CN103305051A - Low-temperature radiation electrothermal film and preparation method thereof - Google Patents
Low-temperature radiation electrothermal film and preparation method thereof Download PDFInfo
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- CN103305051A CN103305051A CN 201310186181 CN201310186181A CN103305051A CN 103305051 A CN103305051 A CN 103305051A CN 201310186181 CN201310186181 CN 201310186181 CN 201310186181 A CN201310186181 A CN 201310186181A CN 103305051 A CN103305051 A CN 103305051A
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Abstract
The invention discloses a low-temperature radiation electrothermal film and a preparation method thereof. The carbon nanometer conductive ink comprises the following components in mass percent: 1 to 5% of carbon nano tube, 94 to 98% of solvent, and 0.2 to 2% of surface active agent. The preparation method comprises the following steps: manufacturing a hot melt adhesive layer on a polyester film; printing a carbon nanometer conductive ink layer onto the hot melt adhesive layer; printing a generating and heating ink layer on the ink layer; manufacturing an electrode; and then hot-processing and compounding the polyester film through a hot melt adhesive film. The low-temperature electric radiant heater film has the characteristics that the peeling strength is high and the electro thermal power can be flexibly adjusted.
Description
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Technical field
The present invention relates to a kind of low-temp radiating electrothermal membrane and preparation method thereof, belong to the thermo electric material technology.Concrete, relate to a kind of manufacture method of prescription, manufacturing process and associated electrical hotting mask of carbon nano conductive printing ink, belong to the thermo electric material technical field.
Background technology
Use electric heating membrane type heating to have water saving, save land, economize material and be convenient to the advantages such as adjusting, metering.Low-temp radiating electrothermal membrane is used for heating residential, and the important way of hot-water heating can be used for northern China rural area or southern warming as an alternative, and needs the northern big city central heating of control source of pollution.Common Electric radiant Heating Film is to be made between insulation polyester film through processing, hot pressing by electrically conductive ink printing, metal electrode bar on the market.The electrically conductive ink that forms electro-thermal coatings is the key problem in technology of this series products.
It is electrothermal printing ink that patent CN01124036.9 has announced a kind of carbon that adds silver powder; Patent CN200510202542.9 has announced a kind of receiving-microstage graphite and graphitized carbon black is the electric-heating coatings of electro-conductive material; Patent CN201010219932.7 has announced the water-based electric heating coating that a kind of carbon is, can adapt to multiple coating method; Patent CN201210160997.8 has announced a kind of carbon series electric heating coating that adds the infrared emission material.The electric heating printing ink that above-mentioned patent is announced or electric-heating coatings product, and at present commercially available electric heating printing ink (electric thermal power is approximately 200 to 300W/m in order to satisfy the electrical property design requirements
2), all need to add approximately 50% carbon series conductive material of massfraction; 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 larger, and viscosity is higher, and it is narrow that typography adapts to window.So problems such as stripping strength is not ideal enough, printing quality is difficult to control, product electric thermal power density is even not that the low-temp radiating electrothermal membrane of existing electric heating printing ink preparation exists.
Carbon nanotube has excellent mechanics and electric property.A small amount of even carbon nanotube is dispersed in matrix inside will form conductive network.Patent CN201010246953.8 has announced a kind of carbon series electric heating coating that comprises carbon nanotube.Patent CN200780043467.2 and CN201110333623.7 have announced and have comprised the electrically conductive ink that carbon nanotube is done electro-conductive material, and they all might be used to make electrothermal device.Yet the carbon nanotube in the above-mentioned electrically conductive ink can't keep homogeneously dispersed state same in the printing ink after the printing drying, resin, the residual compositions such as tensio-active agent also can reduce the conductivity of electro-thermal coatings.The carbon current nanotube is done electro-conductive material and is used for electric heating printing ink and has undesirable and the problem that Costco Wholesale is higher of conductivity.
Summary of the invention
In view of this, the purpose of this invention is to provide a kind of carbon nano conductive printing ink.
For achieving the above object, the invention provides a kind of carbon nano conductive printing ink, the mass percent of described carbon nano conductive printing ink consists of: carbon nanotube 1～5%, solvent 94～98% and tensio-active agent 0.2～2%, this ink printing forms carbon nanotube layer, as the part of the electro-thermal coatings of low-temp radiating electrothermal membrane.
As the preferred version of above-mentioned a kind of carbon nano conductive printing ink, the resistivity of wherein said carbon nanotube is below 0.2 ohm meter.The mass percent of concrete carbon nanotube is 1-5%; Preferably, be 2-4%.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 large; 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 in the technical scheme of the present invention is the multi-walled carbon nano-tubes of resistivity 0.2 ohm-meter of Shenzhen lattice Lay Fitow battery material company limited sale, uses front without any pre-treatment.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 the preferred version of above-mentioned a kind of carbon nano conductive printing ink, wherein said solvent is the monohydroxy-alcohol with two or three carbon atoms; Consider safety, environmental influence, cost and drying effect, optional lower molecular weight monohydroxy-alcohol comprises ethanol, n-propyl alcohol, Virahol.Preferably, solvent is ethanol, and mass percent is 94～98%.More preferably, solvent is industrial alcohol, and mass percent is 95-97%.Be to promote the drying of micro-moisture, need to add mass percent and be 2～6% ethyl acetate or acetone as dry promotor.
