimensional graphemes and 0.5 the first dispersing agent of parts by weight is added, and carried out at dispersion with high speed machine stirring After managing 0.5h, 2 parts by weight of carbon nanotubes are added, continue to carry out decentralized processing 0.5h with high-shear emulsion machine, it later will mixing Liquid is transferred in planetary ball mill further milled processed 20 minutes, and 62 parts by weight acetic acid second are added during milled processed Ester adjusts the viscosity of electric heating ink, and the defoaming agent of 0.5 parts by weight is finally added in obtained milled mixtures, and formation contains three Tie up the electric heating ink of graphene.Made electric heating ink solid content 8%, viscosity 4500cps, fineness are less than or equal to 50 microns;It adopts With silk-screen printing technique, printing obtains ink film layer in PET base material, and dries 30 minutes at 90 DEG C.Ink film layer is in base Adhesive force on material is 0 grade, and the hardness of ink film layer is 4H, and electric conductivity is 33 Ω/side, and electric radiation transformation efficiency is 70%.
Embodiment 2
6.5 parts by weight epoxy resin are dissolved in 30 parts by weight cyclohexanone, use magnetic agitation;It is complete to resin After dissolution, the first dispersing agent of 8 parts by weight three-dimensional graphemes and 0.5 parts by weight and the second dispersing agent of 1 parts by weight is added, is used in combination After high-shear emulsion machine carries out decentralized processing 0.5h, 2 parts by weight of carbon nanotubes are added, continue to be divided with high-shear emulsion machine Processing 1h is dissipated, mixed liquor is transferred in sand mill further milled processed 30 minutes later, is added during milled processed The cyclohexanone of 52 parts by weight adjusts the viscosity of electric heating ink, and the stream of 0.9 parts by weight is finally added in obtained milled mixtures The defoaming agent of flat agent and 0.1 parts by weight forms the most electric heating ink containing three-dimensional grapheme.Made electric heating ink solid content 18%, viscosity 15000cps, fineness are less than or equal to 50 microns;Using coating process, printing obtains ink film in PET base material Layer, and dried 30 minutes at 120 DEG C.Ink film layer adhesive force on base material is 0 grade, and the hardness of ink film layer is 3H, is led It is electrically 66 Ω/side, electric radiation transformation efficiency is 69%.
Embodiment 3
6 parts by weight of polyurethane are dissolved in 30 parts by weight dibasic acid ester mixtures, use magnetic agitation;To resin After being completely dissolved, 7 parts by weight three-dimensional graphemes are added, after carrying out decentralized processing 0.5h with high-shear emulsion machine, 8 parts by weight are added Carbon black, continue to carry out decentralized processing 1h with high-shear emulsion machine, mixed liquor be transferred in sand mill further grind later Processing 30 minutes, and the dibasic acid ester mixture that 49 parts by weight are added during milled processed adjusts the viscosity of ink, finally The levelling agent and 0.05 parts by weight defoaming agent of 0.95 parts by weight are added in obtained milled mixtures, formation contains three-dimensional graphite The electric heating ink of alkene.Made electric heating ink solid content 21%, viscosity 24500cps, fineness are less than or equal to 50 microns;Using silk Wire mark brush, printing obtains ink film layer in PET base material, and dries 30 minutes at 120 DEG C.Ink film layer is on base material attached Put forth effort to be 0 grade, the hardness of ink film layer is 6H, and electric conductivity is 47 Ω/side, and electric radiation transformation efficiency is 67%.
Embodiment 4
The acrylic resin of 9 parts by weight is dissolved in 30 parts by weight of propylene glycol methyl ether acetates, is stirred using magnetic force It mixes;After resin is completely dissolved, the second of 10 parts by weight three-dimensional graphemes, the first dispersing agent of 1 parts by weight and 2 parts by weight is added Dispersing agent after carrying out decentralized processing 0.5h with high-shear emulsion machine, adds the carbon black of 5 parts by weight, continues to use high-shear emulsifying Machine carries out decentralized processing 1h, is later transferred to mixed liquor in sand mill further milled processed 30 minutes, and in milled processed During be added 43 parts by weight propylene glycol methyl ether acetate adjust ink viscosity, finally in obtained milled mixtures The levelling agent of 0.8 parts by weight and the defoaming agent of 0.1 parts by weight is added, forms the electric heating ink containing three-dimensional grapheme.Made Electric heating ink solid content 27%, viscosity 34500cps, fineness are less than or equal to 50 microns;Using coating process, printed in PET base material Brush obtains ink film layer, and dries 30 minutes at 120 DEG C.Ink film layer adhesive force on base material is 0 grade, ink film layer Hardness is 5H, and electric conductivity is 56 Ω/side, and electric radiation transformation efficiency is 71%.
