CN114989662A - High-temperature-resistant electrothermal ink for heating non-combustible electronic cigarette and preparation method thereof - Google Patents
High-temperature-resistant electrothermal ink for heating non-combustible electronic cigarette and preparation method thereof Download PDFInfo
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- CN114989662A CN114989662A CN202210881342.3A CN202210881342A CN114989662A CN 114989662 A CN114989662 A CN 114989662A CN 202210881342 A CN202210881342 A CN 202210881342A CN 114989662 A CN114989662 A CN 114989662A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention belongs to the technical field of electrothermal ink, and particularly relates to high-temperature-resistant electrothermal ink for heating non-combustible electronic cigarettes and a preparation method thereof, wherein the high-temperature-resistant electrothermal ink comprises the following raw materials in parts by weight: 0.2-5 parts of graphene, 0.5-5 parts of carbon nano tubes, 15-25 parts of graphite, 40-60 parts of high-temperature resistant inorganic binder, 5-15 parts of high-temperature resistant filler, 0.1-1 part of dispersing agent, 1-5 parts of temperature coefficient regulator and 10-15 parts of diluent, wherein the temperature coefficient regulator is at least one of copper oxide, manganese oxide, yttrium oxide and bismuth oxide. The high-temperature-resistant electrothermal ink disclosed by the invention has low resistance and high heating efficiency, and can be applied to an environment of 400 ℃ for a long time.
Description
Technical Field
The invention belongs to the technical field of electric heating ink, and particularly relates to high-temperature-resistant electric heating ink for heating non-combustible electronic cigarettes and a preparation method thereof.
Background
The heating non-combustion cartridge is originally developed by foreign tobacco companies such as Felmo International, and is characterized in that a special cartridge is put into a heating device, nicotine and smoke in the cartridge are released in a low-temperature baking mode, and the low-temperature baking temperature is about 300 ℃ and is far lower than the combustion temperature of the traditional cigarette more than 800 ℃. The data show that the content of carcinogenic substances in the smoke of the heating non-combustion cigarette is 80 percent less than that of the common cigarette, so that the intake of a smoker to a mutagen is reduced by 70 percent, the morbidity of bronchitis and pneumonia of the smoker is reduced by 46 percent and 36 percent, the harm of tobacco products to human bodies is greatly reduced, and the cigarette becomes a new trend leading tobacco consumption.
The existing heating non-combustion electronic cigarette mainly adopts a metal ceramic heating element to heat tobacco shreds, and the manufacturing method comprises the steps of printing tungsten-molybdenum or silver-palladium-ruthenium series thick film slurry on a ceramic tape casting blank, carrying out hot pressing lamination, and then sintering ceramic and metal together under the protection of 1600 ℃ hydrogen atmosphere to form the ceramic heating element. However, the conventional cermet heating element has a low heating efficiency because of its heat conduction heating method.
Disclosure of Invention
The first purpose of the invention is to provide a high-temperature resistant electrothermal ink for heating a non-combustible electronic cigarette, which has low resistance and high heating efficiency and can be applied to an environment of 400 ℃ for a long time.
The second purpose of the invention is to provide a preparation method of the high-temperature-resistant electrothermal ink, which is simple and suitable for industrial production.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the invention provides high-temperature-resistant electrothermal ink for heating non-combustible electronic cigarettes, which comprises the following raw materials in parts by weight:
the temperature coefficient regulator is at least one of copper oxide, manganese oxide, yttrium oxide and bismuth oxide.
The high-temperature-resistant electrothermal ink disclosed by the invention has the advantages that the graphite, the graphene and the carbon nano tube are used as conductive phases and are compounded with the high-temperature-resistant inorganic binder, the high-temperature-resistant filler, the dispersing agent, the temperature coefficient regulator and the diluent, so that the prepared electrothermal ink has low curing temperature, low resistance and high heating efficiency.
According to the invention, graphite, graphene and carbon nano tubes are used as conductive phases, so that a large amount of far infrared rays can be radiated, the electric heating coating prepared by the electric heating ink can be used for carrying out heat conduction heating and far infrared heating at the same time, and the heating efficiency is higher compared with that of a metal electric heating coating.
According to the invention, by adding the dispersing agent, all components in the electrothermal ink can be uniformly dispersed, particularly, graphite, graphene and carbon nano tubes are uniformly dispersed in an electrothermal ink system, so that the conductivity of the electrothermal ink can be improved, and an electrothermal coating prepared from the electrothermal ink can meet the design requirement of a heating body for heating a non-burning electronic cigarette.
The temperature coefficient regulator is added, so that the temperature coefficient of the electrothermal ink is reduced, the circuit design in a limited space is facilitated, and the heating time can be shortened.