As the preferred version of above-mentioned a kind of carbon nano conductive printing ink, wherein said tensio-active agent is the combination of a kind of anion surfactant and a kind of nonionogenic tenside; Selectable tensio-active agent comprises: anion surfactant, and such as C
8-16H
17-33SO
3 -Na
+, C
8-16H
17-33SO
4 -Na
+, C7F
15COO
-K
+, C
7F
15COO
-Na
+, (CF
3)
2CF (CF
2)
4COO
-Na
+Deng; Cats product; Such as C
8-16H
17-33N
+(CH3) Br
-, C
14H
29N
+(C
2H
5)
3Br
-, C
14H
29N
+(C
4H
9)
3Br
-Deng; Nonionogenic tenside is such as C
8-15The polynary Volpo S 10 of straight or branched alkyl, C
8-15Straight or branched alkyl-phenol-polynary Volpo S 10, straight-chain alkyl glucoside etc.; Amphoterics is such as C
8-16H
17-33N
+(CH
3)
2CH
2COO
-Series.Above-mentioned tensio-active agent all to carbon nanotube in solvent dispersion and stable effectively; Preferred from the angle of easy acquisition, select Sodium dodecylbenzene sulfonate (SDBS), cetyl trimethylammonium bromide (CTAB) or polyoxyethylene octyl phenyl ether (Triton X-100), content is 0.2-2%(wt); More preferably, select Sodium dodecylbenzene sulfonate and Triton X-100, composite according to the ratio of 2:1 to 6:1, total content is 0.2-2%(wt).
The present invention also provides the preparation method of above-mentioned carbon nano conductive printing ink, carries out dispersion machine after will mixing according to each component that above-mentioned mass percent takes by weighing and grinds, and obtains described carbon nano conductive printing ink, and its range of viscosities is 1Pa.S-200Pa.S.
As the preparation method's of above-mentioned a kind of carbon nano conductive printing ink preferred version, its concrete steps comprise:
(1) measure by mass percentage solvent, join the there-necked flask of 1000ml under 300 rev/mins, stir the lower tensio-active agent that adds by mass percentage in this rotating speed subsequently, the purity of wherein said ethanol is 95%(wt);
(2) stir after 4-6 minute, add carbon nanotube by mass percentage, continue under the aforementioned rotating speed and stirred 10-20 minute;
(3) above-mentioned finely dispersed slurry is on average added the test-type dispersion machine in two batches and grind, abrasive material is 2mm toughened glass ball, rotating speed 950-1000 rev/min, every batch is ground three times, the each grinding 8-12 minute, interval 8-12 minute, detecting fineness with scraper plate fineness instrument at last was 19 microns;
(4) collect the there-necked flask of 1000ml after ground slurry merges, sampling makes it in the gravure claimed range of 20～25s or in the silk-screen claimed range of 30～40s according to " the GB/T 13217.4-2008 liquid ink viscosity method of inspection " estimated viscosity;
(5) do not meet above-mentioned requirements such as estimated viscosity, adding ethanol or underpressure distillation go out partial solvent under 200-300 rev/min stirring, adjust the gravure requirement that viscosity meets 20～25s; Perhaps underpressure distillation goes out solvent, adjusts the silk-screen requirement that viscosity meets 30～40s;
(6) transfer in the sealed vessel for subsequent usely, if period of storage surpasses a week, need to repeat above-mentioned steps (3), (4), (5).
The present invention also provides the low-temp radiating electrothermal membrane that contains above-mentioned carbon nano conductive printing ink, described low-temp radiating electrothermal membrane comprises a bottom polyethylene terephthalate thin film, be provided with a hot melt adhesive layer on the described bottom polyethylene terephthalate thin film, be provided with a carbon nano conductive printing ink layer on the described hot melt adhesive layer, be provided with a conductive exothermal ink lay on the described carbon nano conductive printing ink layer, be respectively arranged with an electrode on the both lateral sides edge of described conductive exothermal ink lay, be provided with a upper strata polyethylene terephthalate thin film by a hot melt adhesive film on described conductive exothermal ink lay and the electrode.
The present invention further provides the preparation method of above-mentioned low-temp radiating electrothermal membrane, may further comprise the steps:
Steps A is made hot melt adhesive layer in the bottom polyethylene terephthalate thin film;
Step B at hot melt adhesive layer printing carbon nano conductive printing ink layer, and carries out hot-rolling and presses;
Step C is at carbon nano conductive printing ink layer coating conductive exothermal ink lay;
Step D, on the both lateral sides edge of conductive exothermal ink lay on printing conductive silver slurry and paste copper strips as electrode;
Step e, the compound upper strata of hot pressing polyethylene terephthalate thin film.
