CN110194910A - Electric heating ink and preparation method thereof with low-work voltage and farsighted infrared emittance - Google Patents
Electric heating ink and preparation method thereof with low-work voltage and farsighted infrared emittance Download PDFInfo
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- CN110194910A CN110194910A CN201910523124.0A CN201910523124A CN110194910A CN 110194910 A CN110194910 A CN 110194910A CN 201910523124 A CN201910523124 A CN 201910523124A CN 110194910 A CN110194910 A CN 110194910A
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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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- 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
Abstract
The present invention provides the electric heating ink and preparation method thereof with low-work voltage and farsighted infrared emittance, and based on the gross mass of electric heating ink, according to mass percent meter, electric heating ink includes: three-dimensional grapheme 5~20%；Two-dimensional graphene 1~10%；Carbon nanotube 1~5%；Conductive carbon black 5~20%；Resin-bonded material 15~45%；Solvent 15~30%；Dispersing agent 1~10%；And auxiliary agent 0.5~5%.In the electric heating ink, three-dimensional grapheme, two-dimensional graphene, carbon nanotube and conductive carbon black can spatially form synergistic effect, so that electric heating ink is while meeting electric heating property standard, it is suitble to work under 36V safe voltage below, and far infrared radiation rate height, safety and environmental protection, electric heating property is stable, not oxidizable, preparation method is simple, is easy to mass preparation.
Description
Technical field
The present invention relates to thermo electric material technical fields, specifically, being related to low-work voltage and farsighted infrared emittance
Electric heating ink and preparation method thereof.
Background technique
In recent years, it with national " coal changes electricity " policy expansion, can heat, the electric heating product with far-infrared physiotherapy effect
It progresses into our lives, people is allowed to have comfortable experience.It is wide, many kinds of that electric heating product is related to field, such as low temperature
Electric radiant Heating Film, heating picture, intelligent heating clothes, heating carpet etc..In electric heating product, electric heating material is key problem in technology, is pressed
Heating principle divides, and electric heating material can be divided mainly into resistance wire, electric heating ink coating, and wherein electric heating ink coating belongs to planar
Fever, heating efficiency, electric heating uniformity, safety are much higher than linear fever.In the related technology, electric heating ink be mostly
Used under 220V high voltage condition, and the safe voltage of human body in 36V hereinafter, directly contact high working voltage product, can be to being made
User brings some potential safety problems, in addition, the problems such as that there is also heat fades is big, at high cost, film layer is easy the moisture absorption, influences to produce
The thermal stability and service life of product.
Thus, electric heating ink the relevant technologies still have much room for improvement.
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 the electric heating ink for proposing that a kind of operating voltage is low, far infrared radiation rate is high or hot property is stable.
In one aspect of the invention, the present invention provides a kind of electricity with low-work voltage and farsighted infrared emittance
Hot oil ink.According to an embodiment of the invention, the gross mass based on the electric heating ink, according to mass percent meter, the electric heating
Ink includes: three-dimensional grapheme 5~20%；Two-dimensional graphene 1~10%；Carbon nanotube 1~5%；Conductive carbon black 5~20%；
Resin-bonded material 15~45%；Solvent 15~30%；Dispersing agent 1~10%；And auxiliary agent 0.5~5%.In the electric heating ink, two
Dimension graphene, carbon nanotube and conductive carbon black can be adsorbed on the surface of three-dimensional grapheme or be filled in three-dimensional grapheme
In pore structure, allows three-dimensional grapheme, two-dimensional graphene, carbon nanotube and conductive carbon black spatially to form collaboration and make
With, so that electric heating ink while meeting electric heating property standard, is suitble to work under 36V safe voltage below, and
Far infrared radiation rate height, safety and environmental protection, electric heating property is stable, not oxidizable, preparation method is simple, is easy to mass preparation.
According to an embodiment of the invention, above-mentioned electric heating ink meets at least one of the following conditions: the carbon nanotube with
The mass ratio of the conductive carbon black is less than or equal to 1:6；The three-dimensional grapheme and the mass ratio of the two-dimensional graphene are greater than
2:1。
According to an embodiment of the invention, the specific surface area of the three-dimensional grapheme is greater than 2000m2/ g, the number of plies are less than 15 layers,
With porous structure.
According to an embodiment of the invention, the three-dimensional grapheme is globular graphite alkene.
According to an embodiment of the invention, the partial size of the globular graphite alkene is micron order.
According to an embodiment of the invention, the two-dimensional graphene have layer structure, the number of plies be less than 10 layers, piece diameter be 10~
20 microns, gray scale is≤0.1%.
According to an embodiment of the invention, the carbon nanotube includes in wound form carbon nanotube and aligned carbon-nanotubes
It is at least one.
According to an embodiment of the invention, the resistivity of the conductive carbon black is less than 10 Ω m.
According to an embodiment of the invention, the resin-bonded material includes: the first resin, first resin includes modified poly-
At least one of ester resin, acrylic resin and polyurethane；Second resin, second resin include epoxy resin, silicon tree
At least one of rouge and fluororesin.
According to an embodiment of the invention, the gross mass based on the electric heating ink, according to mass percent meter, the electric heating
Ink includes first resin 10~30% and second resin 5~15%.
According to an embodiment of the invention, the solvent is selected from butanediol, n-butanol, butyl glycol ether, Glycolic acid n butyl ester
At least one of with diethylene glycol ether acetate.