The high-temperature-resistant filler is added, so that the mechanical property and the high-temperature-resistant property of the electrothermal coating can be improved, the coating can be used in a high-temperature environment for a long time, and the resistance value is not easy to change due to high temperature.
Wherein the carbon nanotube is at least one of a single-walled carbon nanotube and a multi-walled carbon nanotube. Preferably, the carbon nano tube is a single-walled carbon nano tube, the conductivity of the single-walled carbon nano tube is better, the conductivity of the electric heating ink is better facilitated to be improved, the sheet resistance of the electric heating ink after being cured can reach 3 omega/sq, and when the electric heating ink is applied to a heating body which is not used for burning an electronic cigarette, a coating can be designed to be planar, compared with a metal thick film which can only be designed to be linear, the electric heating coating made of the electric heating ink disclosed by the invention can generate heat more uniformly, and the phenomenon that the smoking taste of the electronic cigarette is influenced due to the burning of tobacco shreds or tobacco tar caused by overhigh local temperature can be effectively avoided.
Wherein the temperature coefficient regulator is a mixture of copper oxide, yttrium oxide and manganese oxide according to the weight ratio of 1:0.5-2: 3-4. By adopting the temperature coefficient regulator with the type and the proportion, the temperature coefficient of the electrothermal ink is smaller, the resistance value is more stable, the electrothermal ink is not easily influenced by temperature, the circuit design in a limited space is facilitated, and the heating time can be shortened.
Wherein the high-temperature resistant inorganic binder is at least one of silica sol, aluminum sol, titanium sol, aluminum phosphate, aluminum chromium phosphate, aluminum dihydrogen phosphate, calcium dihydrogen phosphate and magnesium dihydrogen phosphate. The adhesive has good high-temperature resistance, is beneficial to improving the high-temperature resistance of the electrothermal ink, further improves the stability of the resistance value of the electrothermal ink, and enables the electrothermal ink not to be influenced by temperature easily, and the adhesive has good bonding effect, so that the phenomenon that an electrothermal coating is not easy to fall off.
Wherein the high-temperature resistant filler is at least one of alumina powder, boron oxide, silicon micropowder, mica powder, talcum powder, titanium dioxide, boron nitride, silicon carbide, mullite and cordierite.
The dispersing agent is at least one of lignosulfonate, sodium cholate, octylphenol polyoxyethylene ether, a naphthalene sulfonic acid formaldehyde condensate, sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide, span, octadecenamine acetate, alkyl quaternary ammonium salt, aminopropylamine dioleate, polyaminoamide phosphate, a multi-built polyol-polyethyleneimine block copolymer and dodecylphenol polyoxyethylene ether. The dispersing agent has better dispersing effect, and is more beneficial to uniformly dispersing the graphene and the carbon nano tube conductive agent in an electric heating ink system and improving the conductivity of the electric heating ink.
Wherein the diluent is at least one of ethylene glycol, propylene glycol, glycerol and butanediol.
The invention also provides a preparation method of the high-temperature-resistant electrothermal ink, which comprises the following preparation steps:
step one, uniformly mixing a dispersing agent and a high-temperature-resistant inorganic binder, then adding graphite, graphene and carbon nano tubes, then adding a filler, a temperature coefficient regulator and a diluent, and stirring for 10-20min under the condition of 500 plus 2000 r/min;
step two, carrying out ultrasonic treatment on the slurry stirred in the step one, wherein the ultrasonic frequency is 40-80kHz, and the ultrasonic time is 20-60 min;
grinding the slurry subjected to ultrasonic treatment by using a three-roll grinder for 3-5 times, wherein the gap between a feeding roll and a discharging roll is 5-7 mu m, and the gap between the discharging roll and the discharging roll is 3-5 mu m;
and step four, defoaming the ground slurry to prepare the high-temperature-resistant electrothermal ink for heating the non-combustible electronic cigarette.
In the first step, the stirring speed can be, but is not limited to, 500r/min, 800r/min, 1000r/min, 1200r/min, 1500r/min, 1800r/min, 2000r/min, and the stirring time can be, but is not limited to, 10min, 12min, 15min, 18min, 20 min.
In the second step, the ultrasonic frequency can be, but is not limited to, 40kHz, 50kHz, 60kHz, 70kHz, 80kHz, and the ultrasonic time can be, but is not limited to, 20min, 30min, 40min, 50min, 60 min.
In the third step, the gap between the feeding rollers can be, but is not limited to, 5 μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, and the gap between the discharging rollers can be, but is not limited to, 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm.
And in the fourth step, a centrifugal defoaming machine is adopted for defoaming, the rotating speed during defoaming is 1000-2000r/min, and the defoaming time is 3-5 min. Specifically, the rotating speed can be, but is not limited to, 1000r/min, 1200r/min, 1500r/min, 1800r/min, 2000r/min, and the defoaming time can be, but is not limited to, 3min, 3.5min, 4min, 4.5min, 5 min.
