CN109679260A - A kind of composite water soluble conductive emulsion, preparation method and water-soluble conducting ink - Google Patents
A kind of composite water soluble conductive emulsion, preparation method and water-soluble conducting ink Download PDFInfo
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
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- 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
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- 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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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
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- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
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- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The present invention provides a kind of composite water soluble conductive emulsion, preparation method and water-soluble conducting ink, belongs to carbon-based material technical field.Composite water soluble conductive emulsion includes water, carbon materials A and resin aqueous emulsion, wherein, the mass percent that carbon materials A accounts for composite water soluble conductive emulsion is 0.1%-40%, the mass percent that resin aqueous emulsion accounts for composite water soluble conductive emulsion is 5%-60%, is 100-4000cp in the viscosity of (25 ± 1) DEG C composite water soluble conductive emulsion.Water-soluble conducting ink includes the one or more of composite water soluble conductive emulsion and carbon materials B, water-based ink auxiliary agent and cosolvent.This water-soluble conducting ink uses above-mentioned composite water soluble conductive emulsion, and dispersion effect is more preferable, and the electric conductivity for the conductive coating that mobility more preferably, by water-soluble conducting ink is prepared is more preferable.
Description
Technical field
The present invention relates to conductive emulsion technical fields, in particular to a kind of composite water soluble conductive emulsion, its preparation side
Method and water-soluble conducting ink.
Background technique
Since carbon nanomaterial has a very high specific surface area, it is evenly dispersed in the solution after meeting so that solution viscosity
It sharply increases, will generally lose flowability at 5% or so.So it is usually that carbon nanomaterial progress surface is modified, with
The raw material of lotion carries out home position polymerization reaction to obtain multiple emulsion.
In the prior art, the modification of carbon nanomaterial surface can hinder phase interconnection of the carbon nanomaterial after forming conductive coating
It connects, so that conductivity increases.
Summary of the invention
The purpose of the present invention is to provide a kind of composite water soluble conductive emulsion, preparation method and water-soluble conducting inks, make
For the viscosity of composite water soluble conductive emulsion within the scope of 100-4000cp, the resistivity of coating obtained is lower.
In a first aspect, the embodiment of the present invention provides a kind of composite water soluble conductive emulsion, including water, carbon materials A and aqueous
Resin emulsion, wherein the mass percent that carbon materials A accounts for composite water soluble conductive emulsion is 0.1%-40%, water-base resin cream
The mass percent that liquid accounts for composite water soluble conductive emulsion is 5%-60%, in the viscosity of (25 ± 1) DEG C composite water soluble conductive emulsion
For 100-4000cp.
The viscosity of content and composite water soluble conductive emulsion to carbon materials A and resin aqueous emulsion limits,
During carbon materials A is spread in aqueous systems, the lipophilicity of carbon materials A is gradually manifested, so that carbon materials A can be with
It is dissolved into the inside of resin aqueous emulsion, carbon materials A is wrapped in resin aqueous emulsion, due to point of resin aqueous emulsion
Property and good fluidity are dissipated, carbon materials A is wrapped in resin aqueous emulsion, obtained composite water soluble conductive emulsion can have
The carbon materials A of high-content, and its viscosity is low and dispersion effect is good, avoids generating reunion.
With reference to first aspect, in another embodiment, carbon materials A accounts for the mass percent of composite water soluble conductive emulsion and is
1%-30%, the mass percent that resin aqueous emulsion accounts for composite water soluble conductive emulsion is 30%-60%；Optionally, carbon
The mass percent that materials A accounts for composite water soluble conductive emulsion is 5%-20%, and resin aqueous emulsion accounts for composite water soluble conductive emulsion
Mass percent be 40%-60%；Optionally, resin aqueous emulsion include acrylic emulsion, styrene-acrylic emulsion, epoxy emulsion,
The lotion of polyaminoester emulsion, polythene wax emulsion and ptfe emulsion and its derivative it is one or more；Optionally,
The viscosity of composite water soluble conductive emulsion is 1000-2000cp at (25 ± 1) DEG C.
With reference to first aspect, in another embodiment, carbon materials A includes in carbon nanotube, graphene and fullerene
It is one or more；Optionally, the caliber of carbon nanotube is 0.01-20 μm, and optionally, the caliber of carbon nanotube is 0.1-10 μ
M, optionally, the caliber of carbon nanotube are 0.1-1 μm；Optionally, the length of carbon nanotube is 0.1-50 μm, optionally, carbon
The length of nanotube is 0.1-20 μm, and optionally, the length of carbon nanotube is 1-10 μm；Optionally, the piece of graphene is layer by layer
Number is 1-10 layers, and optionally, the lamella number of plies of graphene is 1-5 layers, and optionally, the lamella number of plies of graphene is 1-2 layers；
Optionally, the piece diameter of graphene is having a size of 0.01 μm -20 μm, and optionally, the piece diameter of graphene is optional having a size of 0.1-10 μm
, the piece diameter of graphene is having a size of 0.1-1 μm.