According to an embodiment of the invention, the dispersing agent is in polypyrrole, polyethylene glycol and sodium carboxymethylcellulose
It is at least one.
According to an embodiment of the invention, the auxiliary agent includes defoaming agent, levelling agent, adhesive force auxiliary agent, thickener, wetting
At least one of agent, coupling agent and promotion film forming agent.
According to an embodiment of the invention, above-mentioned electric heating ink meets at least one of the following conditions: operating voltage be less than or
Equal to 36V；Suitable for discharging the ray of 5~17 micron wave lengths；The normal direction radiance of the ray is less than or equal to 85%；Accelerate old
The power attenuation for changing test is less than or equal to 1%.
In another aspect of this invention, the present invention provides a kind of methods prepared in mentioned-above electric heating ink.Root
According to the embodiment of the present invention, this method comprises: three-dimensional grapheme, two-dimensional graphene, carbon nanotube, conductive carbon black, resin are glued
A part, solvent and dispersant in ramming material, and pre-dispersed processing is carried out to obtained mixture, it obtains pre-dispersed
Material；By in the pre-dispersed material, the resin-bonded material another part and the auxiliary agent mix, and to obtained mixture
It is ground, obtains the electric heating ink.The step of preparation process of this method " one pot goes out " is simple, easy to operate, easy,
To equipment and technical staff, harsh requirement, preparation cost be not low, it is easy to accomplish industrialized production, good economy performance, and obtain
Electric heating ink there is lower operating voltage, higher far infrared radiation rate and preferable hot stabilizability.
According to an embodiment of the invention, after the milled processed, further includes: the product obtained to the milled processed
The step of carrying out viscosity-adjusting agent.
According to an embodiment of the invention, a part in the resin-bonded material is the first resin, the resin-bonded material
In another part be the second resin.
According to an embodiment of the invention, the fineness of the particulate matter in the electric heating ink is 10~20 microns.
According to an embodiment of the invention, the pre-dispersed processing is to disperse 1h using disperser；The milled processed is to adopt
It is ground 1~3 hour with technical grade grinder.
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 electricity with low-work voltage and farsighted infrared emittance
Hot oil ink.According to an embodiment of the invention, the gross mass based on the electric heating ink, according to mass percent meter, the electric heating
Ink includes: three-dimensional grapheme 5~20%；Two-dimensional graphene 1~10%；Carbon nanotube 1~5%；Conductive carbon black 5~20%；
Resin-bonded material 15~45%；Solvent 15~30%；Dispersing agent 1~10%；And auxiliary agent 0.5~5%.In the electric heating ink, two
Dimension graphene, carbon nanotube and conductive carbon black can be adsorbed on the surface of three-dimensional grapheme or be filled in three-dimensional grapheme
In pore structure, allows three-dimensional grapheme, two-dimensional graphene, carbon nanotube and conductive carbon black spatially to form collaboration and make
With, so that electric heating ink while meeting electric heating property standard, is suitble to work under 36V safe voltage below, and
Far infrared radiation rate height, safety and environmental protection, electric heating property is stable, not oxidizable, preparation method is simple, is easy to mass preparation.
Some specific embodiments according to the present invention, based on the gross mass of the electric heating ink, according to mass percent meter,
The concrete content of three-dimensional grapheme can for 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%,
16%, 17%, 18%, 19%, 20% etc.；The concrete content of two-dimensional graphene can for 1%, 2%, 3%, 4%, 5%,
6%, 7%, 8%, 9%, 10% etc.；The concrete content of carbon nanotube can be 1%, 2%, 3%, 4%, 5% etc.；It is conductive
The concrete content of carbon black can for 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%,
17%, 18%, 19%, 20% etc.；The concrete content of resinoid bond can for 15%, 18%, 20%, 22%, 25%,
26%, 28%, 30%, 33%, 35%, 37%, 39%, 40%, 42%, 43%, 44%, 45%, 48%, 50% etc.；It is molten
The concrete content of agent can be 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30% etc.；
The concrete content of dispersing agent can be 5%, 6%, 7%, 8%, 9%, 10% etc.；The concrete content of auxiliary agent can for 0.5%,
1%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, 5.0% etc..Inventor tests by many experiments
It is found after card, in above-mentioned content range, three-dimensional grapheme, two-dimensional graphene, carbon nanotube and conductive carbon black can be assisted sufficiently
Same-action, and then electric heating ink has preferable electric conductivity and hot stabilizability, while can be in the operating voltage for being lower than 36V
It is effectively worked, and can radiate under different operating voltage 5~17 microns of far ir ray, and spoke with higher
Penetrate rate；Resin-bonded material can make electric heating oil ink have film forming, levelability, adhesion property, corrosion resistance, high temperature resistant, no
The advantages that easy to aging, and solvent, dispersing agent and auxiliary agent etc. can further promote each component in electric heating ink to be uniformly dispersed, and have
Better service performance.If each component, not within above range, the filming performance of electric heating ink is poor, and due to resin
The constraint of binding material, which acts on, to be changed, and conductive filler can reunite, and then lead to the Electric radiant Heating Film power formed by the electric heating ink
Decaying is very fast, substantially reduces the service life of final products.
