WO2020253519A1 - 发热电子浆料组合物、发热电子浆料及其制备方法、电子烟发热体和电子烟 - Google Patents

发热电子浆料组合物、发热电子浆料及其制备方法、电子烟发热体和电子烟 Download PDF

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WO2020253519A1
WO2020253519A1 PCT/CN2020/093947 CN2020093947W WO2020253519A1 WO 2020253519 A1 WO2020253519 A1 WO 2020253519A1 CN 2020093947 W CN2020093947 W CN 2020093947W WO 2020253519 A1 WO2020253519 A1 WO 2020253519A1
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Prior art keywords
water
heat
generating electronic
heating
based carrier
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PCT/CN2020/093947
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English (en)
French (fr)
Inventor
王洪军
易长勇
薛雪波
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深圳麦克韦尔科技有限公司
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Application filed by 深圳麦克韦尔科技有限公司 filed Critical 深圳麦克韦尔科技有限公司
Priority to EP20826706.2A priority Critical patent/EP3959998A4/en
Priority to US17/615,935 priority patent/US20230404151A1/en
Publication of WO2020253519A1 publication Critical patent/WO2020253519A1/zh

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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10—Chemical features of tobacco products or tobacco substitutes
    • A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10—Chemical features of tobacco products or tobacco substitutes
    • A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/46—Shape or structure of electric heating means
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/70—Manufacture
    • 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
    • C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
    • C09D101/02—Cellulose; Modified cellulose
    • 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/20—Diluents or solvents
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/80—Processes for incorporating ingredients
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/20—Devices using solid inhalable precursors
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/013—Heaters using resistive films or coatings
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/017—Manufacturing methods or apparatus for heaters