The specific surface area of carbon materials A is larger, and can mutually merge with resin aqueous emulsion, and obtained composite water soluble is led
The content of the carbon materials A of electric lotion can further increase, and the viscosity of composite water soluble conductive emulsion is low and dispersion effect is good,
It avoids generating reunion.
With reference to first aspect, in another embodiment, composite water soluble conductive emulsion further includes dispersing agent, and dispersing agent accounts for compound
The mass percent of waterborne conductive lotion is not higher than 0.1%, and optionally, dispersing agent accounts for the quality hundred of composite water soluble conductive emulsion
Score be not higher than 0.01%, optionally, dispersing agent account for composite water soluble conductive emulsion mass percent be not higher than
0.0001%；Optionally, dispersing agent is water-soluble polymer；Optionally, the molecular weight of water-soluble polymer is 10,000-100 hundred million,
Optionally, the molecular weight of water-soluble polymer is 1,000,000-10 hundred million, and optionally, the molecular weight of water-soluble polymer is 1000
Ten thousand -1 hundred million；Optionally, water-soluble polymer includes polyvinyl alcohol, polyvinylamine, polyvinylpyrrolidone, polyethylene glycol, poly- third
One of olefin(e) acid, polyacrylamide, polyurethane, water-base epoxy polymer and water-soluble cellulose are a variety of.
The addition of dispersing agent can make the dispersion effect of composite water soluble conductive emulsion more preferable, and the dispersing agent of high molecular weight exists
The speed spread into aqueous systems is slower, can make evenly dispersed state of the carbon-based material A in aqueous systems and with aqueous tree
Smooth transition between the state of fat liquor droplet coalescence avoids generating reunion.
Second aspect, the embodiment of the present invention provide a kind of composite water soluble conductive emulsion, including water, carbon materials A and aqueous
Resin emulsion, wherein the mass percent that carbon materials A accounts for composite water soluble conductive emulsion is 0.1%-40%, water-base resin cream
The mass percent that liquid accounts for composite water soluble conductive emulsion is 5%-60%；Wherein, at least part of carbon materials A is wrapped up
In resin aqueous emulsion.
The content of carbon materials A and resin aqueous emulsion are limited, and at least part of carbon materials A is wrapped up
In resin aqueous emulsion, enable composite water soluble conductive emulsion that there is the original good dispersion of lotion and mobility, and energy
Enough with the carbon materials of high-content.
The third aspect, the present invention provide a kind of preparation method of composite water soluble conductive emulsion, include the following steps: carbon
Materials A and dispersing agent disperse to obtain aqueous liquid dispersion in water.Seed emulsion is prepared, pre-emulsion is prepared.First by pre-emulsion
It is added in seed emulsion, adds aqueous liquid dispersion.
Due to the effect of dispersing agent, carbon materials A can be made slowly uniformly to diffuse in aqueous systems, that is to say, that carbon
Materials A diffuses in aqueous systems together with dispersing agent, forms uniform aqueous liquid dispersion, and due to being initially formed seed emulsion,
The emulsion droplet of resin aqueous emulsion is formed, pre-emulsion is added, seed emulsion gradually polymerize with pre-emulsion, lotion liquid
Drop is gradually increased, and is added after carbon materials A aqueous liquid dispersion, and the concentration of dispersing agent reduces, and carbon materials A gradually manifests parent
Oiliness, since emulsion droplet is gradually increased, the surface area of emulsion droplet is larger, and carbon materials A is gradually merged with emulsion droplet, makes
Carbon materials A fusion is wrapped in emulsion droplet in droplet surface or at least part, so that the composite water soluble made is conductive
The good dispersion of lotion, mobility is good, and viscosity is low.
In conjunction with the third aspect, in another embodiment, pre-emulsion is divided into the first pre-emulsion and the second pre-emulsion,
First the first pre-emulsion is added in seed emulsion, adds aqueous liquid dispersion, is eventually adding the second pre-emulsion.First make to plant
Sub- lotion gradually polymerize with the first pre-emulsion, and emulsion droplet is gradually increased, and aqueous liquid dispersion is added afterwards, and the concentration of dispersing agent subtracts
Small, carbon materials A gradually manifests lipophilicity, so that carbon materials A is mutually merged with emulsion droplet, adds the second pre-emulsification
Liquid, the second pre-emulsion continue to polymerize with emulsion droplet, are wrapped in carbon materials A gradually in emulsion droplet or at least one
It point is wrapped in emulsion droplet, thus further such that the good dispersion of the composite water soluble conductive emulsion arrived, mobility is good, and
Viscosity is low.