According to an embodiment of the invention, in order to enable three-dimensional grapheme, two-dimensional graphene, carbon nanotube and conductive carbon black can
With better performance synergistic effect, above-mentioned electric heating ink meets at least one of the following conditions: the carbon nanotube is led with described
The black mass ratio of electrical carbon be less than or equal to 1:6 (it is specific such as 1:6,1:6.5,1:7,1:7.5,1:8,1:8.5,1:9,1:9.5,1:
10 etc.)；It is 10% (specific to be less than or equal to the gross mass of the electric heating ink for the mass percentage of the two-dimensional graphene
Such as 10%, 9%, 8%, 7%, 6%, 5%, 4%, 3%, 2%, 1%)；The three-dimensional grapheme and the two-dimentional graphite
The mass ratio of alkene be greater than 2:1 (such as 2.1:1,2.5:1,2.8:1,3:1,3.2:1,3.5:1,3.8:1,4:1,4.2:1,4.5:1,
4.8:1,5:1 etc.).Specifically, electric heating ink can only meet said one condition, such as only meet carbon nanotube and conductive carbon
Black mass ratio is less than 1:6；Also it can satisfy above-mentioned two condition, such as meet the mass ratio of carbon nanotube and conductive carbon black simultaneously
Less than 1:6 and the mass percentage of two-dimensional graphene is less than or equal to the 10% of the gross mass of the electric heating ink；It can also be with
Meet above three condition simultaneously.As a result, by adjusting three-dimensional grapheme, two-dimensional graphene, carbon nanotube and conductive carbon black
Content and proportion can make four kinds of substances cooperate with optimal ratio, act synergistically so that electric heating ink have compared with
Low operating voltage, higher far infrared radiation rate and preferable hot stabilizability.Compared with above range, if above-mentioned match
Than too large or too small, electric heating ink performance may change, as electric heating ink mobility be deteriorated, rate of drying it is slack-off,
Electric heating ink internal resistance raising etc., if the film layer square resistance of electric heating ink formation is larger, voltage is lower than work temperature when 36V
Degree is relatively relatively low, and heating and heating effect opposite can be deteriorated.
According to an embodiment of the invention, term " three-dimensional grapheme " used herein is selected from high-specific surface area, high conductance
Rate product type, specifically, the specific surface area of the three-dimensional grapheme can be greater than 2000m2/ g is (specific such as 2001m2/g、
2050m2/g、2100m2/g、2150m2/g、2200m2/ g etc.), the number of plies is (specific such as 14 layers, 13 layers, 12 layers, 11 less than 15 layers
Layer, 10 layers etc.), there is porous structure, in some specific embodiments, the aperture of porous structure can be (specific for 10~100nm
Such as 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm), porosity of=30% is (specifically such as
30%, 35%, 40%, 45%, 50%, 55%, 60% etc.).In the porosity ranges, three-dimensional grapheme can will be two-dimentional
Graphene, carbon nanotube and conductive carbon black etc. are adsorbed in surface and porous structure, so effectively spatially play collaboration,
With effect, so that the service performance of electric heating ink is more preferably.If the aperture of three-dimensional grapheme is too small, the two-dimensional graphene of large stretch of diameter without
It is porous interior that method is interspersed in three-dimensional grapheme, while the amount of being adsorbed of carbon pipe or carbon black is lower, is formed by Structure Network relatively
Fragility, stability are poor；If the aperture of three-dimensional grapheme is excessive, a large amount of conducting filler enters in three-dimensional grapheme hole, is
Guarantee that normal conductive mesh is established, need to add a greater amount of conductive materials, although conductive mesh overlapped overall stability is
It improves, but considerably increases filler material cost.
Some specific embodiments according to the present invention, the three-dimensional grapheme are globular graphite alkene.Specifically, the graphene
It is to be prepared by raw material of coal, belongs to coal base graphene, there is high-specific surface area, grading-hole, be a large-sized micron ball,
And surface has more random hole.Suitable for supercapacitor, electrocondution slurry, Electric radiant Heating Film, composite material and environmental-protection adsorption etc.
Field.In the present invention, porous three-dimensional grapheme sphere provides " fixing lock " effect for carbon nanotube and conductive carbon black overlap joint,
Specifically, carbon nanotube belongs to one-dimensional linear material, two-dimensional graphene is sheet layer material, three-dimensional grapheme be have it is porous micro-
Rice ball all not can avoid and fill closely knit in entire conductive network, Nano grade is led at this time when three intersects combinations in any case
The black introducing of electrical carbon, can be sufficient filling with small gap in conductive mesh, keep its overlap joint more perfect.
According to an embodiment of the invention, the two-dimensional graphene can be micro- selected from highly conductive, great Pian Jing, low ash degree graphene
Sheet type, is specifically as follows the graphene with layer structure that this field is routinely thought, the number of plies is (specific such as 9 less than 10 layers
Layer, 8 layers, 7 layers, 6 layers, 5 layers, 4 layers etc.), piece diameter be 10~20 μm (it is specific as 10 microns, 11 microns, 12 microns, 13 microns,
14 microns, 15 microns, 16 microns, 17 microns, 18 microns, 19 microns, 20 microns etc.), gray scale is≤0.1% (specifically such as
0.1%, 0.09%, 0.08%, 0.07%, 0.06%, 0.05%, 0.04%, 0.03%, 0.02% etc.).As a result, piece diameter compared with
Big two-dimensional graphene overlapping rate is higher, the graphene conductivity with higher of few layer, low ash degree, it is ensured that electric heating ink
The film layer sheet resistance of formation is suitable.
