CN107903713A - Highly conductive watersoluble plumbago alkene electrically conductive ink and preparation method thereof, composition - Google Patents
Highly conductive watersoluble plumbago alkene electrically conductive ink and preparation method thereof, composition Download PDFInfo
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- CN107903713A CN107903713A CN201711222869.0A CN201711222869A CN107903713A CN 107903713 A CN107903713 A CN 107903713A CN 201711222869 A CN201711222869 A CN 201711222869A CN 107903713 A CN107903713 A CN 107903713A
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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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- 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
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated 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
- C09D11/106—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
Abstract
The present invention is on a kind of highly conductive watersoluble plumbago alkene electrically conductive ink and preparation method thereof, composition, and the composition for highly conductive watersoluble plumbago alkene electrically conductive ink includes the component of following mass fraction:20 30 parts of conductive unit, 15 30 parts of bridging agent, 0.1 20 parts of auxiliary agent, 50 100 parts of water.Composition using the present invention and preparation method, sheet resistance≤20 Ω/, conductive unit content≤30% of the highly conductive watersoluble plumbago alkene electrically conductive ink prepared have that conductive unit content is low, mechanical property is good and the advantage of high conductivity.Meanwhile using water as solvent, there is environmentally protective, nontoxic, the non-ignitable significant Environmental Safety such as not quick-fried.
Description
Technical field
The present invention relates to electrically conductive ink field, more particularly to a kind of highly conductive watersoluble plumbago alkene electrically conductive ink and its preparation side
Method, composition.
Background technology
Electrically conductive ink is addition conductive filler powder, such as carbon black, graphite, silver, copper, shape in macromolecule polymer material
Into a kind of conductive polymeric composite, be widely used in printed circuit board (PCB), thin film switch, REID radio frequency identifications, print
Brush resistance etc..By the difference of conductive filler property, electrically conductive ink, which can be divided into gold system electrically conductive ink, silver system electrically conductive ink, copper system, leads
Electric ink and carbon series conductive ink etc., gold system electrically conductive ink high comprehensive performance, but price are high, and application range is limited only to thick film
Integrated circuit etc. has the product of particular/special requirement.Silver system electrically conductive ink electric conductivity is only second to bronze, but, temperature more sensitive to temperature
Highly conductive ability is strong, on the contrary then poor.Copper system electrically conductive ink is cost-effective using relatively broad, but there are it is oxidizable the shortcomings that.
Carbon series conductive ink is cheap, not oxidizable, and performance is stablized, but electric conductivity is relatively poor.
At present, the conductive filler that carbon series conductive ink uses mainly has electrically conductive graphite, acetylene black, carbon black, carbon nanotubes, stone
Black alkene etc., it is mainly used in printed resistor and thin film switch.Graphene is stripped out from graphite material, by carbon atom
The two dimensional crystal of only one layer of atomic thickness of composition.Connection in graphene between each carbon atom is very flexible, outer when applying
During portion's mechanical force, carbon atom face, so that carbon atom need not be rearranged to adapt to external force, is also maintained for finishing with regard to flexural deformation
Structure is stablized.The lattice structure of this stabilization makes carbon atom have outstanding electric conductivity.It is prepared into using graphene as conductive filler
The electrically conductive ink arrived has good electric conductivity and printing, with metal system electrically conductive ink, such as gold system, silver system, copper system conduction
Ink is compared, and Graphene conductive ink has huge cost advantage；Compared with traditional carbon series conductive ink product, graphene
Electrically conductive ink has significant advantage again in terms of electric conductivity.
At present, the research and development of electrically conductive ink are concentrated mainly on solvent-based ink, improve the major measure of the electric conductivity of ink
It is the content for increasing conductive agent, commonly reaches the content of 30-95%, although the electric conductivity of ink can be greatly improved in this,
But in actual use, due to the too high levels of conductive agent, workability, presentation quality and the stability in use of film
Poor etc. property, film pliability and poor adhesive force, phenomena such as being also easy to produce micro-crack and come off, and solvent-based ink contains greatly
Poisonous and hazardous volatile organic matter is measured, severely impacts human body health and environmental pollution.