In conjunction with the third aspect, in another embodiment, the preparation method of seed emulsion, comprising: by emulsifier and initiator
Mixing adds resin monomer and forms seed emulsion.Optionally, the preparation method of pre-emulsion, comprising: by emulsifier and resin
Monomer is mixed to form pre-emulsion.Optionally, emulsifier includes fatty acid salt, RA rosin acid, sulfate, sulfonate, alkylammonium
With one of quaternary ammonium salt or a variety of.Optionally, resin monomer includes acrylate monomer, phenprobamate monomer, epoxy resin
Monomer and phenolic resin monomer it is one or more.Optionally, initiator include azodiisobutyronitrile, dibenzoyl peroxide,
One of cumyl peroxide, dialkyl and diacyl peroxides are a variety of.
Fourth aspect, the embodiment of the present invention provide a kind of water-soluble conducting ink, including composite water soluble conductive emulsion and carbon
Cellulosic material B, water-based ink auxiliary agent and cosolvent it is one or more.Water-soluble conducting ink is used to prepare conductive coating, conductive
Property is good.
In conjunction with fourth aspect, in another embodiment, water-based ink auxiliary agent includes levelling agent, thickener, defoaming agent, pH tune
Save one of agent, mould inhibitor, drying retardant, quick dry agent or a variety of；Cosolvent includes optionally having including water and organic solvent
Solvent include ethyl alcohol, ethylene glycol, propyl alcohol, propylene glycol, isopropanol, acetone, butanol, butanediol, isobutanol, butanone, isobutyl ketone,
N-Methyl pyrrolidone, n,N-Dimethylformamide, n,N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, dioxy
One of six rings are a variety of；Carbon materials B includes carbon black, carbon nanotube, graphite, graphene, carbon fiber, one in fullerene
Kind is a variety of.
In conjunction with fourth aspect, in another embodiment, carbon materials A and carbon materials B account for consolidating for water-soluble conducting ink
The mass percent of content is 20%-60%, and optionally, carbon materials A and carbon materials B account for consolidating for water-soluble conducting ink
The mass percent of content is 30%-50%.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The composite water soluble conductive emulsion of the embodiment of the present invention, preparation method and water-soluble conducting ink are carried out below specific
Explanation.
Composite water soluble conductive emulsion includes water, carbon materials A and resin aqueous emulsion, wherein carbon materials A accounts for Compound Water
Property conductive emulsion mass percent be 0.1%-40%, resin aqueous emulsion accounts for the quality percentage of composite water soluble conductive emulsion
Number is 5%-60%, is 100-4000cp in the viscosity of (25 ± 1) DEG C composite water soluble conductive emulsion.
Wherein, viscosity determining procedure are as follows: tested using NDJ-5 rotational viscometer, control fluid to be measured temperature 25
It ± 1 DEG C, is tested under the conditions of 30rpm using No. 3 rotors.If it may be selected when other than its range ability in institute's viscosimetric
His model rotor and other speed conditions.
Optionally, it is 1%-30%, water-base resin cream that carbon materials A, which accounts for the mass percent of composite water soluble conductive emulsion,
The mass percent that liquid accounts for composite water soluble conductive emulsion is 30%-60%；Optionally, carbon materials A accounts for the conductive cream of composite water soluble
The mass percent of liquid is 5%-20%, and the mass percent that resin aqueous emulsion accounts for composite water soluble conductive emulsion is 40%-
60%；The viscosity of composite water soluble conductive emulsion is 1000-2000cp at (25 ± 1) DEG C.
In the composite water soluble conductive emulsion obtained within the scope of this, preferably, mobility is more for the dispersibility of carbon materials A in water
It is good, and a part of carbon materials A or carbon materials A are wrapped in resin aqueous emulsion, it can be to avoid between carbon materials A
Strong attraction, avoid generate reunion, make the good dispersion of entire composite water soluble conductive emulsion, mobility is good.
Composite water soluble conductive emulsion includes water, carbon materials A and resin aqueous emulsion, wherein carbon materials A accounts for Compound Water
Property conductive emulsion mass percent be 0.1%-40%, resin aqueous emulsion accounts for the quality percentage of composite water soluble conductive emulsion
Number is 5%-60%；Wherein, at least part of carbon materials A is wrapped in resin aqueous emulsion.
Since at least part of carbon materials A or carbon materials A are wrapped in resin aqueous emulsion, that is to say, that cream
Carbon materials A is enclosed in liquid drop, emulsion droplet separates carbon materials A, avoids the attraction between carbon materials A, avoids
Reunite, and since lotion itself has good dispersion stabilization and mobility, so, carbon materials are wrapped up in emulsion droplet
After A, dispersibility and mobility are still preferable, and the viscosity of the composite water soluble conductive emulsion made is low.