Definitions

  • the present invention relates to the technical field of electronic materials, in particular to a heat-generating electronic paste composition, a heat-generating electronic paste and a preparation method thereof, an electronic cigarette heater and an electronic cigarette.
  • Electronic paste is a composite material that integrates the characteristics of multiple materials. It is the basic material for the manufacture of thick film components. It can be subdivided into many types according to different uses and sintering temperature, such as conductive paste and resistance paste. And high temperature, medium temperature, low temperature sintering slurry, etc. With the rapid development of the electronic information industry, the demand for electronic pastes is increasing. Among them, heating electronic pastes are widely used, and can be used in thick film resistors, resistor networks, hybrid integrated circuits, electronic cigarettes, fast electric kettles, windshields, showcases, special-purpose resistors, electrodes, etc.
  • a heat-generating electronic slurry composition comprising a water-based carrier and a functional phase, the water-based carrier comprising a water-soluble binder and water, and the functional phase comprising a conductive material.
  • a method for preparing heat-generating electronic paste includes the following steps:
  • the water-based carrier and the functional phase are mixed, and the second heating treatment is performed to obtain a heat generating electronic paste; wherein the functional phase includes a conductive material.
  • An electronic cigarette heating element which includes a base and a heating circuit formed on the base, and the heating circuit is made of the above heating electronic paste.
  • An electronic cigarette which includes the above electronic cigarette heating element.
  • Fig. 1 is a preparation flow chart of a heat generating electronic paste composition according to an embodiment
  • Fig. 2 is a preparation flow chart of an electronic cigarette heating element according to an embodiment.
  • the heat-generating electronic paste composition of one embodiment includes a water-based carrier and a functional phase, the water-based carrier includes a water-soluble binder and water, and the functional phase includes a conductive material.
  • the weight ratio of the water-based carrier to the functional phase is 1: (2-5). Within the above range, it is beneficial to promote the compatibility between the water-based carrier and the functional phase, and at the same time improve the heating effect .
  • the weight ratio of the water-soluble binder to water is (15-30):100.
  • the water-based carrier can have suitable viscosity and water retention, which is beneficial to the dispersion of the functional phase, while ensuring that the process requirements are met when processed into a heating circuit, and the heating effect is improved.
  • the water-soluble binder is at least one selected from modified starch, methyl cellulose, hydroxymethyl cellulose, and carboxymethyl cellulose.
  • the water-soluble binder is modified starch and methyl cellulose.
  • modified starch and methyl cellulose as the water-based binder can further optimize the microstructure of the water-based carrier, and achieve the simultaneous effect of the suspension and water retention of the water-based carrier.
  • weight ratio of modified starch to methyl cellulose is 1: (1 to 3).
  • modified starch refers to a substance obtained by modifying starch molecules by physical, chemical or enzymatic treatment. By introducing new functional groups on the starch molecule or changing the size of the starch molecule and the properties of starch granules, its properties can be changed. Further, the weight average molecular weight of the modified starch may be 10,000 to 80,000. Specifically, the modified starch includes at least one of pregelatinized starch, cross-linked starch, and etherified starch.
  • methyl cellulose is:
  • R is -H or -CH 3 .
  • the weight average molecular weight of methyl cellulose may be 20,000 to 100,000.
  • the conductive material is a substance with conductivity, and can be various metal materials, as long as it does not chemically react with water at room temperature.
  • the conductive material is at least one of stainless steel, nickel-chromium alloy, and iron-chromium aluminum alloy.
  • the conductive material is powder.
  • the functional phase further includes a surface modifier for surface modification of the conductive material to further improve the compatibility between the functional phase and the water-based carrier.
  • the surface modifier includes at least one of microcrystalline cellulose, hydroxymethyl cellulose, and carboxymethyl cellulose.
  • the above-mentioned surface modifiers can promote thorough mixing between the conductive material and the water-based carrier.
  • the weight ratio of the surface modifier to the conductive material is (3-8):100.
  • the heat-generating electronic paste composition further includes functional additives for improving the functionality of the heat-generating electronic paste, optimizing product performance, and prolonging the service life of the product.
  • the functional additive includes at least one of a thixotropic agent and a preservative.
  • the thixotropic agent is a functional additive for improving the thixotropy of the water-based carrier.
  • the thixotropic agent is at least one selected from hydrogenated castor oil, oleic acid and stearic acid. Further, based on 100 parts by weight of the water-based carrier, the content of the thixotropic agent is 0.3 to 1 part by weight.
  • the preservative is a functional additive for preventing mold and spoilage of the water-based carrier.
  • the preservative is at least one selected from sodium benzoate, sorbate, dehydroacetate and ammonium nitrate. Further, based on 100 parts by weight of the water-based carrier, the content of the preservative is 0.2 to 0.8 parts by weight.
  • a method for preparing heat-generating electronic paste includes the following steps:
  • S101 Mix the water-soluble binder with water, and perform the first heating treatment to obtain a water-based carrier.
  • the conditions of the first heat treatment include: a temperature of 80°C to 90°C, and a time of 4h to 6h.
  • the first heat treatment is performed under water bath conditions. Further, the first heating treatment is performed under agitation, and the rotation speed of the agitation may be 200 revolutions/minute to 400 revolutions/minute.