Preferred version as the preparation method of above-mentioned a kind of low-temp radiating electrothermal membrane, wherein step is among the A, be coated with hot melt adhesive layer in the bottom polyethylene terephthalate thin film, the thickness of bottom polyethylene terephthalate thin film is 100～200 microns, 50～100 microns of the thickness of hot melt adhesive layer; The hot melting temperature of described hot melt adhesive layer is 80～150 degrees centigrade, and can carry out hot melting cohesion to the carbon nanotube layer without binder under hot pressing and become as a whole.
Preferred version as the preparation method of above-mentioned a kind of low-temp radiating electrothermal membrane wherein among the step B, is printed on carbon nano conductive printing ink layer on the hot melt adhesive layer, is 2～10 microns through the thickness of printed layers after the dry out solvent.
As the preparation method's of above-mentioned a kind of low-temp radiating electrothermal membrane preferred version, wherein among the step C, printing conductive heating ink lay is 50～150 microns through its thickness after the dry out solvent on carbon nanotube layer.
As the preparation method's of above-mentioned a kind of low-temp radiating electrothermal membrane preferred version, wherein among the step D, the thickness of printed silver slurry is 5～30 microns, and width is 5～10 millimeters; The thickness of pasting copper strips is 0.2～0.5 millimeter, and width is 5～10 millimeters.
As the preparation method's of above-mentioned a kind of low-temp radiating electrothermal membrane preferred version, wherein in the step e, in conductive exothermal ink lay and the compound upper strata of hot pressing polyethylene terephthalate thin film above the electrode, and use hot melt adhesive film to make tack coat; Its at the middle and upper levels the thickness of polyethylene terephthalate thin film be 100～200 microns, 40～100 microns of hot melt adhesive film thickness.
Low-temp radiating electrothermal membrane provided by the present invention is compared with existing commercial like product, but has that stripping strength is high, characteristics of electric thermal power flexible and electric thermal power even density.
The beneficial effect that the present invention has is as follows:
(1) stripping strength is high.
Low-temp radiating electrothermal membrane provided by the present invention, its carbon nano conductive printing ink layer is to adopt the blank printing ink that does not contain carbonaceous material, compare with direct printing common electrical deep fat China ink, body material is had higher adhesion strength, be conducive to improve the stripping strength of Electric radiant Heating Film.
Adopt the low-temp radiating electrothermal membrane of the inventive method preparation, contain similar resin material in the blank printing ink of lower floor and the upper strata electric heating printing ink, in printing and the subsequent drying process, the mutually diffusion bonding of the resin of levels printing ink can guarantee that Electric radiant Heating Film has designed stripping strength.
(2) electric power can be adjusted neatly as required.
Low-temp radiating electrothermal membrane provided by the present invention for the adjusting of electric thermal power, except the electroconductibility and print thickness that can adjust conduction electricity heating ink lay, also can be adjusted electroconductibility and the print thickness of carbon nano conductive printing ink layer.And latter's adjustable range is larger; Therefore this low-temp radiating electrothermal membrane, electric power can be adjusted more neatly as required.
(3) degree of irregularity of electric thermal power density can be reduced effectively.
Low-temp radiating electrothermal membrane provided by the present invention after its carbon nano conductive printing ink printing, through not exclusively dry, has formed conductive network.In the printing of subsequently conductive exothermal ink lay and the complete drying engineering, but the impact of the conductive network that the resin diffusion bonding of levels printing ink has formed carbon nanotube is very little, can ignore.So the carbon nanotube layer that not resiniferous carbon nano conductive printing ink printing forms, conductivity is higher than common conductive exothermal ink lay, and the two is relation in parallel.
Low-temp radiating electrothermal membrane provided by the present invention, solid content is lower in its carbon nano conductive printing ink, and the thin and thick deviation of the carbon nanotube layer that printing forms can be controlled very littlely, and its electroconductibility is higher than the hot ink lay of common electrical.So the conductive coating that the hot ink lay of carbon nanotube layer and common electrical is compounded to form, the degree of irregularity of its electric thermal power density can be reduced effectively.
Description of drawings
Fig. 1 is low-temp radiating electrothermal membrane structural profile schematic diagram of the present invention.
Symbology among the figure:
1 bottom polyethylene terephthalate (PET) film;
The 2-hot melt adhesive layer;
3-carbon nano conductive printing ink layer;
4-conductive exothermal ink lay;
5-copper strips electrode (conductive silver paste adhesion);
The 6-hot melt adhesive film;
7-upper strata polyethylene terephthalate (PET) film.
Embodiment
Be noted that following specifying all is example, be intended to further specify the invention provides, except as otherwise noted, all Science and Technology terms used herein have the identical meanings of usually understanding with the technical field of the invention personnel.
The invention provides a kind of carbon nano conductive printing ink, the mass percent of described carbon nano conductive printing ink consists of: carbon nanotube 1～5%, solvent 94～98% and tensio-active agent 0.2～2%, this ink printing forms carbon nanotube layer.