Optionally, resin aqueous emulsion includes acrylic emulsion, styrene-acrylic emulsion, epoxy emulsion, polyaminoester emulsion, polyethylene
Wax emulsion and the lotion of ptfe emulsion and its derivative it is one or more.Carbon materials A includes carbon nanotube, stone
One of black alkene and fullerene are a variety of.
Carbon materials A has very high specific surface area, evenly dispersed in the solution the viscosity of solution to be made sharply to increase later
Add, so, carbon materials A is mixed with above-mentioned resin aqueous emulsion, since resin aqueous emulsion can wrap up carbon materials A,
Carry out the two compound, to obtain high carbon materials additive amount, and the composite water soluble conductive emulsion of low viscosity.
In the present embodiment, the caliber of carbon nanotube is 0.01-20 μm, and optionally, the caliber of carbon nanotube is 0.1-10 μ
M, optionally, the caliber of carbon nanotube are 0.1-1 μm.The length of carbon nanotube is 0.1-50 μm, optionally, carbon nanotube
Length is 0.1-20 μm, and optionally, the length of carbon nanotube is 1-10 μm.The lamella number of plies of graphene is 1-10 layers, optional
, the lamella number of plies of graphene is 1-5 layers, and optionally, the lamella number of plies of graphene is 1-2 layers.The piece diameter size of graphene
Be 0.01 μm -20 μm, optionally, the piece diameter of graphene is having a size of 0.1-10 μm, optionally, the piece diameter of graphene having a size of
0.1-1 μm.
In the present embodiment, composite water soluble conductive emulsion further includes dispersing agent, make carbon materials A in resin aqueous emulsion and
Disperse in water it is more uniform, dispersing agent account for composite water soluble conductive emulsion mass percent be not higher than 0.1%, optionally, point
The mass percent that powder accounts for composite water soluble conductive emulsion is not higher than 0.01%, and optionally, dispersing agent accounts for composite water soluble conduction
The mass percent of lotion is not higher than 0.0001%, and the content of dispersing agent is lower, it is avoided more to be adsorbed on carbon materials A
Surface, so that carbon materials A is preferably wrapped in resin aqueous emulsion.
Further, dispersing agent is water-soluble polymer；Optionally, the molecular weight of water-soluble polymer is 10,000-100
Hundred million, optionally, the molecular weight of water-soluble polymer is 1,000,000-10 hundred million, and optionally, the molecular weight of water-soluble polymer is 1000
Ten thousand -1 hundred million.Optionally, water-soluble polymer includes polyvinyl alcohol, polyvinylamine, polyvinylpyrrolidone, polyethylene glycol, poly- third
One of olefin(e) acid, polyacrylamide, polyurethane, water-base epoxy polymer and water-soluble cellulose are a variety of.
Using the dispersing agent of high molecular weight, dispersing agent is added dropwise in water, dispersing agent is not quickly all to spread in water,
But be gradually diffused to aqueous systems with a slowly process, when dispersing agent and carbon materials A are newborn in water-base resin
In liquid when diffusion, since dispersing agent is diluted, concentration is reduced, and carbon materials A gradually manifests lipophilicity, so that carbon materials A
It can be dissolved into the inside of resin aqueous emulsion, so, state carbon materials A evenly dispersed in aqueous systems being capable of steady mistake
The state for crossing the droplet coalescence to carbon materials A and resin aqueous emulsion, merges emulsion droplet mutually with carbon materials A, keeps away
Exempt from the strong attraction between carbon materials A, avoids generating reunion.
The preparation method of above-mentioned composite water soluble conductive emulsion, includes the following steps:
(1), carbon materials A and dispersing agent are dispersed in water to obtain aqueous liquid dispersion.Wherein, dispersing agent is above-mentioned high score
The dispersing agent of son amount, aqueous liquid dispersion disperse to obtain by high speed shear, come into full contact with carbon materials A with dispersing agent, in water
In it is fully dispersed, high speed shear be carried out in high speed shear dispersal device, such as: dispersion impeller, airslide disintegrating mill, at ultrasonic wave
Manage one of device, ball mill, sand mill or a variety of combinations.Its shear velocity can be between 5000rpm-24000rpm.
Wherein, after aqueous liquid dispersion is formed, deionized water can be used and clean, remove dispersing agent.
(2), seed emulsion is prepared.The preparation method of seed emulsion, comprising: emulsifier and initiator are mixed, added
Resin monomer forms seed emulsion.Prepare pre-emulsion.The preparation method of pre-emulsion, comprising: by emulsifier and resin monomer
It is mixed to form pre-emulsion.
Wherein, emulsifier includes one of fatty acid salt, RA rosin acid, sulfate, sulfonate, alkylammonium and quaternary ammonium salt
Or it is a variety of.Resin monomer include acrylate monomer, phenprobamate monomer, epoxy monomer and phenolic resin monomer one kind
Or it is a variety of.Initiator includes azodiisobutyronitrile, dibenzoyl peroxide, cumyl peroxide, dialkyl and mistake
Aoxidize one of diacyl or a variety of.