Therefore, low conductive filler content how is prepared, there is the good water-soluble conducting ink of high conductivity, mechanical property also
Need further to be researched and developed.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of highly conductive watersoluble plumbago alkene electrically conductive ink and its preparation
Method, the electrically conductive ink have the advantages that conductive agent content is low, mechanical property is good and high conductivity.
The embodiment of the present invention provides a kind of composition for highly conductive watersoluble plumbago alkene electrically conductive ink, including following quality
The component of number:20-30 parts of conductive unit, 15-30 parts of bridging agent, 0.1-20 parts of auxiliary agent, 50-100 parts of water.
The embodiment of the present invention provides a kind of composition for highly conductive watersoluble plumbago alkene electrically conductive ink, including following matter again
Measure the component of number:15-25 parts of conductive unit, 20-25 parts of bridging agent, 1-15 parts of auxiliary agent, 60-90 parts of water.
Preferably, conductive unit content≤30%.
Preferably, the conductive unit is led for graphene or the mixture of graphene and other conductive units, described other
One or more of the electric unit in carbon nanotubes, conductive carbon black and electrically conductive graphite；The mass fraction of the graphene is
10-25 parts.
Preferably, the bridging agent is aqueous acrylic emulsion, aqueous polyurethane emulsion, aqueous epoxy resin emulsion, benzene
One or more in acrylic emulsion, silicone acrylic emulsion, acrylate and vinyl acetate emulsion, fluorine carbon emulsion and ethylene-vinyl acetate copolymer EVA lotions.
Preferably, the auxiliary agent is selected from least one of following mass fraction component：
1-5 parts of defoamer, 0.1-5 parts of auxiliary rheological agents, 2-5 parts of moistening flatting agent, 10-20 parts of wetting dispersing agent, coupling agent
One or more in 1-3 parts of 1-3 parts, 1-5 parts of coalescents, 0.1-0.5 parts of Antisepticize and mildew preventive and pH adjusting agent；
The defoamer be selected from mineral oil, paraffin oil, organosilicon, polyethers, mineral oil emulsion, polyether-modified mineral oil,
One or more in organic silicon modified by polyether, polyether-modified dimethyl silicone polymer；
The auxiliary rheological agents are selected from cellulose ether and its derivative, association type alkali swollen thickener, non-association type alkali soluble
One in the non-polyurethane thickener of swollen thickener, polyurethane thickener, hydrophobically modified, solvay-type organo-metallic compound thickener
Kind is several；
The moistening flatting agent is selected from ionic acrylic copolymer, nonionic acrylic copolymer, polyether-modified
Dimethyl silicone polymer, organic silicon modified by polyether, fluorine-carbon modified organosilicon, fluorine-carbon modified polyacrylate aqueous solution, organosilicon
One kind or several in acrylate, modified polyorganosiloxane lotion, nonionic polyethylene fat, mixing nonionic surfactant
Kind.
The wetting dispersing agent is selected from ammonium polyacrylate salt, polyacrylic acid sodium salt, polyacrylic acid sylvite, sodium polycarboxylate
Salt, polycarboxylic acids ammonium salt, hydrophobically modified polycarboxylic acids sylvite, phosphoric acid ester complexes, self-emulsifying modified polyacrylate, polycarboxylic acids alkanol
Amine, fatty acid modified polyester, alkyl phenol ethoxy sulfate, octyl phenol polyoxyethylene ether, ethoxylated fatty acid, ethyoxyl side chain
Alcohol, anionic wetting dispersing agent, cationic wetting dispersing agent, non-ionic wetting dispersing agent, the affinity groups containing pigment
One or more in high molecular polymer.
