CN109666339A - Electric heating ink and preparation method thereof - Google Patents
Electric heating ink and preparation method thereof Download PDFInfo
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- 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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- 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
- C09D11/52—Electrically conductive inks
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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
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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
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
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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
- C09D11/10—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
- C09D11/104—Polyesters
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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
- C09D11/106—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
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
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
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.
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