As shown in Figure 1, the present invention also provides the low-temp radiating electrothermal membrane that contains above-mentioned carbon nano conductive printing ink, described low-temp radiating electrothermal membrane comprises bottom polyethylene terephthalate (PET) film 1, be provided with a hot melt adhesive layer 2 on described bottom polyethylene terephthalate (PET) film 1, be provided with a carbon nano conductive printing ink layer 3 on the described hot melt adhesive layer 2, be provided with a conductive exothermal ink lay 4 on the described carbon nano conductive printing ink layer 3, be respectively arranged with a copper strips electrode (conductive silver paste adhesion) 5 on the both lateral sides edge of described conductive exothermal ink lay 4, be provided with upper strata polyethylene terephthalate (PET) film 7 by a hot melt adhesive film 6 on described conductive exothermal ink lay and the electrode.
The present invention will be further described below in conjunction with drawings and Examples.
Carbon nanotube in the embodiment of the present invention is the multi-walled carbon nano-tubes (Shenzhen lattice Lay Fitow battery material company limited) that resistivity is lower than 0.2 ohm-meter; Conductive exothermal printing ink is selected the product (Shenzhen treasured adds beneficial Science and Technology Ltd.) of rear sheet resistance 400 Ω of seal/ (25 μ m ± 10%); Blank printing ink (Shenzhen treasured adds beneficial Science and Technology Ltd.).Used other materials is commercially available among the prescription of carbon nano conductive printing ink and the Electric radiant Heating Film preparation method.
Following table has been listed the embodiment 1-5 (5 prescriptions) of carbon nanotube conducting printing ink, and all material all need not pre-treatment.
A) purity is greater than 95%(wt) industrial alcohol
B) triton X-100, or polyoxyethylene glycol uncle octyl phenyl ether, chemical pure
C) Sodium dodecylbenzene sulfonate, chemical pure
The carbon nano conductive printing ink adopts general printing-ink preparation method.The below 2 is described as follows to fill a prescription:
(1) measures industrial alcohol (95%wt) 438.5g, ethyl acetate 5g, the lower there-necked flask that joins 1000ml in about 300 rev/mins;
(2) and under above-mentioned rotating speed stirring add 0.3g Sodium dodecylbenzene sulfonate SDBS;
(3) stir after 5 minutes, add the 2.0g carbon nanotube, continue under the aforementioned rotating speed and stirred 15 minutes;
(4) above-mentioned finely dispersed slurry is added test-type dispersion machine (YX-400 in two batches, Guangzhou space star mechanical means company limited) grinds, abrasive material is 2mm toughened glass ball, 1000 rev/mins of rotating speeds, every batch is ground three times, the each grinding 10 minutes, interval 10 minutes, detecting fineness with scraper plate fineness instrument at last is 19 microns;
(5) collect the there-necked flask of 1000ml after ground slurry merges, sampling according to " the GB/T 13217.4-2008 liquid ink viscosity method of inspection ", use No. 3 grace to examine glass estimated viscosity to be 21s, it is in the gravure claimed range of 20～25s;
(6) do not meet above-mentioned gravure technique requirement such as estimated viscosity, can go out partial solvent in stirring lower adding ethanol or underpressure distillation, adjust the gravure requirement that viscosity meets 20～25s; Also can underpressure distillation go out solvent, adjust the silk-screen requirement that viscosity meets 30～40s.
(7) transfer in the sealed vessel for subsequent usely, if period of storage surpasses a week, need to repeat above-mentioned steps (4), (5), (6).
Among the preparation method of Electric radiant Heating Film: hot melt adhesive applies and can adopt craft or spreadometer, and printing ink can craft or machine silk screen printing and machine Automatic continuous intaglio, and compound upper strata PET film needs coating machine.
Embodiment 1:
The screen printing template that adopts Shenzhen sakata Xin Sida screen print materials firm to provide, their design parameter such as following table, length and wide 300mm and the 200mm of being respectively, wherein half tone B is manufactured with the wide rectangular printing surface of 7mm in the half tone both sides, be used for the printed silver slurry, use urethane scraper hand-printing.
| ? | The order number | Wire diameter (micron) | Aperture (micron) | Thickness (micron) | Tension force (N/cm) |
| Half tone A | 325 | 28 | 40－50 | 56 | 30 |
| Half tone B | 500 | 18 | 30－40 | 27 | 25 |
Operation steps is as follows:
(1) prepare material and instrument: clean half tone B and dry, cut out long and wide PET film and the hot melt adhesive film (approximately 50 microns on M-716A type, thickness) that is slightly larger than half tone B size, the PET film thickness is 120 microns.
(2) make hot melt adhesive layer: the PET film is deployed on the smooth hand-printing platform, half tone A is loaded onto printing platform, with stainless steel scraper printed liquid hot melt adhesive (BY8015), take off after the printing and put into 70 degrees centigrade of baking ovens after compressing, dry 20 minutes; Republish once, recording the first composite membrane thickness after the drying is 180 microns (60 microns of hot melt adhesive layers), adopts acetone to clean web plate A, and then water rinses out the acetone soln on the web plate A.