The coupling agent is selected from silane coupling agent, titanate coupling agent, aluminate coupling agent, phosphate coupling agent, boron
One or more in acid esters coupling agent, bimetallic coupling agent, chromium complex.
The coalescents be selected from alcohol ester 12, ethylene glycol ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether,
Diethylene glycol monobutyl ether, triethylene glycol monomethyl ether, Triethylene glycol ethyl ether, triethylene glycol butyl ether, propylene glycol monomethyl ether, the third two
Alcohol list propyl ether, propylene glycol monobutyl ether, glycol tertiary butyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol mono butyl
Ether, tripropylene glycol n-butyl ether, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetic acid esters, dimethyl ether, ethylene glycol phenyl
One or more in ether, propylene glycol phenylate, diacetone alcohol；
The Antisepticize and mildew preventive is selected from isothiazolinone derivatives, benzimidazole compound, substituted arene compound, has
One or more in machine bromine compounds, organic amine compound, compound in triazine class；
The pH adjusting agent is selected from ammonium hydroxide, monoethanolamine, diethanol amine, triethanolamine, dimethylethanolamine, methyl diethyl
One or more in hydramine, 2-amino-2-methyl-1-propanol.
The embodiment of the present invention also provides a kind of prepares highly conductive watersoluble plumbago alkene electrically conductive ink using combinations of the above thing
Method, comprises the following steps：
(1) each raw material is weighed according to mass fraction, is graphene mass fraction by graphene, water and mass fraction
The wetting dispersing agent of 50%-80% is mixed, and obtains the first mixture；
(2) first mixture progress energy-gathered ultrasonic is disperseed, obtains watersoluble plumbago alkene dispersion liquid；
(3) give in the watersoluble plumbago alkene dispersion liquid and add other conductive units, add defoamer, coupling agent and residue
Wetting dispersing agent be mixed, obtain the second mixture；
(4) the second mixture that will be obtained through step (3) is ground, then ground slurries filtration, acquisition is water-based
Electrocondution slurry；
(5) the waterborne conductive slurry and the bridging agent that obtain step (4), auxiliary rheological agents, moistening flatting agent, coalescents,
Antisepticize and mildew preventive, pH adjusting agent are mixed evenly, that is, obtain highly conductive watersoluble plumbago alkene electrically conductive ink.
Preferably, the stir speed (S.S.) in the step (1) and step (3) is 500-1000rpm, mixing time 30-
60min；
Ultrasonic device rated power is 3000W in the step (2), working frequency is 20 ± 1kHz, ultrasonic time 8-
20h；
Grinding rate in the step (4) is 2500-3000rpm, milling time 8-20h；
Stir speed (S.S.) is 400-800rpm, mixing time 30-60min in the step (5).
The embodiment of the present invention provides a kind of highly conductive watersoluble plumbago alkene electrically conductive ink again, is prepared into according to above-mentioned method
Arrive.
The embodiment of the present invention provide again a kind of highly conductive watersoluble plumbago alkene electrically conductive ink far infrared heating, printed resistor,
Thin film switch, radio frequency identification, intelligent packaging, conducting wire, the application on electromagnetic shielding.
By above-mentioned technical proposal, the highly conductive watersoluble plumbago alkene electrically conductive ink of the present invention at least has following advantages：
Due to present invention employs above-mentioned technical proposal, the sheet resistance of the highly conductive watersoluble plumbago alkene electrically conductive ink developed≤
20 Ω/, conductive unit content≤30%, have that conductive unit content is low, mechanical property is good and the advantage of high conductivity.Together
When, using water as solvent, there is environmentally protective, nontoxic, the non-ignitable significant Environmental Safety such as not quick-fried.
Embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Preferred embodiment, to according to highly conductive watersoluble plumbago alkene electrically conductive ink proposed by the present invention and preparation method thereof its specific embodiment party
Formula, structure, feature and its effect, describe in detail as after.In the following description, different " embodiment " or " embodiment " refers to
It is not necessarily the same embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be by any suitable shapes
Formula combines.