According to an embodiment of the invention, the preparation method of above-mentioned three-dimensional grapheme is not particularly limited, as long as can obtain
The three-dimensional grapheme met the requirements.In some embodiments, the three-dimensional grapheme can be prepared by following steps:
By feed coal (fixed carbon content can be 30%~80%, such as lignite, bituminous coal, anthracite), in microwave reaction furnace, (frequency can
Think 915MHz~2450MHz) in carry out pyrolysis processing, the temperature of pyrolysis processing can be 500~900 DEG C, and the time can be
0.1~3 hour, to obtain pyrolysis char；By the pyrolysis char and activator (including but not limited to KOH, KCl, K2CO3、
MgO、MgCl2、NaOH、NaCl、Na2CO3、ZnCl2、NaOH、FeCl3With Fe (NO3)3At least one of) mix (at kneading
Reason, kneading temperature can be 100~300 DEG C, and the time can be 1~10 hour), the mass ratio of pyrolysis char and activator can be with
For 1:0.1~1:5, to obtain mixed material；The mixed material is carried out in the microwave reaction furnace, under inert atmosphere
It is activated (temperature of activation processing can be 700~1200 DEG C, and the time can be 0.1~3 hour), to obtain described three
Tie up graphene.As a result, by the pyrolysis processing in micro-wave oven, the volatile matter in feed coal can be removed, as hydrogen, methane,
Carbon monoxide, carbon dioxide and tar etc.；Semicoke micropore increases in pyrolytic process, is conducive to filling for pyrolysis char and activator
Divide mixing；It is shunk while pyrolysis char weightlessness in pyrolytic process, forms crackle, be conducive to pyrolysis char and activator
Be sufficiently mixed；Compared to common method for pyrolysis, be pyrolyzed in microwave reaction furnace, may make feed coal it is heated more evenly,
Pyrolysis is more abundant, and improves pyrolytic reaction rate；In addition, microwave acts directly on pyrolysis char in activation process, by heat
The interior friction of solution semicoke is heated, and is put into the container for absorbing microwave material compared to by pyrolysis char, microwave action is holding
Container is heated on device, the method for indirect heating pyrolysis char is then conducted by heat, the present invention is using microwave reaction furnace
Heating means are more efficient, and heat utilization ratio is higher；Moreover, obtained three-dimensional grapheme have hole prosperity, large specific surface area,
The advantages that pore-size distribution is controllable；In addition, the pollution of above-mentioned preparation method is small, low energy consumption, technique when length, easy to control, preparation cost
It is low, it is easy to industrialized production.
According to an embodiment of the invention, the method for preparing three-dimensional grapheme can also include: to the product of activation processing into
At least one of following processing step of row: de- ambiguity carbon processing；Pickling processes；High temperature purification treatment.It is obtained as a result, to above-mentioned
To three-dimensional grapheme purified, obtain the three-dimensional grapheme of high-purity, it is specific: three-dimensional can be removed by pickling processes
Most of metal impurities in graphene, by high temperature purification treatment be removal remain in more difficult removal in graphene metal it is miscellaneous
Matter is the miscellaneous carbon removed in graphene by taking off the processing of ambiguity carbon.In addition, those skilled in the art can also be according to different
Post-processing step prepares the different three-dimensional grapheme of purity.
According to an embodiment of the invention, the carbon nanotube may include wound form carbon nanotube and aligned carbon-nanotubes
At least one of.The arrangement of wound form pipe is mixed and disorderly as a result, and mistake is vertical to intersect, and compared to single branch pipe, networking is preferable, is more advantageous to
Intersect networking with other components in electric heating ink.And array carbon pipe, regularly arranged, similar beard, it increases and electric heating oil
The contact surface area of other components in ink, therefore when reaching the sheet resistance value of a certain determination, array carbon pipe and other materials have compared with
Good contact, keeps carbon pipe additive amount less, advantageously reduces cost, while reducing feed time, improves production efficiency.
According to an embodiment of the invention, the resistivity of the conductive carbon black can be (specific such as 9.9 Ω less than 10 Ω m
m、9.5Ω·m、9Ω·m、8.8Ω·m、8.5Ω·m、8.2Ω·m、8.0Ω·m、7.8Ω·m、7.5Ω·m、7.2
Ω m, 7.0 Ω m, 6.8 Ω m, 6.5 Ω m, 6.3 Ω m, 5.0 Ω m, 5.5 Ω m, 4.0 Ω m etc.),；Such as
The including but not limited to XE-2B of Degussa company, the Germany and BP2000 etc. of Cabot company, the U.S..There is good lead as a result,
Electrically, enable to electric heating ink that there is ideal electric heating property, while after can intersecting with filled graphite alkene with carbon nanotube
Existing white space increases the combination between conducting filler, reduces the internal resistance of electric heating ink, and carbon black has preferable profit
Slip can greatly improve the levelability and film forming of electric heating ink.