(3) make carbon nano conductive printing ink layer: the first composite membrane that makes in the step (2) is deployed on the smooth hand-printing platform, and PET film wherein is at the lowest layer; Half tone A is installed, with the carbon nano conductive printing ink of stainless steel scraper printing abovementioned steps (1), takes off after the printing and put into 70 degrees centigrade of baking ovens after compressing, dry 30 minutes; Republish once, recording the second composite membrane thickness after the drying is 183 microns (being 3 microns of carbon nano conductive printing ink bed thickness), adopts acetone to clean half tone A, and then water rinses out the acetone soln on the half tone A.
(4) make the conductive exothermal ink lay: the second composite membrane (carbon nano conductive printing ink layer) that makes in the step (3) is deployed on the smooth hand-printing platform, PET film wherein is at the lowest layer, the A net is installed, compress rear with stainless steel scraper printing conductive heating printing ink (Shenzhen treasured adds beneficial Science and Technology Ltd.), take off after the printing and put into 70 degrees centigrade of baking ovens, dry 30 minutes; Republish once, recording the 3rd composite membrane thickness after the drying is 250 microns (being 67 microns of conductive exothermal printing ink bed thickness), adopts acetone to clean half tone A, and then water rinses out the acetone soln on the half tone A.
(5) make silver slurry and electrode strip: the 3rd composite membrane that makes in the step (4) is deployed on the smooth hand-printing platform, and PET film wherein is at the lowest layer; Half tone B is installed; Printed silver is starched on the both sides of the edge of this conductive exothermal ink lay respectively; Clean half tone with alcohol after the printing; The copper strips compression of cutting out is attached on this silver slurry; Put into 110 degrees centigrade of baking ovens 30 minutes, and so that the silver slurry is dry, obtained the 4th composite membrane; The sheet resistance of measuring the Electric radiant Heating Film of preparation with the sheet resistance instrument is 103 Ω/.
(6) compound upper strata PET film: the 4th composite membrane that makes in the step (5) is deployed on the smooth table top, and PET film wherein is at the lowest layer; Above hot melt adhesive film (M-716A type) is superimposed on; Again the PET film stack is combined in above the hot melt adhesive film; Use common office plastic packaging machine, Temperature Setting is at 130 degrees centigrade, and transfer rate is chosen in the slowest shelves (approximately 1cm/S), obtains described low-temp radiating electrothermal membrane (Fig. 1).
Embodiment 2:
Printing is 3 times in making carbon nano conductive printing ink layer step, and other operations are identical with embodiment 1, record approximately 5 microns of carbon nano conductive printing ink thickness, and the sheet resistance of measuring before the PET film step of compound upper strata is 81 Ω/.
Embodiment 3:
Use the carbon nano conductive printing ink of prescription 3 in making carbon nano conductive printing ink layer step, other operations are identical with embodiment 1, record approximately 4 microns of carbon nano conductive printing ink thickness, and the sheet resistance of measuring before the PET film step of compound upper strata is 89 Ω/.
Embodiment 4:
Use the carbon nano conductive printing ink of prescription 4 in making carbon nano conductive printing ink layer step, other operations are identical with embodiment 1, record approximately 6 microns of carbon nano conductive printing ink thickness, and the sheet resistance of measuring before the PET film step of compound upper strata is 65 Ω/.
The relevant test result of the low-temp radiating electrothermal membrane of above 4 embodiment preparation is listed in the following table 1.As can be seen from Table 1: the sheet resistance of Electric radiant Heating Film can be regulated by the thickness of control carbon nano conductive printing ink layer.
The test result of table 1 embodiment 1-4 relatively
| | Embodiment | 1 | |
|
Embodiment 4 |
| The thickness (micron) of carbon nano conductive |
3 | 5 | 4 | 6 | |
| Record sheet resistance (Ω/) before the compound upper strata PET | 103 | 81 | 89 | 65 |
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; that is, the technical scheme of the complex electrocaloric film that every employing guide layer and conductive heating layer are combined with each other all falls in the protection domain of patent of the present invention.
Claims (14)
1. a carbon nano conductive printing ink is characterized in that, the mass percent of described carbon nano conductive printing ink consists of: carbon nanotube 1～5%, solvent 94～98% and tensio-active agent 0.2～2%.
2. carbon nano conductive printing ink according to claim 1 is characterized in that, the resistivity of described carbon nanotube is below 0.2 ohm meter.
3. carbon nano conductive printing ink according to claim 1 is characterized in that, it is 94～98% ethanol, n-propyl alcohol, Virahol or its combination that described solvent contains mass percent, and mass percent is 2～6% ethyl acetate, acetone or its combination.
4. carbon nano conductive printing ink according to claim 1 is characterized in that, described tensio-active agent is the combination of Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide or polyoxyethylene octyl phenyl ether.