Embodiment 5
By 12 parts by weight of polyurethane and polyester (mass ratio of polyurethane and polyester is 3:2) resin in 30 parts by weight ethyl cards It must be dissolved in alcohol, use magnetic agitation;After resin is completely dissolved, three-dimensional grapheme, 1 parts by weight of 5 parts by weight are added The first dispersing agent and the second dispersing agent of 10 parts by weight add 10 after carrying out decentralized processing 0.5h with high-shear emulsion machine The carbon black of parts by weight continues to carry out decentralized processing 1h with high-shear emulsion machine, mixed liquor is transferred in sand mill into one later Step milled processed 30 minutes, and the ethyl carbitol that 37 parts by weight are added during milled processed adjusts the viscosity of ink; The levelling agent of 0.8 weight powder and the defoaming agent of 0.2 parts by weight are finally added in obtained milled mixtures, is formed containing three-dimensional The electric heating ink of graphene.Made electric heating ink solid content 33%, viscosity 44500cps, fineness are less than or equal to 50 microns;It adopts With silk-screen printing, printing obtains ink film layer in PET base material, and dries 30 minutes at 90 DEG C.Ink film layer is on substrate Adhesive force be 0 grade, the hardness of ink film layer is 5H, and electric conductivity is 86 Ω/side, and electric radiation transformation efficiency is 66%.
Embodiment 6
By the epoxy resin of 20 parts by weight and acrylic resin (the mass ratio 1:1 of epoxy resin and acrylic resin) 30 It is dissolved in the cyclohexanone and ethyl carbitol (volume ratio of cyclohexanone and ethyl carbitol is 1:1) of parts by weight, uses magnetic Power stirring;After resin is completely dissolved, the three-dimensional grapheme of 8 parts by weight and the first dispersing agent and 6 parts by weight of 1 parts by weight is added The second dispersing agent, after carrying out decentralized processing 0.5h with high-shear emulsion machine, add the carbon black of 10 parts by weight, continue to be cut with height It cuts mulser and carries out decentralized processing 1h, be later transferred to mixed liquor in sand mill further milled processed 30 minutes, and grinding Cyclohexanone and ethyl carbitol (volume ratio 1:1) that 25 parts by weight are added during mill processing adjust the viscosity of ink;Most The defoaming agent of 0.3 parts by weight is added in obtained milled mixtures afterwards, forms the electric heating ink containing three-dimensional grapheme.It is made Electric heating ink solid content 45%, viscosity 64500cps, fineness be less than or equal to 50 microns;Using coating process, in PET base material Printing obtains ink film layer, and dries 30 minutes at 90 DEG C.Ink film layer adhesive force on base material is 0 grade, ink film layer Hardness be 5H, electric conductivity be 114 Ω/side, electric radiation transformation efficiency be 67%.
Comparative example 1
Using formula and preparation step same as Example 2, difference is: three-dimensional grapheme is replaced with two-dimentional graphite Alkene.It is formed by the viscosity 10500cps of electric heating ink, can only be formed a film using coating process in PET, and dry 30 at 90 DEG C Minute.Ink adhesive force on substrate is 2 grades, and the hardness of ink film layer is 2H, and electric conductivity is 180 Ω/side, electric radiation conversion Efficiency is 61%.
Comparative example 2
Using formula and preparation step same as Example 3, difference is: three-dimensional grapheme is replaced with two-dimentional graphite Alkene.It is formed by the viscosity 90000cps of electric heating ink, can only be formed a film with coating process in PET, and dry 30 points at 90 DEG C Clock.Ink adhesive force on substrate is 3 grades, and the hardness of ink film layer is 3H, and electric conductivity is 210 Ω/side, electric radiation conversion effect Rate is 63%.
The test result of the electric heating ink and ink film layer that prepare in each embodiment and comparative example is referring to following table table 1.
Table 1
Wherein, the testing standard of adhesive force are as follows: ASTMD3359-2009;The testing standard of electric radiation transformation efficiency are as follows: GB/T 7287-2008。
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned Embodiment is changed, modifies, replacement and variant.

