CN103275552A - Carbon electric heating printing ink and preparation method thereof - Google Patents
Carbon electric heating printing ink and preparation method thereof Download PDFInfo
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- CN103275552A CN103275552A CN 201310187239 CN201310187239A CN103275552A CN 103275552 A CN103275552 A CN 103275552A CN 201310187239 CN201310187239 CN 201310187239 CN 201310187239 A CN201310187239 A CN 201310187239A CN 103275552 A CN103275552 A CN 103275552A
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Abstract
The invention provides carbon electric heating printing ink and a preparation method thereof. The carbon electric heating printing ink comprises the components in percentage by mass: 0-2% of carbon nano tube, 4-12% of superconducting carbon black, 15-30% of conducting graphite, 10-25% of resin, 40-60% of solvent and 0.2-6% of assistant. The preparation method comprises the following steps of: crushing particle polyester resin in resin till the average grain diameter is below 0.5mm; then, uniformly mixing the resin with the carbon nano tube, the superconducting carbon black, the conducting graphite, the solvent, the assistant and other components in the resin; grinding the mixture till fineness is less than 50 mu m through a three-roll grinder; then, grinding till fineness is less than 20 mu m through the grinder; and filtering. The viscosity range of the carbon electric heating printing ink is 40-100Pa.S. The carbon electric heating printing ink provided by the invention has lower solid content, is good in adaptability to the printing process, and can be printed on base materials such as paper, plastic and woods to form electric heating coatings.
Description
Technical field
The present invention relates to a kind of carbon for low-temp radiating electrothermal membrane is electric heating printing ink and preparation method thereof, belongs to the thermo electric material technology.
Background technology
Low-temp radiating electrothermal membrane substitutes hot-water heating and is used for heating residential, has water saving, saves land, economizes material and is convenient to advantages such as adjusting, metering.Common low-temp radiating electrothermal membrane is to be that electric heating ink printing, metal electrode bar are made between insulation polyester film through processing, hot pressing by carbon on the market.The carbon that forms electro-thermal coatings is that electric heating printing ink is the key problem in technology of this series products.
Chinese patent CN01124036.9 has announced that a kind of carbon that adds silver powder is electric heating printing ink, Chinese patent CN200510202542.9 has announced that a kind of receiving-microstage graphite and graphitized carbon black are the electric-heating coatings of electro-conductive material, Chinese patent CN201010219932.7 has announced the water-based electric heating coating that a kind of carbon is, Chinese patent CN201210160997.8 has announced a kind of carbon series electric heating coating that adds the infrared emission material.(electric thermal power about 200 is to 300W/m in order to satisfy the electrical property design requirements for the electric heating printing ink that above-mentioned patent is announced or coating and present commercially available electric heating printing ink
2), all need to add the carbon series conductive material of massfraction about 50%; In order to guarantee enough stripping strengths, must add a certain amount of resin in the electrically conductive ink and make tackiness agent.The solid content of these electric heating printing ink is bigger, and viscosity is higher, and it is narrow that typography adapts to window.Stripping strength is not ideal enough so the low-temp radiating electrothermal membrane of existing electric heating printing ink preparation exists, printing quality is difficult to control, product electric thermal power density problem such as even inadequately.
Carbon nanotube has excellent mechanics and electric property, and content even carbon nanotube seldom is dispersed in the matrix and will forms conductive network.The superconduction carbon black is bigger than the specific surface area of common graphitized carbon black, and forms the side chain network structure easily, and addition just can form conductive network in less in collective's material.The superconduction carbon black has been applied to conduction and Antistatic Paint, plastics, rubber, battery material, cable shield material etc.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of carbon is electric heating printing ink and preparation method thereof, this printing ink electro-conductive material adopts the combination of carbon nanotube, superconduction carbon black and electrically conductive graphite, have than low-solid content when satisfying the electric heating property demand, printing or coating processes adaptability are improved, are particularly useful for the higher gravure printing technique of production efficiency.