5. carbon nano conductive printing ink according to claim 1 is characterized in that, described tensio-active agent is that Sodium dodecylbenzene sulfonate and polyoxyethylene octyl phenyl ether are composite according to the ratio of 2:1 to 6:1, and total content is 0.2-2%(wt).
6. the preparation method of each described carbon nano conductive printing ink of claim 1-5, it is characterized in that, carry out the dispersion machine grinding and regulate viscosity after will mixing according to each component that above-mentioned mass percent takes by weighing, obtain described carbon nano conductive printing ink, its range of viscosities is 1Pa.S-200Pa.S.
7. preparation method according to claim 6 is characterized in that, concrete steps comprise:
(1) measure by mass percentage solvent, join the there-necked flask of 1000ml under 300 rev/mins, stir the lower tensio-active agent that adds by mass percentage in this rotating speed subsequently, the purity of wherein said ethanol is 95%(wt);
(2) stir after 4-6 minute, add carbon nanotube by mass percentage, continue under the aforementioned rotating speed and stirred 10-20 minute;
(3) above-mentioned finely dispersed slurry is on average added dispersion machine in two batches and grind, abrasive material is 2mm toughened glass ball, rotating speed 950-1000 rev/min, every batch is ground three times, the each grinding 8-12 minute, interval 8-12 minute, detecting fineness with scraper plate fineness instrument at last was 19 microns;
(4) collect the there-necked flask of 1000ml after ground slurry merges, sampling makes it in the gravure claimed range of 20～25s or in the silk-screen claimed range of 30～40s according to " the GB/T 13217.4-2008 liquid ink viscosity method of inspection " estimated viscosity;
(5) do not meet above-mentioned requirements such as estimated viscosity, adding ethanol or underpressure distillation go out partial solvent under 200-300 rev/min stirring, adjust the gravure requirement that viscosity meets 20～25s; Perhaps underpressure distillation goes out solvent, adjusts the silk-screen requirement that viscosity meets 30～40s;
(6) transfer in the sealed vessel for subsequent usely, if period of storage surpasses a week, need to repeat above-mentioned steps (3), (4), (5).
8. low-temp radiating electrothermal membrane that contains carbon nano conductive printing ink claimed in claim 1, it is characterized in that, described low-temp radiating electrothermal membrane comprises a bottom polyethylene terephthalate thin film, be provided with a hot melt adhesive layer on the described bottom polyethylene terephthalate thin film, be provided with a carbon nano conductive printing ink layer on the described hot melt adhesive layer, be provided with a conductive exothermal ink lay on the described carbon nano conductive printing ink layer, be respectively arranged with an electrode on the both lateral sides edge of described conductive exothermal ink lay, be provided with a upper strata polyethylene terephthalate thin film by a hot melt adhesive film on described conductive exothermal ink lay and the electrode.
9. the preparation method of a low-temp radiating electrothermal membrane claimed in claim 8 is characterized in that, may further comprise the steps:
Steps A is made hot melt adhesive layer in the bottom polyethylene terephthalate thin film;
Step B at hot melt adhesive layer printing carbon nano conductive printing ink layer, and carries out hot-rolling and presses;
Step C is at carbon nano conductive printing ink layer coating conductive exothermal ink lay;
Step D, on the both lateral sides edge of conductive exothermal ink lay on printing conductive silver slurry and paste copper strips as electrode;
Step e, the compound upper strata of hot pressing polyethylene terephthalate thin film.
10. method according to claim 9, it is characterized in that, step is among the A, is coated with hot melt adhesive layer in the bottom polyethylene terephthalate thin film, the thickness of bottom polyethylene terephthalate thin film is 100～200 microns, 50～100 microns of the thickness of hot melt adhesive layer; The hot melting temperature of described hot melt adhesive layer is 80～150 degrees centigrade.
11. method according to claim 9 is characterized in that, among the step B, carbon nano conductive printing ink layer is printed on the hot melt adhesive layer, the thickness of printed layers is 2～10 microns after the process dry out solvent.
12. method according to claim 9 is characterized in that, among the step C, printing conductive heating ink lay is 50～150 microns through its thickness after the dry out solvent on carbon nanotube layer.
13. method according to claim 9 is characterized in that, among the step D, the thickness of printed silver slurry is 5～30 microns, and width is 5～10 millimeters; The thickness of pasting copper strips is 0.2～0.5 millimeter, and width is 5～10 millimeters.
14. method according to claim 9 is characterized in that, in the step e, in conductive exothermal ink lay and the compound upper strata of hot pressing polyethylene terephthalate thin film above the electrode, and uses hot melt adhesive film to make tack coat; Its at the middle and upper levels the thickness of polyethylene terephthalate thin film be 100～200 microns, 40～100 microns of hot melt adhesive film thickness.