It should be noted that the content of resin monomer is lower in seed emulsion, and in pre-emulsion, the content of resin monomer
It is higher.That is, the emulsifier of 40-60 parts by weight and the initiator of 10-20 parts by weight are stirred in water, heat up
To 75-85 DEG C, it is slowly added to the resin monomer of 1-5 parts by weight, heat preservation 20-40min carries out emulsion polymerization and forms seed cream
Liquid.The emulsifier of 40-60 parts by weight and the resin monomer of 80-100 parts by weight are mixed and carry out emulsion polymerization formation pre-emulsification
Liquid.
(3), first pre-emulsion is added in seed emulsion, adds aqueous liquid dispersion.Pre-emulsion and seed emulsion
Emulsion polymerization is carried out, is added after the aqueous liquid dispersion containing carbon materials A, carbon materials A is merged with emulsion droplet, makes carbon
Materials A fusion is wrapped in emulsion droplet on emulsion droplet surface or at least part, so that the composite water soluble made is led
The good dispersion of electric lotion, mobility is good, and viscosity is low.
It is wrapped in emulsion droplet to merge more carbon materials A with emulsion droplet, pre-emulsion is divided into
One pre-emulsion and the second pre-emulsion；First the first pre-emulsion is added in seed emulsion, adds aqueous liquid dispersion, finally
The second pre-emulsion is added.Second pre-emulsion continues to polymerize with emulsion droplet, and more carbon materials A is made to be wrapped in lotion liquid
In drop, the structure of emulsion droplet package carbon materials A is obtained.
In detail, first the initiator of the first pre-emulsion and 5-10 parts by weight is slowly added into seed emulsion, then plus
Enter the aqueous liquid dispersion of carbon materials A, and the initiator of the second pre-emulsion and 5-10 parts by weight is slowly added into, after
Continue and keep 20-40min in the case where 75-85 DEG C, be cooled to 45-55 DEG C, after being neutralized using ammonium hydroxide, is collected by filtration compound
Waterborne conductive lotion.
It should be understood that be gradually added into pre-emulsion to be added in seed emulsion, it can be gradually by pre- cream
Change drop to enter in seed emulsion, after pre-emulsion instills a period of time, will be added containing the aqueous liquid dispersion of carbon materials A
Into emulsion droplet, and continue to instill pre-emulsion, in this way, the pre-emulsion instilled before adding aqueous liquid dispersion is defined as
First pre-emulsion, the pre-emulsion instilled after aqueous liquid dispersion is added are defined as the second pre-emulsion.
Wherein, the resin monomer of seed emulsion and the first pre-emulsion accounts for the resin list of seed emulsion and pre-emulsion
The mass percent of the weight of body is charging progress.Such as: the resin monomer that seed emulsion and the first pre-emulsion use is
The amount for the resin monomer that 80kg, seed emulsion and total pre-emulsion use is 100kg, then the progress that feeds is 80%.Namely
It says, charging progress is smaller, and the amount of the second pre-emulsion is bigger, and carbon materials A's is wrapped in the more internal of emulsion droplet, charging
Progress is bigger, and the amount of the second pre-emulsion is less, and carbon materials A is wrapped in the more external of emulsion droplet.
The preparation for first passing through seed emulsion, forms emulsion droplet, and the first pre-emulsion is added, and the first pre-emulsion is being planted
Emulsion polymerization is carried out around sub- lotion, is gradually increased emulsion droplet, during emulsion polymerization, by carbon materials A's
When aqueous liquid dispersion joins, dispersing agent is diluted by whole system, and the concentration of dispersing agent reduces, and carbon materials A gradually appears
Lipophilic out, emulsion droplet is attractive to carbon materials A, and carbon materials A is merged with emulsion droplet.Add the second pre- cream
Change liquid, the second pre-emulsion continues to polymerize with emulsion droplet, and emulsion droplet is gradually increased, to form emulsion droplet package carbon
The structure of materials A.Wherein, the high molecular weight of dispersing agent hinders it quickly to spread, and leads to the concentration of dispersing agent around carbon materials A
Slowly reduce so that homogeneously dispersed state of the carbon materials A in aqueous systems be able to smooth transition to emulsion droplet plocoid
State avoids the strong attraction between carbon materials A, will not generate reunion.
A kind of water-soluble conducting ink, including composite water soluble conductive emulsion and carbon materials B, water-based ink auxiliary agent and help
Solvent it is one or more.
Carbon materials B can be further added in composite water soluble conductive emulsion, can increase the amount of conductive filler, thus
Further increase the electric conductivity of conductive coating, and carbon materials A content it is higher when, carbon materials B can not be added.