The invention has the beneficial effects that:
the invention solves the problems of high cost, high sintering temperature, linear heating, low thermal efficiency and environmental pollution of thick film paste for electronic cigarettes, the product is an aqueous system, only needs 500 ℃ for solidification, can be suitable for substrates such as microcrystalline glass, quartz glass, ceramics and the like, can be applied within 400 ℃ for a long time, and meets the use requirement of heating non-combustible electronic cigarettes;
according to the invention, the resistance value of the coating formed by the electrothermal ink is not easy to change in a high-temperature environment by adding the temperature coefficient regulator, and the coating formed by the electrothermal ink can be used for a long time at 400 ℃ by selecting the specific type of temperature coefficient regulator, specifically, the resistance value of the formed electrothermal coating is changed by less than 8.5% at 400 ℃ after the formed electrothermal coating is used for 1000 hours, and the conductivity is stable.
Detailed Description
In order to make the objects, technical solutions and technical effects of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and the embodiments described below are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art without making any creative effort in combination with the embodiments of the present invention belong to the protection scope of the present invention. Those whose specific conditions are not specified in the examples are carried out according to conventional conditions or conditions recommended by the manufacturer; the reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
In the description of the present invention, the term "and/or" describing an association relationship of associated objects means that there may be three relationships, for example, a and/or B, may mean: a alone, A and B together, and B alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the description of the present invention, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (a), b, and c", may each represent: a, b, c, a-b (i.e. a and b), a-c, b-c, or a-b-c, wherein a, b, and c can be single or multiple respectively.
It should be understood that the weight of the related components mentioned in the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, it is within the scope of the disclosure that the content of the related components is scaled up or down according to the embodiments of the present invention. Specifically, the weight described in the embodiments of the present invention may be a unit of mass known in the chemical field such as μ g, mg, g, kg, etc.
In addition, unless the context clearly uses otherwise, an expression of a word in the singular is to be understood as including the plural of the word. The terms "comprises" or "comprising" are intended to specify the presence of stated features, quantities, steps, operations, elements, portions, or combinations thereof, but are not intended to preclude the presence or addition of one or more other features, quantities, steps, operations, elements, portions, or combinations thereof.
In order to clearly understand the details of the above-described implementation and operation of the present invention for those skilled in the art and to significantly embody the advanced performance of the embodiments of the present invention, the above-described technical solution is illustrated by a plurality of embodiments below.
Example 1
A high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette comprises the following raw materials in parts by weight:
the temperature coefficient regulator is a mixture of copper oxide, yttrium oxide and manganese oxide according to the weight ratio of 1:1: 3.5.
Wherein the high-temperature resistant inorganic binder is a mixture of aluminum sol and aluminum dihydrogen phosphate according to the weight ratio of 1: 20.
Wherein the high-temperature resistant filler is a mixture of alumina powder and boron oxide according to the weight ratio of 1: 1.
The dispersing agent is a mixture of sodium lignosulphonate and dodecyl phenol polyoxyethylene ether in a weight ratio of 1: 1.
The preparation method of the high-temperature-resistant electrothermal ink for heating the non-combustible electronic cigarette comprises the following preparation steps:
step one, according to the weight ratio of the components, uniformly mixing a dispersing agent and a high-temperature-resistant inorganic binder, then adding graphite, graphene and single-walled carbon nanotubes, adding a filler, a temperature coefficient regulator and a diluent, and stirring for 20min at the condition of 1000 r/min;
step two, carrying out ultrasonic treatment on the slurry stirred in the step one by using a medical ultrasonic machine, wherein the ultrasonic frequency is 40kHz, and the ultrasonic time is 20 min;
grinding the slurry subjected to ultrasonic treatment by using a three-roll grinder for 5 times, wherein the gap between a feeding roll and a discharging roll is 6 microns, and the gap between the discharging roll and the feeding roll is 4 microns, and taking out;
and step four, defoaming the ground slurry by using a centrifugal defoaming machine, wherein the rotating speed during defoaming is 1000r/min, and the defoaming time is 3min, so that the high-temperature-resistant electrothermal ink for heating the non-combustible electronic cigarette is prepared.
The preparation method of the high-temperature-resistant electrothermal ink coating comprises the steps of printing the prepared high-temperature-resistant electrothermal ink on a quartz glass substrate by adopting a screen printing technology, and curing the ink coating by using a tunnel furnace, wherein the curing condition is that the ink coating is cured for 10min at 80 ℃, then cured for 10min at 150 ℃, and finally cured for 30min at 500 ℃, and the thickness of the cured ink coating is 25 mu m.
Example 2
A high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette comprises the following raw materials in parts by weight:
wherein the temperature coefficient regulator is a mixture of copper oxide, yttrium oxide and manganese oxide according to the weight ratio of 1:0.5: 3.