Embodiment 1
In the present embodiment, the mass fraction composition of each raw material is：Graphene：10 parts, conductive carbon black：10 parts, water-based poly- ammonia
Ester lotion：15 parts, anionic wetting dispersing agent：10 parts, titanate coupling agent：1 part, organic silicon modified by polyether levelling agent：2
Part, polyether antifoam agent：1 part, alcohol ester 12：5 parts, isothiazolinone derivatives Antisepticize and mildew preventive：0.1 part, ammonium hydroxide：1 part, association
Type alkali swollen thickener：1 part, water：50 parts.
A kind of highly conductive watersoluble plumbago alkene electrically conductive ink provided by the invention, preparation process are as follows：
(1) by 50 parts of water, 5 parts of dispersants, at room temperature, 10min is stirred under the rotating speed of 500rpm, then slowly added
Enter 10 parts of graphenes, 60min is stirred under 1000rpm rotating speeds；
(2) and then by step (1) mixture obtained is put into energy-gathered ultrasonic dispersion machine, is in ultrasonic power
3000W, frequency are ultrasonic disperse 8h under 20kHz, obtain watersoluble plumbago alkene dispersion liquid；
(3) the watersoluble plumbago alkene dispersion liquid that step (2) obtains is put into high speed dispersion grinder, in the rotating speed of 500rpm
5 parts of dispersants of lower addition, 1 part of coupling agent, 1 part of defoamer, are then slowly added into 10 parts of conductive carbon blacks, in the rotating speed of 1000rpm
Lower stirring 60min；
(4) mixture that step (3) obtains is ground, 20h is ground under the rotating speed of 2500rpm, filtering and discharging, is obtained
Obtain waterborne conductive slurry；
(5) by step (4) obtain waterborne conductive slurry and 15 parts of aqueous polyurethane emulsions, 2 parts of moistening flatting agents, 5 parts
12,0.1 parts of Antisepticize and mildew preventives of alcohol ester, 1 part of ammonium hydroxide, 1 part of thickener mixing, 30min is stirred under 800rpm rotating speeds, is obtained high
Conductive water-based Graphene conductive ink.
Embodiment 2
In the present embodiment, the mass fraction composition of each raw material is：Graphene：12 parts, electrically conductive graphite powder：4 parts, conductive carbon
It is black：6 parts, aqueous acrylic emulsion：23 parts, ammonium polyacrylate dipersant：12 parts, 2 parts of silane acid esters coupling agent, organosilicon third
4 parts of olefin(e) acid ester moistening flatting agent, organic silicon defoamer：2 parts, coalescents ethylene glycol monobutyl ether：3 parts, benzimidazole compound
Antisepticize and mildew preventive：0.2 part, pH adjusting agent 2-amino-2-methyl-1-propanol：3 parts, cellulose ether thickener：0.1 part, water：80
Part.
A kind of highly conductive watersoluble plumbago alkene electrically conductive ink provided by the invention, preparation process are as follows：
(1) by 80 parts of water, 8 parts of dispersants, at room temperature, 10min is stirred under the rotating speed of 500rpm, then slowly added
Enter 12 parts of graphenes, 60min is stirred under 1000rpm rotating speeds；
(2) and then by step (1) mixture obtained is put into energy-gathered ultrasonic dispersion machine, is in ultrasonic power
3000W, frequency are ultrasonic disperse 12h under 20kHz, obtain watersoluble plumbago alkene dispersion liquid；
(3) the watersoluble plumbago alkene dispersion liquid that step (2) obtains is put into high speed dispersion grinder, in the rotating speed of 500rpm
4 parts of dispersants of lower addition, 2 parts of coupling agents, 2 parts of defoamers, are then slowly added into 4 parts of electrically conductive graphite powders, 6 parts of conductive carbon blacks,
60min is stirred under the rotating speed of 1000rpm；
(4) mixture that step (3) obtains is ground, 16h is ground under the rotating speed of 2800rpm, filtering and discharging, is obtained
Obtain waterborne conductive slurry；
(5) by step (4) obtain waterborne conductive slurry and 23 parts of aqueous acrylic emulsions, 4 parts of moistening flatting agents, 3 parts
Ethylene glycol monobutyl ether, 0.2 part of Antisepticize and mildew preventive, 3 parts of pH adjusting agents, 0.1 part of thickener mixing, are stirred under 800rpm rotating speeds
40min, obtains highly conductive watersoluble plumbago alkene electrically conductive ink.