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| CN103555067A (en) * | 2013-10-24 | 2014-02-05 | 张贤波 | Conductive ink for regulating power as well as preparation method and application of conductive ink |
| CN103763798A (en) * | 2014-02-19 | 2014-04-30 | 黑龙江中惠地热股份有限公司 | Electrothermal film with temperature power coefficient and manufacturing method |
| CN103776082A (en) * | 2014-02-21 | 2014-05-07 | 黑龙江中惠地热股份有限公司 | PTC (Positive Temperature Coefficient) electric heating floor film and manufacturing method thereof |
| CN103823593A (en) * | 2014-02-27 | 2014-05-28 | 蓝思科技（长沙）有限公司 | Method for preparing cover glass with colorful window frame and application of cover glass |
| CN104449046A (en) * | 2014-12-09 | 2015-03-25 | 上海宥拓化学有限公司 | Conductive ink and application thereof |
| CN104575687A (en) * | 2014-10-28 | 2015-04-29 | 天津工业大学 | Carbon nano tube flexible and transparent conductive thin film with strong adhesive force and method for preparing thin film |
| WO2015096591A1 (en) * | 2013-12-23 | 2015-07-02 | 北京阿格蕾雅科技发展有限公司 | High-dispersion carbon nanotube composite conductive ink |
| CN105307299A (en) * | 2015-10-23 | 2016-02-03 | 黄山金菱新材料有限公司 | Carbon crystal electric heating paper, compound paper by adopting electric heating paper and preparation method thereof |
| CN107097546A (en) * | 2017-04-27 | 2017-08-29 | 东莞泰升玻璃有限公司 | A kind of type of heat glass panel and its manufacture method |
| CN107197543A (en) * | 2017-05-31 | 2017-09-22 | 华东师范大学 | A kind of preparation method of the low dimensional nano-sized carbon electric heating film of Nano Silver surface modification |
| CN108027435A (en) * | 2015-09-30 | 2018-05-11 | 海拉两合有限公司 | For the method for manufacturing antenna house and corresponding antenna house |
| CN109068412A (en) * | 2018-07-11 | 2018-12-21 | 安徽宝利乐暖环保科技有限公司 | A kind of containing graphene and the water nano heating film of carbon nanotube and preparation method thereof |
| CN109104778A (en) * | 2018-08-07 | 2018-12-28 | 江阴亿霖包装有限公司 | A kind of production method of low-temp radiating electrothermal membrane |
| CN109306209A (en) * | 2018-08-31 | 2019-02-05 | 江苏天创新材料科技有限公司 | A kind of preparation method of preparation method and cylinder the printing Electric radiant Heating Film of the black compound electro-thermal ink of graphene/carbon |
| CN109605642A (en) * | 2018-10-19 | 2019-04-12 | 河南永威安防股份有限公司 | A kind of splinter shield molding production technology |
| CN110740530A (en) * | 2019-10-12 | 2020-01-31 | 江西铜业技术研究院有限公司 | Preparation method of aqueous carbon nanotube electrothermal films |
| CN111269463A (en) * | 2020-04-02 | 2020-06-12 | 中国科学技术大学 | Ultrathin low-voltage electric heating film material in low-temperature environment and preparation method thereof |
| CN111621198A (en) * | 2020-07-17 | 2020-09-04 | 武汉世帝牧文化传媒有限公司 | Low-voltage heating ink and preparation method thereof |
| CN111712003A (en) * | 2020-06-29 | 2020-09-25 | 佛山(华南)新材料研究院 | Low-voltage infrared electrothermal film and preparation method thereof |
| CN111759579A (en) * | 2020-07-17 | 2020-10-13 | 湖北蕲艾堂科技有限公司 | Heating bag |
| CN111839885A (en) * | 2020-07-17 | 2020-10-30 | 湖北蕲艾堂科技有限公司 | Heating plate |
| CN111839886A (en) * | 2020-07-17 | 2020-10-30 | 湖北蕲艾堂科技有限公司 | Heating eye patch |
| CN112738929A (en) * | 2019-10-14 | 2021-04-30 | 崔亮 | Water-based electrothermal film and preparation method thereof |
| CN114351506A (en) * | 2022-01-06 | 2022-04-15 | 阳光王子(寿光)特种纸有限公司 | Novel electrogenerated heating decorative paper and preparation method thereof |
| CN115156526A (en) * | 2022-07-29 | 2022-10-11 | 南京极舒热磁健康科技有限公司 | Graphene rare earth conductive heating material and preparation method and application thereof |
| CN115707577A (en) * | 2022-11-01 | 2023-02-21 | 何春松 | Preparation method of thick film heating print body of glass |
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2013
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| CN103555067B (en) * | 2013-10-24 | 2015-11-25 | 张贤波 | Electrically conductive ink of a kind of regulating power and its preparation method and application |
| CN103555067A (en) * | 2013-10-24 | 2014-02-05 | 张贤波 | Conductive ink for regulating power as well as preparation method and application of conductive ink |