Claims (10)

1. a kind of electric heating ink characterized by comprising
The three-dimensional grapheme of 2~25 parts by weight;
The resin of 3~25 parts by weight;
The conductive auxiliary agent of 2~25 parts by weight;
The oiliness organic solvent of 30~93 parts by weight.
2. electric heating ink according to claim 1, which is characterized in that further include at least one of:
First dispersing agent of 0~1 parts by weight;
Second dispersing agent of 0~10 parts by weight;
The auxiliary agent of 0~1 parts by weight.
3. electric heating ink according to claim 1, which is characterized in that the resin is selected from polyester resin, epoxy resin, gathers At least one of urethane resin and acrylic resin;
The conductive auxiliary agent is selected from least one of carbon nanotube, carbon black, acetylene black and graphite;
The oiliness organic solvent is selected from cyclohexanone, ethyl acetate, dibasic acid ester mixed liquor, propylene glycol methyl ether acetate and ethyl At least one of carbitol.
4. electric heating ink according to claim 2, which is characterized in that first dispersing agent is selected from polyvinylpyrrolidone At least one of ketone, cetyl trimethylammonium bromide, neopelex and lauryl sodium sulfate;
Second dispersing agent in sodium carboxymethylcellulose, ethyl cellulose, polyacrylic acid and polyethylene glycol at least one Kind;
The auxiliary agent is in wetting dispersing agent, defoaming agent, levelling agent, coalescing agent and adhesion promoter and substrate wetting agents At least one.
5. electric heating ink according to any one of claims 1 to 4, which is characterized in that the solid content of the electric heating ink It is 7%~45%.
6. electric heating ink according to any one of claims 1 to 4, which is characterized in that the viscosity of the electric heating ink 4500~64500cps.
7. electric heating ink according to any one of claims 1 to 4, which is characterized in that the fineness of the electric heating ink is small In or equal to 50 microns.
8. a kind of method for preparing electric heating ink described in any one of claim 1~7 characterized by comprising
Resin is dissolved in a part of oiliness organic solvent, to obtain the first mixed liquor;
First mixed liquor is uniformly mixed with three-dimensional grapheme, to obtain the second mixed liquor;
Oiliness organic solvent described in second mixed liquor, conductive auxiliary agent and another part is mixed, to obtain the electric heating Ink.
9. according to the method described in claim 8, it is characterized in that, second mixed liquor and the conductive auxiliary agent are mixed it After be ground, and during the milled processed be added another part described in oiliness organic solvent, to obtain The electric heating ink.
10. according to the method described in claim 9, it is characterized in that, the step of preparing second mixed liquor includes: will be described First mixed liquor, the three-dimensional grapheme are uniformly mixed at least one of the first dispersing agent and the second dispersing agent;
Optional, further include the steps that auxiliary agent is added after the milled processed.
CN201910141372.9A 2019-02-26 2019-02-26 Electric heating ink and preparation method thereof Pending CN109666339A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110194910A (en) * 2019-06-17 2019-09-03 新奥石墨烯技术有限公司 Electric heating ink and preparation method thereof with low-work voltage and farsighted infrared emittance
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
CN113122072A (en) * 2019-12-30 2021-07-16 山东欧铂新材料有限公司 Graphene conductive ink for heating film and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103113786A (en) * 2013-03-07 2013-05-22 苏州牛剑新材料有限公司 Graphene conductive ink and preparation method thereof
WO2016085584A2 (en) * 2014-10-15 2016-06-02 Northwestern University Graphene-based ink compositions for three-dimensional printing applications
CN106883684A (en) * 2017-04-01 2017-06-23 北京创新爱尚家科技股份有限公司 Graphene three-dimensional composite water soluble electric heating ink and preparation method thereof
CN106882796A (en) * 2017-03-23 2017-06-23 复旦大学 A kind of preparation method of three-dimensional grapheme structure/high-quality graphene
CN107384026A (en) * 2017-08-22 2017-11-24 华惠福科技股份有限公司 A kind of watersoluble plumbago alkene/CNT compound electro-thermal conversion ink and preparation method
WO2018136810A1 (en) * 2017-01-19 2018-07-26 Graphene Technologies, Inc. Multifunctional nanocomposites reinforced with impregnated cellular carbon nanostructures
CN108753043A (en) * 2018-04-12 2018-11-06 重庆市中光电显示技术有限公司 Electrically conductive ink and its preparation method and application for flexible touch screen conducting wire

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103113786A (en) * 2013-03-07 2013-05-22 苏州牛剑新材料有限公司 Graphene conductive ink and preparation method thereof
WO2016085584A2 (en) * 2014-10-15 2016-06-02 Northwestern University Graphene-based ink compositions for three-dimensional printing applications
WO2018136810A1 (en) * 2017-01-19 2018-07-26 Graphene Technologies, Inc. Multifunctional nanocomposites reinforced with impregnated cellular carbon nanostructures
CN106882796A (en) * 2017-03-23 2017-06-23 复旦大学 A kind of preparation method of three-dimensional grapheme structure/high-quality graphene
CN106883684A (en) * 2017-04-01 2017-06-23 北京创新爱尚家科技股份有限公司 Graphene three-dimensional composite water soluble electric heating ink and preparation method thereof
CN107384026A (en) * 2017-08-22 2017-11-24 华惠福科技股份有限公司 A kind of watersoluble plumbago alkene/CNT compound electro-thermal conversion ink and preparation method
CN108753043A (en) * 2018-04-12 2018-11-06 重庆市中光电显示技术有限公司 Electrically conductive ink and its preparation method and application for flexible touch screen conducting wire

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110194910A (en) * 2019-06-17 2019-09-03 新奥石墨烯技术有限公司 Electric heating ink and preparation method thereof with low-work voltage and farsighted infrared emittance
CN113122072A (en) * 2019-12-30 2021-07-16 山东欧铂新材料有限公司 Graphene conductive ink for heating film and preparation method thereof
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

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