Wherein the high-temperature resistant inorganic binder is a mixture of aluminum chromium phosphate and aluminum dihydrogen phosphate according to a weight ratio of 8: 1.
Wherein the high-temperature resistant filler is a mixture of mica powder and boron nitride in a weight ratio of 1: 2.
Wherein the dispersing agent is a mixture of a naphthalenesulfonic acid formaldehyde condensate and octylphenol polyoxyethylene ether in a weight ratio of 1: 1.
The preparation method of the high-temperature-resistant electrothermal ink for heating the non-combustible electronic cigarette is the same as that of the embodiment 1.
The preparation method of the high-temperature resistant electrothermal ink coating is the same as that of the example 1.
Example 3
A high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette comprises the following raw materials in parts by weight:
wherein the temperature coefficient regulator is a mixture of copper oxide, yttrium oxide and manganese oxide according to the weight ratio of 1:2: 4.
Wherein the high-temperature resistant inorganic binder is aluminum chromium phosphate.
Wherein the high-temperature resistant filler is mullite.
Wherein the dispersant is a mixture of lignosulfonate and sodium cholate in a weight ratio of 1: 1.
The preparation method of the high-temperature-resistant electrothermal ink for heating the non-combustible electronic cigarette is the same as that of the embodiment 1.
The preparation method of the electrothermal ink coating is the same as that of the example 1.
The electrothermal ink coatings prepared in examples 1 to 3 were subjected to the following tests, and the test results are recorded in table 1.
Firstly, testing the sheet resistance of the coating;
secondly, after the coating is placed in an environment with the temperature of 400 ℃ for 1000 hours, the resistance change of the coating is tested and calculated.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. The high-temperature-resistant electrothermal ink for heating the non-combustible electronic cigarette is characterized by comprising the following raw materials in parts by weight:
the temperature coefficient regulator is at least one of copper oxide, manganese oxide, yttrium oxide and bismuth oxide.
2. The high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette according to claim 1, wherein the carbon nanotubes are at least one of single-walled carbon nanotubes and multi-walled carbon nanotubes.
3. The high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette according to claim 1, wherein the temperature coefficient regulator is a mixture of copper oxide, yttrium oxide and manganese oxide in a weight ratio of 1:0.5-2: 3-4.
4. The high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette according to claim 1, wherein the high-temperature-resistant inorganic binder is at least one of silica sol, alumina sol, titanium sol, aluminum phosphate, aluminum chromium phosphate, aluminum dihydrogen phosphate, calcium dihydrogen phosphate, and magnesium dihydrogen phosphate.
5. The high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette according to claim 1, wherein the high-temperature-resistant filler is at least one of alumina powder, boron oxide, silica micropowder, mica powder, talc, titanium dioxide, boron nitride, silicon carbide, mullite and cordierite.
6. The high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette according to claim 1, wherein the dispersant is at least one of lignosulfonate, sodium cholate, octylphenol polyoxyethylene ether, naphthalene sulfonic acid formaldehyde condensate, sodium dodecylbenzene sulfonate, cetyltrimethylammonium bromide, span, octadecenamine acetate, alkyl quaternary ammonium salt, aminopropylamine dioleate, polyaminoamide phosphate, polycaprolacton-polyethyleneimine block copolymer, and dodecylphenol polyoxyethylene ether.
7. The high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette according to claim 1, wherein the diluent is at least one of ethylene glycol, propylene glycol, glycerin, and butylene glycol.
8. The method for preparing a high-temperature resistant electrothermal ink for heating a non-combustible electronic cigarette according to any one of claims 1 to 7, comprising the steps of:
step one, uniformly mixing a dispersing agent and a high-temperature-resistant inorganic binder, then adding graphite, graphene and carbon nano tubes, then adding a filler, a temperature coefficient regulator and a diluent, and stirring for 10-20min under the condition of 500 plus 2000 r/min;
step two, carrying out ultrasonic treatment on the slurry stirred in the step one, wherein the ultrasonic frequency is 40-80kHz, and the ultrasonic time is 20-60 min;
grinding the slurry subjected to ultrasonic treatment by using a three-roll grinder for 3-5 times, wherein the gap between a feeding roll and a discharging roll is 5-7 mu m, and the gap between the discharging roll and the discharging roll is 3-5 mu m;
and step four, defoaming the ground slurry to prepare the high-temperature-resistant electrothermal ink for heating the non-combustible electronic cigarette.
9. The method for preparing the high-temperature-resistant electrothermal ink for heating a non-combustible electronic cigarette as recited in claim 8, wherein in the fourth step, a centrifugal defoaming machine is used for defoaming, the rotation speed during defoaming is 1000-2000r/min, and the defoaming time is 3-5 min.
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