According to an embodiment of the invention, resin-bonded material can be in order to enable electric heating ink has better service performance
The resin of resin and high glass-transition temperature including lower glass transition temperatures, the resin of lower glass transition temperatures are main
Have the characteristics that film forming, levelability, adhesion property are good, the printable adaptive of adjustable ink, in order to preferably realize
Pattern transfer；And the resin of high glass-transition temperature can have feature corrosion-resistant, resistant to high temperature, stablize electric heating ink can
It is not susceptible to aging for hot environment, and two kinds of resins are used cooperatively, and can improve the synthesis weatherability of electric heating ink.Root
According to some specific embodiments of the present invention, the resin-bonded material includes: the first resin, and first resin includes modified poly ester
At least one of resin, acrylic resin and polyurethane；Second resin, second resin include epoxy resin, silicone resin
At least one of with fluororesin.According to an embodiment of the invention, the gross mass based on the electric heating ink, according to quality percentage
Than meter, the electric heating ink include first resin 10~30% (it is specific such as 10%, 12%, 15%, 16%, 17%,
18%, 20%, 22%, 25%, 26%, 28%, 30% etc.) and second resin 5~15% (it is specific such as 5%, 6%,
7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15% etc.) have the first of lower glass transition temperatures as a result,
Second resin of resin and glass transition temperature with higher can cooperate effect, so that electric heating ink is comprehensive
It can be preferably.
According to an embodiment of the invention, the solvent is selected from butanediol, n-butanol, butyl glycol ether, Glycolic acid n butyl ester
At least one of with diethylene glycol ether acetate.Thus, it is possible to disperse and dissolve various groups in electric heating ink well
Point, so that each component is uniformly dispersed and is stablized, conducive to the service performance for improving electric heating ink, and material source is extensive, is easy to get, cost
It is lower.
According to an embodiment of the invention, the dispersing agent is in polypyrrole, polyethylene glycol and sodium carboxymethylcellulose
It is at least one.Thus, it is possible to effectively facilitate the dispersion of each component in electric heating ink, it is set to be uniformly dispersed, stablize, and material source
Extensively, cheap, it is easy to accomplish industrialized production.
According to an embodiment of the invention, the auxiliary agent includes defoaming agent, levelling agent, adhesive force auxiliary agent, thickener, wetting
At least one of agent, coupling agent and promotion film forming agent.It is appreciated that specific auxiliary agent type those skilled in the art can root
It suitably selects according to actual operation requirements, no longer excessively repeats herein.
According to an embodiment of the invention, above-mentioned electric heating ink meets at least one of the following conditions: operating voltage be less than or
Equal to 36V (specific such as 36V, 35V, 30V, 25V, 20V, 15V, 10V, 5V)；It is (specific as 5 is micro- suitable for 5~17 microns of release
Rice, 6 microns, 7 microns, 8 microns, 9 microns, 10 microns, 11 microns, 12 microns, 13 microns, 14 microns, 15 microns, 16 microns,
17 microns etc.) ray of wavelength；The normal direction radiance of the ray be greater than or equal to 85% (it is specific such as 85%, 86%, 87%,
88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99% etc.)；Accelerated ageing test
Power attenuation be less than or equal to 1% (specific such as 1%, 0.8%, 0.5%, 0.2%, 0.1%).It is appreciated that this hair
Bright electric heating ink can only meet said one condition, only meet above-mentioned two condition, only meet above three condition or
Meet four conditions of above-mentioned whole.Some specific embodiments according to the present invention, by verification experimental verification, electric heating ink of the invention
It can work under 36V safe voltage below, and can be with Net long wave radiation similar to solar radiation under different operating voltage
The far ir ray that the wavelength of intensity is 5~17 microns, makes human body cell RESONANCE ABSORPTION, promotes health, play certain
Physiotherapy effect, and radiated wavelength range substantially constant, radiance increase, the normal direction under different voltages as voltage increases
Radiance is not less than 85% substantially, while having preferable anti-aging property, and the power attenuation of accelerated ageing test is less than or waits
In 1%.
According to an embodiment of the invention, electric heating ink is usually to coat to form coating on substrate when in use, coating is given
Heat effect is played in energization, by test show electric heating ink of the invention be suitble to PET (polyethylene terephthalate),
The substrates such as PI (polyimides), PVC (polyvinyl chloride), glass, metal, paper are especially suitable for the plastic basis materials tables such as epoxy resin board
Face, adhesive force is good, and service performance is preferable.
In another aspect of this invention, the present invention provides a kind of methods prepared in mentioned-above electric heating ink.Root
According to the embodiment of the present invention, this method comprises: three-dimensional grapheme, two-dimensional graphene, carbon nanotube, conductive carbon black, resin are glued
A part, solvent and dispersant in ramming material, and pre-dispersed processing is carried out to obtained mixture, it obtains pre-dispersed
Material；By in the pre-dispersed material, the resin-bonded material another part and the auxiliary agent mix, and to obtained mixture
It is ground, obtains the electric heating ink.Specifically, first will be in powdery and the biggish three-dimensional graphite of density ratio in this method
Alkene, two-dimensional graphene, carbon nanotube and conductive carbon black are pre-dispersed, can make it is opposite be not easy to disperse, feed relatively slowly, jitter time
Long ingredient preferably disperses, then high speed grinding again, each component can be made to be uniformly dispersed, conducive to the film forming for improving electric heating ink
Property etc. service performances, and the step of preparation process of this method " one pot go out " is simple, easy to operate, easy, to equipment and technology people
Harsh requirement, preparation cost be not low by member, it is easy to accomplish industrialized production, good economy performance, and obtained electric heating ink has
Lower operating voltage, higher far infrared radiation rate and preferable hot stabilizability.