Embodiment 3
In the present embodiment, the mass fraction composition of each raw material is：Graphene：15 parts, electrically conductive graphite powder：2 parts, conductive carbon
It is black：5 parts, carbon nanotubes：6 parts, 28 parts of styrene-acrylic emulsion, the high polymer dispersion containing close pigment group：16 parts, Aluminate
2 parts of coupling agent, 3 parts of nonionic acrylic copolymer moistening flatting agent, mineral oil antifoam agent：3 parts, three ethanol of pH adjusting agent
Amine：2 parts, organic amine compound Antisepticize and mildew preventive：0.4 part, coalescents diethylene glycol monobutyl ether：2 parts, water：90 parts.
A kind of highly conductive watersoluble plumbago alkene electrically conductive ink provided by the invention, preparation process are as follows：
(1) by 90 parts of water, 10 parts of dispersants, at room temperature, 10min is stirred under the rotating speed of 500rpm, then slowly
15 parts of graphenes are added, 40min is stirred under 1000rpm rotating speeds；
(2) and then by step (1) mixture obtained is put into energy-gathered ultrasonic dispersion machine, is in ultrasonic power
3000W, frequency are ultrasonic disperse 16h under 20kHz, obtain watersoluble plumbago alkene dispersion liquid；
(3) the watersoluble plumbago alkene dispersion liquid that step (2) obtains is put into high speed dispersion grinder, in the rotating speed of 500rpm
It is lower addition 6 parts of dispersants, 2 parts of coupling agents, 3 parts of defoamers, be then slowly added into 2 parts of electrically conductive graphite powders, 5 parts of conductive carbon blacks, 6 parts
Carbon nanotubes, 60min is stirred under the rotating speed of 1000rpm；
(4) mixture that step (3) obtains is ground, 12h is ground under the rotating speed of 2800rpm, filtering and discharging, is obtained
Obtain waterborne conductive slurry；
(5) waterborne conductive slurry and 28 parts of styrene-acrylic emulsions, 3 parts of moistening flatting agents, the 2 parts of pH obtained step (4) are adjusted
Agent, 0.4 part of Antisepticize and mildew preventive, 2 parts of coalescents mixing, stir 60min under 600rpm rotating speeds, obtain highly conductive watersoluble plumbago
Alkene electrically conductive ink.
Embodiment 4
In the present embodiment, the mass fraction composition of each raw material is：Graphene：20 parts, conductive carbon black：6 parts, carbon nanotubes：4
Part, 30 parts of aqueous epoxy emulsion, ammonium polyacrylate dipersant：20 parts, 3 parts of titanate coupling agent, modified polyorganosiloxane wetting
5 parts of levelling agent, polyether-modified mineral oil antifoam agent：5 parts, ammonium hydroxide：3 parts, water：100 parts.