In order to improve filming performance, water-based ink auxiliary agent, example can be added according to the demand of graphene water-soluble conducting ink
Such as: water-based ink auxiliary agent includes one of levelling agent, thickener, defoaming agent, pH adjusting agent, mould inhibitor, drying retardant, quick dry agent
Or it is a variety of.
Cosolvent is to aid in water-based ink auxiliary agent resin aqueous emulsion dispersion in ink or only dilution ink is solid
The solvent of content.Wherein, solvent can be inorganic solvent or/and organic solvent.Wherein, inorganic solvent is water；Organic solvent packet
Include ethyl alcohol, ethylene glycol, propyl alcohol, propylene glycol, isopropanol, acetone, butanol, butanediol, isobutanol, butanone, isobutyl ketone, N- methyl
In pyrrolidones, n,N-Dimethylformamide, n,N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran and dioxane
It is one or more.
Carbon materials B includes one of carbon black, carbon nanotube, graphite, graphene, carbon fiber, fullerene or a variety of.Its
In, the material in carbon materials B can be by the modified material in surface.
The mass percent that carbon materials A and carbon materials B accounts for the solid content of water-soluble conducting ink is 20%-60%,
Optionally, it is 30%-50% that carbon materials A and carbon materials B, which accounts for the mass percent of the solid content of water-soluble conducting ink,.
Wherein, solid content refers to be prepared into conductive coating using water-soluble conducting ink after, the quality of conductive coating.It is conductive
The mass percent that filler (gross mass of carbon materials A and carbon materials B) accounts for solid content (conductive coating) is 20%-60%,
The mass percent that conductive filler accounts for solid content is 30%-50%, and the mass percent that conductive filler accounts for solid content is 40%-
60%.Wherein, solid content refers to that water-soluble conducting ink has been made after conductive coating, the quality of conductive coating, waterborne conductive oil
Ink is made after conductive coating, consisting of the gross mass of conductive filler, resin and auxiliary agent.
It is using the method that water-soluble conducting ink prepares conductive coating: water-soluble conducting ink is passed through into coating or printing
Mode is formed in PET film, pulls out a wet film by bar, 100 DEG C of drying and shapings, obtain conductive coating in an oven.
Embodiment one
Here is the parameter such as table 1 of each component for the composite water soluble conductive emulsion that embodiment provides,
The parameter of each component of 1 composite water soluble conductive emulsion of table
In the case where other conditions are constant, composite water soluble conductive emulsion is prepared using the parameter in above-mentioned table 1, and
(25 ± 1) DEG C carry out viscosity test using NDJ-5 rotational viscometer, obtain table 2,
The viscosity of 2 composite water soluble conductive emulsion of table
From table 2 it can be seen that the too high levels of comparative example 1 (carbon materials A), then its viscosity is larger, and comparative example 2 is (aqueous
Resin emulsion) too high levels, then the additive amount of carbon materials A will be less, cannot access answering for high-content carbon materials A
The additive amount of Heshui conductive emulsion, comparative example 3 (dispersing agent) is excessive, then its viscosity is larger.
Further, from embodiment 1 and embodiment 2 as can be seen that the content of carbon materials A is more, viscosity is bigger.From
Embodiment 3 and embodiment 4 are as can be seen that the composite water soluble conductive emulsion obtained using the dispersing agent of high molecular weight, dispersion effect
Fruit is more preferable, and viscosity is smaller.The addition that can be seen that the dispersing agent of high molecular weight from embodiment 6 and embodiment 7, can be further
Reduce the viscosity of composite water soluble conductive emulsion.
Embodiment two
Water-soluble conducting ink is formed after addition carbon materials B in the composite water soluble conductive emulsion that embodiment one provides,
And conductive coating is prepared using the above method, the body resistivity of conductive coating is measured, measuring method is: surveying by four probe method
Coating surface resistivity is obtained, coating layer thickness is measured by micrometer caliper, body resistivity is equal to surface resistivity multiplied by thickness.Obtain table
3,
The additive amount of 3 carbon materials B of table and the body resistivity of conductive coating
From table 3 it can be seen that the too high levels of comparative example 1 (carbon materials A), then its viscosity is larger, and mobility is high, body electricity
Resistance rate is big.The too high levels of comparative example 2 (resin aqueous emulsion), the additive amount of carbon materials A is few, and body resistivity is big.Comparative example 3
The additive amount of (dispersing agent) is excessive, then its viscosity is larger, and body resistivity is big.
Further, the amount addition that can be seen that carbon materials B in embodiment 1 from embodiment 1 and embodiment 2 is less, leads
The amount of the conductive filler of electrocoat is few, and body resistivity is larger, poorly conductive.It can from embodiment 3 and the comparison of embodiment 4
Out, in the identical situation of the additive amount of conductive filler, the addition of high molecular weight dispersant can be such that the dispersion of carbon materials A imitates
Fruit is more preferable, and the electric conductivity of obtained conductive coating is also more preferably.It is from embodiment 8 as can be seen that more in carbon materials A additive amount
In the case of, can not add carbon materials B will not excessively influence the electric conductivity of conductive coating.