According to an embodiment of the invention, can be by three-dimensional grapheme, two-dimensional graphene, carbon nanotube, conductive carbon black, resin
A part, solvent and dispersing agent addition disperser progress in binding material is pre-dispersed, and mixing speed can be 1000~1500rpm
(specific such as 1000rpm, 1100rpm, 1200rpm, 1300rpm, 1400rpm, 1500rpm), being dispersed with stirring device power can
Think 800W, be dispersed with stirring in charging, the specific pre-dispersed time is determined by dispersed paste volume, some specific embodiments
In, can continue after adding material low speed disperse 0.5~1 hour (it is specific as 0.5 hour, 0.6 hour, 0.7 hour, it is 0.8 small
When, 0.9 hour, 1.0 hours etc.).The preparation process can block to avoid sand mill feed and exhaust tube, and material dispersion is uniform, has
Conducive to the uniformity for improving obtained electric heating ink filming performance.
According to an embodiment of the invention, resin-bonded material can in electric heating ink-making process in order to obtain better effect
To be added step by step, a part of resin-bonded material can specifically be added in pre-dispersed step, be added in milled processed step another
A part of resin-bonded material.Specifically, in some embodiments, a part of in resin-bonded material can be to fit in the follow-up process
A part of monomer or raw material of resin are generated in polymerization, another part in resin-bonded material can be for suitable for polymerization generation resin
Another part monomer or raw material (such as curing agent), the above-mentioned resin-bonded material of two parts polymerize spanning tree in subsequent process
Rouge；In other embodiments, a part of of resin-bonded material can be a part of resin material, another part of resin-bonded material
For other resin materials, for example, a part of in the resin-bonded material can be to be above-mentioned with lower glass transition temperatures
First resin, another part in the resin-bonded material can be the second resin with high glass-transition temperature.As a result,
Can be larger to avoid resin viscosity, influence the powder filled material such as three-dimensional grapheme, two-dimensional graphene, carbon nanotube and conductive carbon black
The problems such as dispersion, easily blocking sand mill input and output material pipeline and cavity, and the rear resin that is added is the resin system for adding curing agent,
The technique that substep is added effectively prevents curing agent and directly contacts with conductive fill powder, avoids curing agent from being adsorbed by powder and coats
What is generated is unevenly distributed phenomenon.According to an embodiment of the invention, three-dimensional grapheme involved in this method, two-dimensional graphene,
Carbon nanotube, conductive carbon black, resin-bonded material, solvent, dispersing agent and auxiliary agent can be consistent with the previously described, herein no longer
It repeats one by one.
According to an embodiment of the invention, the milled processed can grind 1~3 hour (specifically using technical grade grinder
Such as 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours), specific power is determined by sand mill different size, some tools
In body embodiment, preparation condition can be small-sized 1L sand mill, power 2KW, revolving speed be 1000~1500rpm (specifically such as
1000rpm, 1100rpm, 1200rpm, 1300rpm, 1400rpm, 1500rpm etc.)；It can also be 5L sand mill, power is
5KW, revolving speed are 1000~1500rpm (specific such as 1000rpm, 1100rpm, 1200rpm, 1300rpm, 1400rpm, 1500rpm
Etc.) etc..It is easy to operate as a result, there is no rigors to technical staff and equipment, and step is less, easy to accomplish, processing week
Phase is obviously shortened, and efficiency significantly improves, it is easy to accomplish industrialized production.
According to an embodiment of the invention, specific milled processed condition can be selected according to desired fineness.It is some
In specific embodiment, the fineness of the particulate matter in electric heating ink can be ground to 10~20 microns (it is specific as 10 microns, it is 11 micro-
Rice, 12 microns, 13 microns, 14 microns, 15 microns, 16 microns, 17 microns, 18 microns, 19 microns, 20 microns etc.) stop grinding afterwards
Mill processing.The fineness can satisfy the print request of later period electric heating ink as a result, such as select 150~200 mesh silk-screen printings
Version, 10~20 μm of fineness can guarantee that slurry through halftone, realizes normal printing film forming.Conversely, if particle is excessively thick, Wu Fazheng
Silk-screen plate is often penetrated, printing trouble is generated.Wherein, it should be noted that the particulate matter in electric heating ink described herein refers to
Any ingredient for being in granular form state in electric heating ink, such as including but not limited to three-dimensional graphite, two-dimensional graphene, carbon nanotube,
Conductive carbon black etc..
According to an embodiment of the invention, after the milled processed, further includes: the product obtained to the milled processed
The step of carrying out viscosity-adjusting agent.Specifically, thickener can be added according in the product that target viscosities phase grinding is handled, have
The thickener of body can be the thickener that this field routinely uses, and be required with no restriction this.As a result, be suitable for it is a variety of printing or
Person's coating processes, it is applied widely.
The embodiment of the present invention is described below in detail.In the case where specified otherwise, the ratio in following embodiment is
Mass ratio, the content of each component are mass percentage.