For achieving the above object, the invention provides a kind of carbon is electric heating printing ink, its mass percent consists of: carbon nanotube 0～2%, superconduction carbon black 2～12%, electrically conductive graphite 5～35%, resin 10-30%, solvent 30～70% and auxiliary agent 0.2～8%, described carbon are that the range of viscosities of electric heating printing ink is at 10Pa.S～200Pa.S.
As preferred version, wherein said carbon nanotube is lower than 0.2 to the ratio of superconduction carbon black.Particularly, the mass percent of carbon nanotube is 0～2%; Preferably, be 0.5～1.5%.Carbon nanotube can be divided into armchair shape nanotube according to constitutional features, zig-zag nanotube and chiral nanotubes, and their conductivity difference is very big; Can be divided into according to whether containing wall defects: improve carbon nanotube (single wall) and contain defective carbon nanotube (many walls), the Single Walled Carbon Nanotube electroconductibility that diameter is little is better; Homogeneity and configuration according to profile can be divided into: straight pipe type, carbon nano-tube bundle, Y type etc., the straight pipe type carbon nano-tube conductive can be better.Consider Costco Wholesale, what select for use in the technical scheme of the present invention is the multi-walled carbon nano-tubes of resistivity 0.2 Ω m, and without any pre-treatment, like product obtains from market easily before using.Obviously, if resistivity less than or near the said products, technical scheme of the present invention can adopt the carbon nanotube of other any kinds, also comprise the carbon nanotube of purifying through pre-treatment or improving dispersing property.
As preferred version, wherein said superconduction carbon black to the ratio of electrically conductive graphite is: 0.1～0.5.The mass percent of superconduction carbon black is 2～12%, preferably, is 4～8%; Select resistivity to be lower than the product of 1.5 Ω m, for example: Dutch AKZO(Aksu. Nobel) the Ketjen black Ketjenblack EC300J, 600JD type of company, the Printex XE-2B of German Degussa company and the BP2000(Black Pearls 2000 of U.S. Cabot company) etc.Electrically conductive graphite is commercially available crystalline flake graphite, and mass percent is 5～30%, preferably, and inaction 10～25%.
As preferred version, wherein said resin comprises particulate state vibrin, water-borne acrylic resin emulsion and aqueous polyurethane resin emulsion, and the mass percent of their solids is 1:0.5～2:0.5～2.Vibrin can be Degussa Dynapol L series 205,206,208,411 in a kind of, preferably, be Dynapol L205; Water-borne acrylic resin can be the lucky Lik-Sang in Zhuhai Jelee WA series emulsion of producing 2007/2008, among the 2007A/2008A and 2017/2018 one, preferably, be Jelee WA 2007A/2008A; Aqueous polyurethane can be the lucky Lik-Sang in Zhuhai Jelee AC series emulsion of producing 830, among 830JW, 831,0304B and the 0304JW one, preferably, be Jelee AC 830JW.
As preferred version, wherein said solvent is the combination of the monohydroxy-alcohol of water and two or three carbon atoms, and water is 0.3～1.2 to the mass ratio of alcohol; Preferably, be water and ethanol mixed solvent.As required, also can add mass percent in the solvent and be lower than 5% ethyl acetate or acetone, as solvent evaporates promotor.
As preferred version, wherein said auxiliary agent comprises: dispersion agent and levelling defoamer, dispersion agent is 0.25～0.50 to the mass percent of levelling defoamer.
As preferred version, wherein said dispersion agent can be Sodium dodecylbenzene sulfonate (SDBS) or polyoxyethylene octyl phenyl ether (Triton X-100).
As preferred version, wherein said levelling defoamer is polyether-modified polysiloxane-based, can be BYK345, BYK348 and BYK349 that German Bi Ke produces, is preferably BYK345.
The present invention also provides the preparation method of above-mentioned carbon nano electroheating printing ink, particulate state vibrin in the resin is crushed to below the median size 0.5mm, then with carbon nanotube, superconduction carbon black, electrically conductive graphite, solvent, auxiliary agent and resin in all the other components mix and be ground to fineness by three-roll grinder and be lower than 50 microns, be ground to fineness with sand mill again and be lower than 20 microns, filtering and namely obtaining carbon is electric heating printing ink.