Embodiment three
Composite water soluble conductive emulsion is carried out for the parameter of each component provided using the embodiment 7 in above-described embodiment one
Preparation.
The preparation method of embodiment 9 is: carbon materials A and dispersing agent being dispersed in water to obtain aqueous liquid dispersion.Preparation
Seed emulsion prepares pre-emulsion, and pre-emulsion is divided into the first pre-emulsion and the second pre-emulsion.First by the first pre-emulsification
Liquid is added in seed emulsion, adds aqueous liquid dispersion, is eventually adding the second pre-emulsion and obtains composite water soluble conductive emulsion.
The preparation method of embodiment 10 is: carbon materials A and dispersing agent being dispersed in water to obtain aqueous liquid dispersion.Preparation
Seed emulsion prepares pre-emulsion.First pre-emulsion is added in seed emulsion, aqueous liquid dispersion is added, obtains Compound Water
Property conductive emulsion.
The preparation method of comparative example 4 is: it is identical as the preparation method of embodiment 10, but do not add dispersing agent.
The preparation method of comparative example 5 is: carbon materials A and dispersing agent being dispersed in water to obtain aqueous liquid dispersion.Preparation
Seed emulsion prepares pre-emulsion.Aqueous liquid dispersion is first added into seed emulsion, is eventually adding pre-emulsion and obtains Compound Water
Property conductive emulsion.
Wherein, embodiment 9, embodiment 10, comparative example 4 and comparative example 5 provide the different charging progresses of resin monomer.
The composite water soluble that embodiment 9, embodiment 10, comparative example 4 and comparative example 5 obtain is detected respectively using the method that embodiment one provides
The viscosity of conductive emulsion, and the method provided using embodiment two are made water-soluble conducting ink, and detect and pass through waterborne conductive
The body resistivity for the conductive coating that ink is prepared obtains table 4,
The viscosity of 4 composite water soluble conductive emulsion of table and the body resistivity of conductive coating
From table 4, it can be seen that not adding dispersing agent compared with comparative example 4 from embodiment 9, can make to be prepared compound
The viscosity of waterborne conductive lotion is high, poor fluidity, poor dispersion.From embodiment 10 compared with comparative example 5, pre-emulsification is first added
Liquid, the viscosity for adding the composite water soluble conductive emulsion that aqueous dispersion obtains is lower, and mobility is more preferable, and dispersibility is more preferably.From
Embodiment 9 and the comparison of embodiment 10 add aqueous liquid dispersion as can be seen that the first pre-emulsion is first added, and are eventually adding the
Two pre-emulsions, that is, aqueous liquid dispersion is added during pre-emulsion is added, obtained composite water soluble conductive emulsion
Viscosity it is lower, mobility is more preferable, and dispersibility is higher, and the conductive effect of obtained conductive coating is more preferable.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of composite water soluble conductive emulsion, which is characterized in that including water composite water soluble conductive emulsion composite water soluble conductive emulsion,
Carbon materials A and resin aqueous emulsion, wherein the carbon materials A accounts for the mass percent of the composite water soluble conductive emulsion
For 0.1%-40%, the mass percent that the resin aqueous emulsion accounts for the composite water soluble conductive emulsion is 5%-60%,
It is 100-4000cp in the viscosity of (25 ± 1) DEG C described composite water soluble conductive emulsion.
2. composite water soluble conductive emulsion according to claim 1, which is characterized in that the carbon materials A accounts for described compound
The mass percent of waterborne conductive lotion is 1%-30%, and the resin aqueous emulsion accounts for the composite water soluble conductive emulsion
Mass percent is 30%-60%；
Optionally, it is 5%-20%, the water that the carbon materials A, which accounts for the mass percent of the composite water soluble conductive emulsion,
Property resin emulsion account for the composite water soluble conductive emulsion mass percent be 40%-60%；
Optionally, the resin aqueous emulsion includes acrylic emulsion, styrene-acrylic emulsion, epoxy emulsion, polyaminoester emulsion, polyethylene
Wax emulsion and the lotion of ptfe emulsion and its derivative it is one or more；
Optionally, the viscosity of the composite water soluble conductive emulsion is 1000-2000cp at (25 ± 1) DEG C.