A kind of highly conductive watersoluble plumbago alkene electrically conductive ink provided by the invention, preparation process are as follows：
(1) by 100 parts of water and 15 parts of dispersants, at room temperature, 10min, Ran Houhuan are stirred under the rotating speed of 500rpm
Slowly 20 parts of graphenes are added, 60min is stirred under 1000rpm rotating speeds；
(2) and then by step (1) mixture obtained is put into energy-gathered ultrasonic dispersion machine, is in ultrasonic power
3000W, frequency are ultrasonic disperse 20h under 20kHz, obtain watersoluble plumbago alkene dispersion liquid；
(3) the watersoluble plumbago alkene dispersion liquid that step (2) obtains is put into high speed dispersion grinder, in the rotating speed of 500rpm
5 parts of dispersants of lower addition, 3 parts of coupling agents, 5 parts of defoamers, are then slowly added into 6 parts of conductive carbon blacks, 4 parts of carbon nanotubes,
60min is stirred under the rotating speed of 1000rpm；
(4) mixture that step (3) obtains is ground, 8h is ground under the rotating speed of 3000rpm, filtering and discharging, is obtained
Obtain waterborne conductive slurry；
(5) the waterborne conductive slurry and 30 parts of aqueous epoxy emulsions, 5 parts of moistening flatting agents, 3 parts of ammonia for obtaining step (4)
Water mixes, and stirs 50min under 600rpm rotating speeds, obtains highly conductive watersoluble plumbago alkene electrically conductive ink.
Embodiment 5
In the present embodiment, the mass fraction composition of each raw material is：Graphene：25 parts of styrene-acrylic emulsions：8 parts of silicone acrylic emulsions：10
Part Sodium Polyacrylate dipersant：9 parts of self-emulsifying modified polyacrylic acid fat dispersants：4 parts of paraffin oil defoamers：2 parts of polyethers change
Property mineral oil antifoam agent：1 part of titanate coupling agent：1 part of aluminate coupling agent：1 part of cellulose ether thickener：0.2 part of polyurethane
Thickener：3 parts of ammonium hydroxide：1 part of 2-amino-2-methyl-1-propanol：70 parts of water.
A kind of highly conductive watersoluble plumbago alkene electrically conductive ink provided by the invention, preparation process are as follows：
(1) by 70 parts of water and 13 parts of dispersants, at room temperature, 10min is stirred under the rotating speed of 500rpm, then slowly
25 parts of graphenes are added, 40min is stirred under 1000rpm rotating speeds；
(2) and then by step (1) mixture obtained is put into energy-gathered ultrasonic dispersion machine, is in ultrasonic power
3000W, frequency are ultrasonic disperse 16h under 20kHz, obtain watersoluble plumbago alkene dispersion liquid；
(3) the watersoluble plumbago alkene dispersion liquid that step (2) obtains is put into high speed dispersion grinder, in the rotating speed of 600rpm
2 parts of coupling agents of lower addition, 3 parts of defoamers, 1 part of ammonium hydroxide, 1 part of 2-amino-2-methyl-1-propanol, are stirred under the rotating speed of 800rpm
Mix 60min；
(4) mixture that step (3) obtains is ground, 16h is ground under the rotating speed of 2600rpm, filtering and discharging, is obtained
Obtain waterborne conductive slurry；
(5) the waterborne conductive slurry and 8 parts of styrene-acrylic emulsions, 10 parts of silicone acrylic emulsions, 0.2 part of cellulose for obtaining step (4)
Ether, 3 parts of polyurethane thickener mixing, stir 40min under 600rpm rotating speeds, obtain highly conductive watersoluble plumbago alkene electrically conductive ink.
By highly conductive watersoluble plumbago alkene conductive ink application obtained by the various embodiments described above on base material, drying at room temperature cures
Afterwards, it is tested for the property, wherein film thickness of dry film is 20-30 μm, and test result is as shown in the table：
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Sheet resistance (Ω/) | 9.62 | 12.89 | 13.23 | 10.54 | 18.92 |
| Adhesive force (level) | 1 | 1 | 1 | 1 | 1 |
| Pliability (mm) | 2 | 2 | 2 | 2 | 2 |
In above example, the sheet resistance parameter of electrically conductive ink is specific to survey by using the double electrical measurement four-point probes of RTS-9
Method for testing is as follows：
By conductive ink application in PET (Polyethylene terephthalate, poly terephthalic acid class plastics) base
On material, after film is completely dried curing, its film thickness of dry film is 20-30 μm, and sample is placed on tester operation console, is operated
Probe station depresses probe, probe is contacted with film coated surface, turn-on current, selects suitable testing range, in electric current value stabilization
After numerical value as defined in instrument, film sheet resistance test is carried out.