  • the conductive material and the surface modifier are mixed to obtain the functional phase. That is, the conductive material is mixed with the surface modifier to obtain the functional phase, and then the water-based carrier is mixed with the functional phase.
  • the surface modifier modifies the surface of the conductive material, so that the conductive material after surface modification has better compatibility when mixed with the water-based carrier.
  • the process of mixing the functional phase and the surface modifier can be carried out under stirring conditions, the stirring speed can be 200 rpm to 400 rpm, and the stirring time can be 4 h to 6 h.
  • the water-based carrier is mixed with the functional phase, then mixed with the functional additive, and then subjected to the second heating treatment.
  • the conditions of the second heat treatment include: a temperature of 80°C to 90°C, and a time of 6h to 8h.
  • the second heat treatment is performed under water bath conditions. Further, the second heating treatment is performed under agitation, and the rotation speed of the agitation can be 200 to 400 rpm.
  • the water-soluble binder and water are mixed to prepare a water-based carrier under suitable heating conditions, and then the obtained water-based carrier is mixed and reacted with the functional phase and optional functional additives to finally prepare the exothermic electronic paste material.
  • the heat generating electronic paste prepared by the above method.
  • the heat-generating electronic paste does not contain organic solvents, and will not produce pungent odors during the subsequent processing into a heat-generating circuit, thereby reducing environmental pollution and avoiding the health of operators.
  • the electronic cigarette heating element includes a base and a heating circuit formed on the base.
  • the heating circuit is made of the above heating electronic paste.
  • a preparation method of an electronic cigarette heating element includes the following steps:
  • the matrix is a porous ceramic matrix or a composite alumina ceramic matrix.
  • the conditions of screen printing include: the printing pressure is 0.1 MPa to 0.6 MPa.
  • the drying conditions include: a temperature of 80°C to 100°C, and a time of 30min to 45min.
  • the drying is performed in an electrothermal curing oven.
  • S203 Sintering the cured and dried matrix to obtain an electronic cigarette heating element.
  • the sintering conditions include: the temperature is 800° C. to 1200° C., and the time is 60 min to 120 min.
  • sintering is performed in a sintering furnace. After the sintering is completed, the cured heating electronic paste forms a heating circuit on the substrate.
  • the heating electronic paste does not contain organic solvents, there is no irritating smell, which improves the comfort of the operator and avoids damage to the operator
  • the body is healthy, and at the same time, additional cleaning procedures are omitted, thus significantly reducing production costs, energy saving and emission reduction.
  • An electronic cigarette which includes the above electronic cigarette heating element.
  • the modified starch is a pregelatinized starch, purchased from Shanghai Yuanju Biotechnology, the product number is Y0365, and the weight average molecular weight is 50,000.
  • Methyl cellulose was purchased from Gade Chemical, CAS: 9004-67-5, with a weight average molecular weight of 30,000.
  • Stainless steel powder was purchased from Aladdin, the product number is S118293.
  • Microcrystalline cellulose was purchased from Yuanye Biology, the product number is S25132.
  • Hydrogenated castor oil was purchased from Fangfu (Guangzhou) Advanced Materials, CAS: 8001-78-3.
  • Sodium benzoate was purchased from Aike Reagent, CAS: 532-32-1.
  • Examples 1 to 6 are used to illustrate the heating electronic paste and the preparation method thereof.
  • step (1) is : Add methyl cellulose to water at 85°C, the weight ratio of methyl cellulose to water is 20:100, and carry out the first heat treatment for 5 hours under the condition of stirring in a water bath at 85°C (stirring speed 250 rpm), over 200 After mesh sieving, a water-based carrier is obtained.
  • step (1) is: Add modified starch to 85°C water, the weight ratio of modified starch to water is 20:100, and carry out the first heating treatment for 5h under the condition of 85°C water bath stirring (stirring speed 250 rpm), after passing 200 mesh sieve A water-based carrier is obtained.
  • step (2) is: Pass the stainless steel powder through a 200-mesh sieve to obtain the functional phase.
  • step (3) is: according to water-based carrier and function
  • the phase weight ratio is 1:4, and then the second heating treatment is carried out for 7 hours under the condition of 85°C water bath stirring (stirring speed 250 revolutions/min), and the exothermic electronic slurry is obtained after passing through a 200 mesh sieve.
  • the heating electronic paste of this comparative example uses organic solvents, and the specific preparation process is as follows:
  • Examples 7-12 are used to illustrate the process of preparing an electronic cigarette heating element by using the heating electronic pastes of Examples 1-6.
  • the heat-generating electronic paste of Example 1 was screen-printed on the porous ceramic substrate at a temperature of 23-27°C, a humidity of 40-60, and a printing pressure of 0.5MPa, and then sent it into an electric curing furnace at 90°C Dry for 40 minutes to solidify the heating electronic paste, and finally send it into a sintering furnace, and sinter it at 1000-1020°C for 1 hour.
  • the cured heating electronic paste forms a heating circuit on the porous ceramic substrate to obtain an electronic cigarette heating element.
  • the heating element of the electronic cigarette is prepared by the method substantially the same as that of Embodiment 7, except that the heating electronic paste of Embodiments 2 to 6 is used to replace the heating electronic paste of Embodiment 1.
  • the heating element for electronic cigarettes was prepared by using substantially the same method as that of Example 7, except that the heating electronic paste of Comparative Example 1 was used instead of the heating electronic paste of Example 1.
  • the electric bridge meter was used to test the initial resistance of the electronic cigarette heating elements prepared in Examples 7-12 and Comparative Example 2 and the resistance after 1000 puffs. The results are listed in Table 1.
  • Example 7 1.019 1.108
  • Example 8 1.126 1.204
  • Example 9 1.098 1.136
  • Example 10 1.134 1.184
  • Example 11 1.158 1.209
  • Example 12 1.176 1.220 Comparative example 2 1.154 1.216