3. composite water soluble conductive emulsion according to claim 1, which is characterized in that the carbon materials A includes carbon nanometer
One of pipe, graphene and fullerene are a variety of；
Optionally, the caliber of the carbon nanotube is 0.01-20 μm, and optionally, the caliber of the carbon nanotube is 0.1-10 μ
M, optionally, the caliber of the carbon nanotube are 0.1-1 μm；
Optionally, the length of the carbon nanotube is 0.1-50 μm, and optionally, the length of the carbon nanotube is 0.1-20 μ
M, optionally, the length of the carbon nanotube are 1-10 μm；
Optionally, the lamella number of plies of the graphene is 1-10 layers, and optionally, the lamella number of plies of the graphene is 1-5 layers,
Optionally, the lamella number of plies of the graphene is 1-2 layers；
Optionally, the piece diameter of graphene is having a size of 0.01 μm -20 μm, and optionally, the piece diameter of the graphene is having a size of 0.1-
10 μm, optionally, the piece diameter of the graphene is having a size of 0.1-1 μm.
4. composite water soluble conductive emulsion according to claim 1-3, which is characterized in that the composite water soluble is led
Electric lotion further includes dispersing agent, the dispersing agent account for the composite water soluble conductive emulsion mass percent be not higher than 0.1%,
Optionally, the dispersing agent account for the composite water soluble conductive emulsion mass percent be not higher than 0.01%, it is optionally, described
The mass percent that dispersing agent accounts for the composite water soluble conductive emulsion is not higher than 0.0001%；
Optionally, the dispersing agent is water-soluble polymer；
Optionally, the molecular weight of the water-soluble polymer is 10,000-100 hundred million, optionally, the molecule of the water-soluble polymer
Amount is 1,000,000-10 hundred million, and optionally, the molecular weight of the water-soluble polymer is 10,000,000-1 hundred million；
Optionally, the water-soluble polymer includes polyvinyl alcohol, polyvinylamine, polyvinylpyrrolidone, polyethylene glycol, poly- third
One of olefin(e) acid, polyacrylamide, polyurethane, water-base epoxy polymer and water-soluble cellulose are a variety of.
5. a kind of composite water soluble conductive emulsion, which is characterized in that including water, carbon materials A and resin aqueous emulsion, wherein institute
Stating carbon materials A and accounting for the mass percent of the composite water soluble conductive emulsion is 0.1%-40%, and the resin aqueous emulsion accounts for
The mass percent of the composite water soluble conductive emulsion is 5%-60%；Wherein, at least part quilt of the carbon materials A
It is wrapped in the resin aqueous emulsion.
6. a kind of preparation method of composite water soluble conductive emulsion, which comprises the steps of:
Disperse the carbon materials A and dispersing agent to obtain aqueous liquid dispersion in water；
Prepare seed emulsion；
Prepare pre-emulsion；
First the pre-emulsion is added in the seed emulsion, adds the aqueous liquid dispersion.
7. preparation method according to claim 6, which is characterized in that by the pre-emulsion be divided into the first pre-emulsion and
First pre-emulsion is first added in the seed emulsion, adds the aqueous liquid dispersion, finally by the second pre-emulsion
Second pre-emulsion is added；
Optionally, the preparation method of the seed emulsion, comprising: emulsifier and initiator are mixed, resin monomer shape is added
At the seed emulsion；
Optionally, the preparation method of the pre-emulsion, comprising: emulsifier and resin monomer are mixed to form the pre-emulsification
Liquid；
Optionally, the emulsifier includes one in fatty acid salt, RA rosin acid, sulfate, sulfonate, alkylammonium and quaternary ammonium salt
Kind is a variety of；
Optionally, the resin monomer includes acrylate monomer, phenprobamate monomer, epoxy monomer and phenolic resin list
Body it is one or more；
Optionally, the initiator includes azodiisobutyronitrile, dibenzoyl peroxide, cumyl peroxide, peroxidating two
One of alkyl and diacyl peroxides are a variety of.
8. a kind of water-soluble conducting ink, which is characterized in that including the conductive cream of the described in any item composite water solubles of claim 1-5
Liquid and carbon materials B's, water-based ink auxiliary agent and cosolvent is one or more.
9. water-soluble conducting ink according to claim 8, which is characterized in that the water-based ink auxiliary agent include levelling agent,
One of thickener, defoaming agent, pH adjusting agent, mould inhibitor, drying retardant, quick dry agent are a variety of；
The cosolvent includes including water and organic solvent, and optionally, the organic solvent includes ethyl alcohol, ethylene glycol, propyl alcohol, third
Glycol, isopropanol, acetone, butanol, butanediol, isobutanol, butanone, isobutyl ketone, N-Methyl pyrrolidone, N, N- dimethyl methyl
One of amide, n,N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, dioxane are a variety of；
The carbon materials B includes one of carbon black, carbon nanotube, graphite, graphene, carbon fiber, fullerene or a variety of.
10. water-soluble conducting ink according to claim 8, which is characterized in that the carbon materials A and the carbon material
Material B account for the water-soluble conducting ink solid content mass percent be 20%-60%, optionally, the carbon materials A with
And it is 30%-50% that the carbon materials B, which accounts for the mass percent of the solid content of the water-soluble conducting ink,.
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