Embodiment 1:
The first resin for accounting for raw material gross mass 25% is deployed first, and ingredient is polyester resin: acrylic resin: solvent
=1:2:7 is dissolved in the solvent for accounting for raw material gross mass 30%, and solvent is dimethyl succinate: dimethyl glutarate: adipic acid
Dimethyl ester=1:1:1；Secondly by the electric heating filler of raw material gross mass 30%, ingredient is three-dimensional grapheme: two-dimensional graphene:
Carbon nanotube: carbon black=3:1:1:6 is slowly scattered in the first resin, stirs at low speed dispersion 1h up to pre-dispersed material；It again will be upper
State that pre-dispersed material, the second resin for accounting for raw material gross mass 10%, the dispersing agent for accounting for raw material gross mass 2%, to account for raw material total
Technical grade grinder is added in the auxiliary agent of quality 3%, wherein the second resin is mainly epoxy resin: silicone resin: fluororesin=1:1:1
Mass ratio, auxiliary agent are mainly the wetting agent for accounting for raw material gross mass 1%, the levelling agent for accounting for raw material gross mass 1%, account for raw material
The defoaming agent of gross mass 1%；It, can after the slurry obtained after above-mentioned substance is sufficiently mixed grinds 1~3h to 10~20 μm of fineness
It is required to be suitably added thickener according to practical viscosity, adjusts ink appropriate viscosity, it is soft in PET, PI or epoxy resin glass-fiber-fabric etc.
Property substrate on be coated with 20~25 μ m thick film layers.It is surveyed according to graphene alliance standard T/CGIA030-2017, GB/T7287-2008
It is as follows to try film layer electric heating property: when voltage is 36V, film layer power density is 2100W/m2, discharge far infrared wave-length coverage
It is 8~13 μm, adhesive force 5B, hardness 6H, normal direction electric radiation rate 85%, 95 DEG C of naked film temperature.
Embodiment 2:
The first resin for accounting for raw material gross mass 25% is deployed first, and ingredient is polyester resin: acrylic resin: solvent
=1:2:7 is dissolved in the solvent for accounting for raw material gross mass 15%, and solvent is dimethyl succinate: dimethyl glutarate: adipic acid
Dimethyl ester=1:1:1；Secondly the electric heating filler of raw material gross mass 40% will be accounted for, ingredient is three-dimensional grapheme: two-dimentional graphite
Alkene: carbon nanotube: carbon black=3:1:0.5:4.5 is slowly scattered in the first resin, and stirring at low speed dispersion 1h is pre-dispersed material；
Again by above-mentioned pre-dispersed material, account for the second resin of raw material gross mass 15%, the dispersing agent for accounting for raw material gross mass 2%, Zhan Yuan
Technical grade grinder is added in the auxiliary agent of material gross mass 3%, wherein the second resin is mainly epoxy resin: silicone resin: fluororesin
=1:1:1, auxiliary agent mainly account for the wetting agent of raw material gross mass 1%, the levelling agent for accounting for raw material gross mass 1%, Zhan Yuancai
Expect the defoaming agent of gross mass 1%；It, can be according to reality after grinding 1~3h to 10~20 μm of fineness after above-mentioned slurry is sufficiently mixed
Viscosity requirement is suitably added thickener, adjusts ink viscosity, is coated on the flexible parent metals such as PET, PI or epoxy resin glass-fiber-fabric
20~25 μ m thick film layers test film layer electric heating property.According to graphene alliance standard T/CGIA030-2017, GB/T7287-
2008, test film layer electric heating property is as follows: when voltage is 36V, film layer power density is 1900W/m2, discharge far infrared model
Enclosing is 7~14 μm, adhesive force 5B, hardness 5H, electric radiation rate 78%, 85 DEG C of naked film temperature.
Comparative example 1:
The first resin for accounting for raw material gross mass 25% is deployed first, and ingredient is polyester resin: acrylic resin: solvent
=1:2:7 is dissolved in the solvent for accounting for raw material gross mass 30%, and solvent is dimethyl succinate: dimethyl glutarate: adipic acid
Dimethyl ester=1:1:1；Secondly 30% electric heating filler of raw material gross mass will be accounted for, ingredient is three-dimensional grapheme: two-dimentional graphite
Alkene: carbon nanotube=2:1.5:1 is slowly scattered in the first resin, and stirring at low speed dispersion 1h is pre-dispersed material；It again will be above-mentioned
Pre-dispersed material, 2% dispersing agent for accounting for raw material gross mass, accounts for the total matter of raw material at the 10% the second resins for accounting for raw material gross mass
Technical grade grinder is added in 3% auxiliary agent of amount, wherein the second resin is mainly epoxy resin: silicone resin: fluororesin=1:1:1,
Auxiliary agent is mainly 1% wetting agent for accounting for raw material gross mass, 1% levelling agent for accounting for raw material gross mass, accounts for raw material gross mass
1% defoaming agent；After grinding 1~3h to 10~20 μm of fineness after above-mentioned slurry is sufficiently mixed, it can be required according to practical viscosity
It is suitably added thickener, adjusts ink viscosity, 20~25 μm are coated on the flexible parent metals such as PET, PI or epoxy resin glass-fiber-fabric
Thickness film layer tests film layer electric heating property.It is tested according to graphene alliance standard T/CGIA030-2017, GB/T7287-2008
Film layer electric heating property is as follows: when voltage is 36V, film layer power density is 1150W/m2, release far infrared range is 8~14
μm, adhesive force 4B, hardness 4H, electric radiation rate 72%, 56 DEG C of naked film temperature.