| WO2015096591A1 (en) * | 2013-12-23 | 2015-07-02 | 北京阿格蕾雅科技发展有限公司 | High-dispersion carbon nanotube composite conductive ink |
| CN103763798A (en) * | 2014-02-19 | 2014-04-30 | 黑龙江中惠地热股份有限公司 | Electrothermal film with temperature power coefficient and manufacturing method |
| CN103776082A (en) * | 2014-02-21 | 2014-05-07 | 黑龙江中惠地热股份有限公司 | PTC (Positive Temperature Coefficient) electric heating floor film and manufacturing method thereof |
| CN103823593A (en) * | 2014-02-27 | 2014-05-28 | 蓝思科技（长沙）有限公司 | Method for preparing cover glass with colorful window frame and application of cover glass |
| CN103823593B (en) * | 2014-02-27 | 2017-06-27 | 蓝思科技（长沙）有限公司 | Prepare method and its application of the protective glass cover plate of colorful window border |
| CN104575687B (en) * | 2014-10-28 | 2017-11-17 | 天津工业大学 | A kind of carbon nano tube flexible transparent conductive film of strong adhesive force and preparation method thereof |
| CN104575687A (en) * | 2014-10-28 | 2015-04-29 | 天津工业大学 | Carbon nano tube flexible and transparent conductive thin film with strong adhesive force and method for preparing thin film |
| CN104449046A (en) * | 2014-12-09 | 2015-03-25 | 上海宥拓化学有限公司 | Conductive ink and application thereof |
| CN108027435A (en) * | 2015-09-30 | 2018-05-11 | 海拉两合有限公司 | For the method for manufacturing antenna house and corresponding antenna house |
| CN105307299B (en) * | 2015-10-23 | 2018-08-14 | 黄山金菱新材料有限公司 | Carbon crystal electrothermo paper, the extrusion coating paper using the electrothermal paper |
| CN105307299A (en) * | 2015-10-23 | 2016-02-03 | 黄山金菱新材料有限公司 | Carbon crystal electric heating paper, compound paper by adopting electric heating paper and preparation method thereof |
| CN107097546A (en) * | 2017-04-27 | 2017-08-29 | 东莞泰升玻璃有限公司 | A kind of type of heat glass panel and its manufacture method |
| CN107197543A (en) * | 2017-05-31 | 2017-09-22 | 华东师范大学 | A kind of preparation method of the low dimensional nano-sized carbon electric heating film of Nano Silver surface modification |
| CN109068412A (en) * | 2018-07-11 | 2018-12-21 | 安徽宝利乐暖环保科技有限公司 | A kind of containing graphene and the water nano heating film of carbon nanotube and preparation method thereof |
| CN109104778A (en) * | 2018-08-07 | 2018-12-28 | 江阴亿霖包装有限公司 | A kind of production method of low-temp radiating electrothermal membrane |
| CN109306209A (en) * | 2018-08-31 | 2019-02-05 | 江苏天创新材料科技有限公司 | A kind of preparation method of preparation method and cylinder the printing Electric radiant Heating Film of the black compound electro-thermal ink of graphene/carbon |
| CN109605642A (en) * | 2018-10-19 | 2019-04-12 | 河南永威安防股份有限公司 | A kind of splinter shield molding production technology |
| CN110740530A (en) * | 2019-10-12 | 2020-01-31 | 江西铜业技术研究院有限公司 | Preparation method of aqueous carbon nanotube electrothermal films |
| CN112738929A (en) * | 2019-10-14 | 2021-04-30 | 崔亮 | Water-based electrothermal film and preparation method thereof |
| CN111269463A (en) * | 2020-04-02 | 2020-06-12 | 中国科学技术大学 | Ultrathin low-voltage electric heating film material in low-temperature environment and preparation method thereof |
| CN111712003A (en) * | 2020-06-29 | 2020-09-25 | 佛山(华南)新材料研究院 | Low-voltage infrared electrothermal film and preparation method thereof |
| CN111759579A (en) * | 2020-07-17 | 2020-10-13 | 湖北蕲艾堂科技有限公司 | Heating bag |
| CN111839885A (en) * | 2020-07-17 | 2020-10-30 | 湖北蕲艾堂科技有限公司 | Heating plate |
| CN111839886A (en) * | 2020-07-17 | 2020-10-30 | 湖北蕲艾堂科技有限公司 | Heating eye patch |
| CN111621198A (en) * | 2020-07-17 | 2020-09-04 | 武汉世帝牧文化传媒有限公司 | Low-voltage heating ink and preparation method thereof |
| CN114351506A (en) * | 2022-01-06 | 2022-04-15 | 阳光王子(寿光)特种纸有限公司 | Novel electrogenerated heating decorative paper and preparation method thereof |
| CN115156526A (en) * | 2022-07-29 | 2022-10-11 | 南京极舒热磁健康科技有限公司 | Graphene rare earth conductive heating material and preparation method and application thereof |
| CN115707577A (en) * | 2022-11-01 | 2023-02-21 | 何春松 | Preparation method of thick film heating print body of glass |
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Application publication date: 20130918 |