Attachment force parameter passes through GB 1720-89《Paint film adhesion determination method》Measure；
Pliability parameter passes through GB/T 1731-93《Paint film flexibility determination method》Measure.
Highly conductive watersoluble plumbago alkene electrically conductive ink prepared by the embodiment of the present invention can be used for far infrared heating, printing electricity
Resistance, thin film switch, radio frequency identification, intelligent packaging, conducting wire, on electromagnetic shielding.With conductive unit content is low, mechanical property
Good and high conductivity advantage.
The above described is only a preferred embodiment of the present invention, not make limitation in any form to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit according to the present invention
Any simple modification, equivalent change and modification made to above example, in the range of still falling within technical solution of the present invention.
Claims (10)
- A kind of 1. composition for highly conductive watersoluble plumbago alkene electrically conductive ink, it is characterised in that:Including following mass fraction Component:20-30 parts of conductive unit, 15-30 parts of bridging agent, 0.1-20 parts of auxiliary agent, 50-100 parts of water.
- A kind of 2. composition for highly conductive watersoluble plumbago alkene electrically conductive ink, it is characterised in that:Including following mass fraction Component:15-25 parts of conductive unit, 20-25 parts of bridging agent, 1-15 parts of auxiliary agent, 60-90 parts of water.
- 3. composition according to claim 1, it is characterised in that：Content≤30% of the conductive unit.
- 4. composition according to claim 1, it is characterised in that：The conductive unit is graphene or graphene and other The mixture of conductive unit, the one kind or several of other described conductive units in carbon nanotubes, conductive carbon black and electrically conductive graphite Kind；The mass fraction of the graphene is 10-25 parts.
- 5. composition according to claim 1, it is characterised in that：The bridging agent is aqueous acrylic emulsion, water-based poly- Urethane lotion, aqueous epoxy resin emulsion, styrene-acrylic emulsion, silicone acrylic emulsion, acrylate and vinyl acetate emulsion, fluorine carbon emulsion and ethene-vinyl acetate One or more in copolymer EVA lotions.
- 6. according to claim 1-5 any one of them compositions, it is characterised in that：The auxiliary agent is selected from following mass fraction group At least one divided：1-5 parts of defoamer, 0.1-5 parts of auxiliary rheological agents, 2-5 parts of moistening flatting agent, 10-20 parts of wetting dispersing agent, coupling agent 1-3 One or more in part, 1-5 parts of coalescents, 0.1-0.5 parts of Antisepticize and mildew preventive and 1-3 parts of pH adjusting agent；The defoamer is selected from mineral oil, paraffin oil, organosilicon, polyethers, mineral oil emulsion, polyether-modified mineral oil, polyethers One or more in modified organic silicon, polyether-modified dimethyl silicone polymer；The auxiliary rheological agents are selected from cellulose ether and its derivative, association type alkali swollen thickener, the non-swollen increasing of association type alkali soluble Thick dose, polyurethane thickener, the non-polyurethane thickener of hydrophobically modified, one kind in solvay-type organo-metallic compound thickener or It is several；The moistening flatting agent is selected from ionic acrylic copolymer, nonionic acrylic copolymer, polyether-modified poly- two Methylsiloxane, organic silicon modified by polyether, fluorine-carbon modified organosilicon, fluorine-carbon modified polyacrylate aqueous solution, organosilicon propylene One or more in acid esters, modified polyorganosiloxane lotion, nonionic polyethylene fat, mixing nonionic surfactant；The wetting dispersing agent is selected from ammonium polyacrylate salt, polyacrylic acid sodium salt, polyacrylic acid sylvite, polycarboxylate