As preferred version, also add total mass after wherein filtering and be lower than 5% ethyl acetate or acetone.
Carbon nano electroheating printing ink of the present invention has adopted the ink adhesive system of optimizing (solvent, resin and auxiliary agent etc.); In this binder system, the carbon nanotube that electroconductibility is strong and the easy superconduction carbon black that forms side chain network conduction network can be uniformly dispersed; So carbon nano electroheating printing ink provided by the invention has the following advantages: have than low-solid content when (a) satisfying the electric heating property demand, printing or coating processes adaptability are improved, be particularly useful for the higher gravure printing technique of production efficiency; (b) can be printed on formation electric-heating coatings layer on the body materials such as paper, plastics, timber.
Embodiment
Be noted that following specifying all is example, be intended to further specify the invention provides that except as otherwise noted, all Science and Technology terms used herein have the identical meanings with the technical field of the invention personnel common sense.
Hereinafter, will describe in detail embodiment of the present invention.
As previously mentioned, a distinguishing feature of carbon nano electroheating printing ink provided by the invention is that solid content is lower, and particularly, resin and carbon series conductive material (carbon nanotube, superconduction carbon black, electrically conductive graphite) total mass per-cent are lower than 55% in the control prescription.
Carbon nanotube is the multi-walled carbon nano-tubes that resistivity is lower than 0.2 Ω m; The superconduction carbon black is Dutch AKZO(Aksu. Nobel) and the Ketjen black Ketjenblack EC300J that provides of company; Electrically conductive graphite is commercially available crystalline flake graphite; Vibrin is Dynapol L205(Germany Evonik company (former German Degussa company)); Water-borne acrylic resin is the Jelee WA 2007A/2008A(emulsion that the lucky Lik-Sang in Zhuhai produces); Aqueous polyurethane is the Jelee AC 830JW(emulsion that the lucky Lik-Sang in Zhuhai produces); Dispersion agent is the levelling dispersion agent, is the BYK345 of German Bi Ke.The optional market of other materials vending articles, all material all need not pre-treatment.
It is the mass percent composition of 5 embodiment of electric heating ink formulations that following table has been listed carbon:
Table 1
A. emulsion solid content 30%(mass percent), listed numerical value is the solids content of conversion;
B. need to count the moisture in the resin emulsion
Described carbon is that 5 embodiment of electric heating ink formulations all can finish according to identical printing ink to manufacture technology, and the concrete operations step comprises:
(a) measure 5# in the table 1 (calculating the quality of the emulsion that needs by the required solid masses of prescription), 6# (calculating the quality of the emulsion that needs by the required solid masses of prescription), 7#, 8# and 9#, mix with 10# successively, add the residual content ((deducting the 5# of input and the moisture quality among the 6# by the required quality of prescription) of calculating good 11#;
(b) (more than 50～100rpm) adds 1#, 2# and 3# successively under the stirring, all adds (200～300rpm) mixing 15-30 minute of back high-speed stirring;
(c) pulverize below the 4# to 2mm, in the adding said mixture material, add the back and continue to stir (200～300rpm) mixing 15-30 minute;
(d) said mixture grinds 2～4 times with three-roll grinder, makes its particle fineness be lower than 50 microns;
(e) be ground to fineness with sand mill again and be lower than 20 microns, need 1mm glass sphere grinding medium;
(f) filtration obtains slurry, stirs to add 12# and 13# down, mix more than 5～10 minutes,
(g) the packing back stores.
Equipment all selects for use single to be processed as the equipment that the printing ink total mass is 200～2000g in the above step.
The ink containment time in the embodiment of the present invention that it should be noted that can not surpass for 2 weeks, can regulate viscosity to print request under stirring and ultra-sonic dispersion with ethanol before using.Storing the printing ink that surpassed for 2 weeks perhaps has large granular materials to separate out, and can reclaim, and uses through grinding with after regulating viscosity.
Table 2 has been listed side's resistance of calculating solid content (conductive carbon material and resin quality per-cent sum), viscosity and the printing back electric heating ink coating of five embodiment.