Comparative example 2:
The first resin for accounting for raw material gross mass 35% is deployed first, and ingredient is polyester resin: acrylic resin: solvent
=1:2:7 is dissolved in the solvent for accounting for raw material gross mass 20%, and solvent is dimethyl succinate: dimethyl glutarate: adipic acid
Dimethyl ester=1:1:1；Secondly 20% electric heating filler of raw material gross mass will be accounted for, ingredient is two-dimensional graphene: carbon nanotube:
Conductive carbon black=2:3:4 is slowly scattered in the first resin, and stirring at low speed dispersion 1h is pre-dispersed material；It again will be above-mentioned pre-dispersed
The 20% the second resins for expecting, accounting for raw material gross mass, account for the 3% of raw material gross mass at 2% dispersing agent for accounting for raw material gross mass
Technical grade grinder is added in auxiliary agent, wherein the second resin is mainly epoxy resin: silicone resin: fluororesin=1:1:1, auxiliary agent are main
It is 1% wetting agent for accounting for raw material gross mass, 1% levelling agent for accounting for raw material gross mass, 1% defoaming for accounting for raw material gross mass
Agent；After grinding 1~3h to 10~20 μm of fineness after above-mentioned slurry is sufficiently mixed, it can be required to be suitably added increasing according to practical viscosity
Thick dose, ink viscosity is adjusted, 20~25 μ m thick film layers are coated on the flexible parent metals such as PET, PI or epoxy resin glass-fiber-fabric, is surveyed
Try film layer electric heating property.Film layer electric heating property is tested according to graphene alliance standard T/CGIA030-2017, GB/T7287-2008
As follows: when voltage is 36V, film layer power density is 500W/m2, release far infrared range is 8~13 μm, and adhesive force is
4B, hardness 3H, electric radiation rate 65%, 30 DEG C of naked film temperature.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
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 with low-work voltage and farsighted infrared emittance, which is characterized in that be based on the electric heating oil
The gross mass of ink, according to mass percent meter, the electric heating ink includes:
Three-dimensional grapheme 5~20%；
Two-dimensional graphene 1~10%；
Carbon nanotube 1~5%；
Conductive carbon black 5~20%；
Resin-bonded material 15~45%；
Solvent 15~30%；
Dispersing agent 1~10%；And
Auxiliary agent 0.5~5%.
2. electric heating ink according to claim 1, which is characterized in that meet at least one of the following conditions:
The mass ratio of the carbon nanotube and the conductive carbon black is less than or equal to 1:6；
The three-dimensional grapheme and the mass ratio of the two-dimensional graphene are greater than 2:1.
3. electric heating ink according to claim 1, which is characterized in that the specific surface area of the three-dimensional grapheme is greater than
2000m2/ g, the number of plies are less than 15 layers, have porous structure；
Optionally, the three-dimensional grapheme is globular graphite alkene；
Optionally, the partial size of the globular graphite alkene is micron order；
The two-dimensional graphene has layer structure, and the number of plies is less than 10 layers, and piece diameter is 10~20 μm, gray scale≤0.1%；
The carbon nanotube includes at least one of wound form carbon nanotube and aligned carbon-nanotubes；
The resistivity of the conductive carbon black is less than 10 Ω m.
4. electric heating ink according to claim 1, which is characterized in that the resin-bonded material includes:
First resin, first resin include at least one of modified polyester resin, acrylic resin and polyurethane；
Second resin, second resin include at least one of epoxy resin, silicone resin and fluororesin；
Optionally, the gross mass based on the electric heating ink, according to mass percent meter, the electric heating ink includes described first
Resin 10~30% and second resin 5~15%.
5. electric heating ink according to claim 1, which is characterized in that the solvent is selected from butanediol, n-butanol, ethylene glycol
At least one of butyl ether, Glycolic acid n butyl ester and diethylene glycol ether acetate；
The dispersing agent is selected from least one of polypyrrole, polyethylene glycol and sodium carboxymethylcellulose；
The auxiliary agent includes defoaming agent, levelling agent, adhesive force auxiliary agent, thickener, wetting agent, coupling agent and promotes in film forming agent
It is at least one.
6. electric heating ink according to any one of claims 1-5, which is characterized in that meet the following conditions at least it
One:
Operating voltage is less than or equal to 36V；
Suitable for discharging the ray of 5~17 micron wave lengths；
Optionally, the normal direction radiance of the ray is less than or equal to 85%；
The power attenuation of accelerated ageing test is less than or equal to 1%；
Power density can reach 2300W/m2。
7. a kind of method prepared in electric heating ink of any of claims 1-6 characterized by comprising
By a part, solvent and the dispersion in three-dimensional grapheme, two-dimensional graphene, carbon nanotube, conductive carbon black, resin-bonded material
Agent mixing, and pre-dispersed processing is carried out to obtained mixture, obtain pre-dispersed material；
By in the pre-dispersed material, the resin-bonded material another part and the auxiliary agent mix, and to obtained mixing
Object is ground, and obtains the electric heating ink.
8. the method according to the description of claim 7 is characterized in that after the milled processed, further includes: to the grinding
Handle the step of obtained product carries out viscosity-adjusting agent.
9. the method according to the description of claim 7 is characterized in that meeting at least one of the following conditions:
A part in the resin-bonded material is the first resin, and another part in the resin-bonded material is the second resin；
The fineness of particulate matter in the electric heating ink is 10~20 microns.
10. the method according to the description of claim 7 is characterized in that it is described it is pre-dispersed processing be using disperser dispersion 0.5~
1 hour；
The milled processed is ground 1~3 hour using technical grade grinder.
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