sodium, poly- Ammonium carboxylate salt, hydrophobically modified polycarboxylic acids sylvite, phosphoric acid ester complexes, self-emulsifying modified polyacrylate, polycarboxylic acids alkanolamine, fat Fat acid modified poly ester, alkyl phenol ethoxy sulfate, octyl phenol polyoxyethylene ether, ethoxylated fatty acid, ethyoxyl branched-chain alcoho, the moon Ionic wetting dispersing agent, cationic wetting dispersing agent, non-ionic wetting dispersing agent, the macromolecule of the affinity groups containing pigment One or more in polymer；The coupling agent is selected from silane coupling agent, titanate coupling agent, aluminate coupling agent, phosphate coupling agent, borate One or more in coupling agent, bimetallic coupling agent, chromium complex；The coalescents are selected from alcohol ester 12, ethylene glycol ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethyl Glycol monobutyl ether, triethylene glycol monomethyl ether, Triethylene glycol ethyl ether, triethylene glycol butyl ether, propylene glycol monomethyl ether, propane diols list Propyl ether, propylene glycol monobutyl ether, glycol tertiary butyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monopropyl ether, Dipropylene glycol mono-n-butyl Ether, Tripropylene glycol n-butyl ether, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetic acid esters, dimethyl ether, ethylene glycol phenyl ether, One or more in propylene glycol phenylate, diacetone alcohol；The Antisepticize and mildew preventive is selected from isothiazolinone derivatives, benzimidazole compound, substituted arene compound, organic bromine One or more in compound, organic amine compound, compound in triazine class；The pH adjusting agent is selected from ammonium hydroxide, monoethanolamine, diethanol amine, triethanolamine, dimethylethanolamine, methyl diethanol One or more in amine, 2-amino-2-methyl-1-propanol.
- 7. usage right requires the method that 1-6 any one of them compositions prepare highly conductive watersoluble plumbago alkene electrically conductive ink, its It is characterized in that, comprises the following steps：(1) each raw material is weighed according to mass fraction, by the 50%- that graphene, water and mass fraction are graphene mass fraction 80% wetting dispersing agent is mixed, and obtains the first mixture；(2) first mixture progress energy-gathered ultrasonic is disperseed, obtains watersoluble plumbago alkene dispersion liquid；(3) give in the watersoluble plumbago alkene dispersion liquid and add other conductive units, add defoamer, coupling agent and remaining profit Hygroscopic water powder is mixed, and obtains the second mixture；(4) the second mixture that will be obtained through step (3) be ground, then by ground slurries filtration, obtain waterborne conductive Slurry；(5) by the waterborne conductive slurry that step (4) obtains and bridging agent, auxiliary rheological agents, moistening flatting agent, coalescents, anti-corrosion Mould inhibitor, pH adjusting agent are mixed evenly, that is, obtain highly conductive watersoluble plumbago alkene electrically conductive ink.
- 8. the method according to the description of claim 7 is characterized in that the stir speed (S.S.) in the step (1) and step (3) is 500-1000rpm, mixing time 30-60min；Ultrasonic device rated power is 3000W in the step (2), working frequency is 20 ± 1kHz, ultrasonic time 8-20h；Grinding rate in the step (4) is 2500-3000rpm, milling time 8-20h；Stir speed (S.S.) is 400-800rpm, mixing time 30-60min in the step (5).
- 9. a kind of highly conductive watersoluble plumbago alkene electrically conductive ink, it is characterised in that be prepared into accordance with the method for claim 8 Arrive.
- 10. the highly conductive watersoluble plumbago alkene electrically conductive ink described in a kind of claim 9 is in far infrared heating, printed resistor, film Switch, radio frequency identification, intelligent packaging, conducting wire, the application on electromagnetic shielding.
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