Table 2
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Solid content (% wt) a | 46 | 43 | 54 | 51 | 52 |
| Viscosity (Pa.S) b | 53 | 47 | 68 | 71 | 97 |
| The resistance of electro-thermal coatings side (Ω/) c | 186 | 135 | 33 | 101 | 47 |
A. electro-conductive material and resin content summation;
B. viscosity test condition: Brookfield HBDV-II+Pro, T spindle E, 10 rpm, 25 ° of C;
C. silk screen printing is in the PET film, 120 ℃ of dryings 30 minutes, 90 ~ 120 microns of thick coatings
From last table 2 as can be known, carbon of the present invention is five embodiment of electric heating printing ink, and solid content (mass percent) is 40～55%, and viscosity is 47～100 Pa.S, all significantly is lower than most commercial like product (50～70%).Embodiment 1 and embodiment 2 for about 50 Pa.S can be applied to intaglio printing, although its print speed can be lower than common base gravure ink (20～25Pa.S).For the bigger embodiment 4 of viscosity, can be used for the quick silk screen typography.Because the adding of the carbon nanotube of good conductivity and superconduction graphite, under the equal print thickness (about 100 microns), embodiment 3 gained carbon are that coating side's resistance of electric heating printing ink can be low to moderate 33 Ω/, and embodiment 5 viscosity are bigger, only are suitable for the low speed silk screen printing.
Above embodiment only is preferred implementation column of the present invention; for the technology among the present invention; under the prerequisite that does not break away from core technology feature of the present invention, can also make some improvements and modifications, these retouchings and improvement also should belong to scope of patent protection of the present invention.
Claims (10)
1. a carbon is electric heating printing ink, and its mass percent consists of: carbon nanotube 0～2%, superconduction carbon black 2～12%, electrically conductive graphite 5～35%, resin 10-30%, solvent 30～70% and auxiliary agent 0.2～8%; Described carbon is that the range of viscosities of electric heating printing ink is 10Pa.S～200Pa.S.
2. carbon according to claim 1 is electric heating printing ink, it is characterized in that, the ratio of described carbon nanotube and superconduction carbon black is lower than 0.2.
3. carbon according to claim 2 is electric heating printing ink, it is characterized in that, the ratio of described superconduction carbon black and electrically conductive graphite is: 0.1～0.5.
4. carbon according to claim 1 is electric heating printing ink, it is characterized in that, described resin comprises particulate state vibrin, water-borne acrylic resin emulsion and aqueous polyurethane resin emulsion, and the mass percent of their solids is 1:0.5～2:0.5～2.
5. will remove 1 described carbon according to right is electric heating printing ink, it is characterized in that, described solvent is the combination of the monohydroxy-alcohol of water and two or three carbon atoms, and water is 0.3～1.2 to the mass ratio of alcohol.
6. will remove 5 described carbon according to right is electric heating printing ink, it is characterized in that, also contains total mass in the described solvent and is lower than 5% ethyl acetate or acetone.
7. will remove 1 described carbon according to right is electric heating printing ink, it is characterized in that, described auxiliary agent comprises: dispersion agent and levelling defoamer, dispersion agent is 0.25～0.50 to the mass percent of levelling defoamer.
8. will remove 1 described carbon according to right is electric heating printing ink, it is characterized in that, described dispersion agent is Sodium dodecylbenzene sulfonate or polyoxyethylene octyl phenyl ether; Described levelling defoamer is polyether-modified polysiloxane-based.
9. the described carbon of claim 1-8 is the preparation method of electric heating printing ink, it is characterized in that, particulate state vibrin in the resin is crushed to below the median size 0.5mm, then with carbon nanotube, superconduction carbon black, electrically conductive graphite, solvent, auxiliary agent and resin in all the other components mix and be ground to fineness by three-roll grinder and be lower than 50 microns, be ground to fineness with sand mill again and be lower than 20 microns, filtering and namely obtaining carbon is electric heating printing ink.
10. will remove 9 described carbon according to right is the preparation method of electric heating printing ink, it is characterized in that, also adds total mass after the filtration and is lower than 5% ethyl acetate or acetone.
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Application publication date: 20130904 |