Abstract

一种发热电子浆料组合物、发热电子浆料及其制备方法、电子烟发热体和电子烟，该发热电子浆料组合物包括水基载体和功能相，该水基载体包括水溶性粘结剂和水，该功能相包括导电材料。该发热电子浆料组合物采用水基载体替代挥发性有机溶剂，在加工为发热线路的过程中能够避免产生刺激性气味，节能环保。

Description

发热电子浆料组合物、发热电子浆料及其制备方法、电子烟发热体和电子烟 技术领域
本发明涉及电子材料技术领域，特别是涉及一种发热电子浆料组合物、发热电子浆料及其制备方法、电子烟发热体和电子烟。
背景技术
电子浆料是一种集多项材料的特性为一身的复合材料，是制造厚膜元件的基础材料，按照用途、烧结温度等不同，可细分为很多种，如导体浆料、电阻浆料及高温、中温、低温烧结浆料等。随着电子信息产业的高速发展，电子浆料的需求日益旺盛。其中，发热电子浆料应用广泛，可用于厚膜电阻器、电阻网络、混合集成电路、电子烟、快速电加热水壶、挡风玻璃、橱窗、特殊用途的电阻器、电极等方面。
现有发热电子浆料多由松油醇作为有机溶剂将纤维素溶胀制得悬浮液，再与功能粉体混合，然后在基体上进行丝网印刷，固化，最后烧结，最终在基体上形成发热线路。然而，在丝网印刷和固化工序时，有机溶剂挥发产生刺激气味，既污染环境，也威胁操作人员的身体健康。为了减小气味，通常进行强排风，不仅增加了洁净成本，且仍然不能彻底根除刺激气味。
发明内容
基于此，有必要提供一种较为环保且有利于降低成本的发热电子浆料组合 物。
此外，还提供一种发热电子浆料及其制备方法、电子烟发热体和电子烟。
一种发热电子浆料组合物，所述组合物包括水基载体和功能相，所述水基载体包括水溶性粘结剂和水，所述功能相包括导电材料。
一种制备发热电子浆料的方法，该方法包括以下步骤：
将水溶性粘结剂与水混合，进行第一加热处理，得到水基载体；
将所述水基载体与功能相混合，进行第二加热处理，得到发热电子浆料；其中，所述功能相包括导电材料。
由上述方法制备得到的发热电子浆料。
一种电子烟发热体，该电子烟发热体包括基体和形成在所述基体上的发热线路，所述发热线路由上述发热电子浆料制成。
一种电子烟，该电子烟包括上述电子烟发热体。
本申请的一个或多个实施例的细节在下面的附图和描述中提出，本申请的其它特征、目的和优点将从说明书、附图及权利要求书变得明显。
附图说明
图1为一实施方式的发热电子浆料组合物的制备流程图；
图2为一实施方式的电子烟发热体的制备流程图。
为了更好地描述和说明这里公开的那些发明的实施例和/或示例，可以参考一副或多副附图。用于描述附图的附加细节或示例不应当被认为是对所公开的发明、目前描述的实施例和/或示例以及目前理解的这些发明的最佳模式中的任何一者的范围的限制。
具体实施方式
为了便于理解本发明，下面将参照相关附图对本发明进行更全面的描述。附图中给出了本发明的较佳的实施例。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。
一实施方式的发热电子浆料组合物，该组合物包括水基载体和功能相，水基载体包括水溶性粘结剂和水，功能相包括导电材料。
在其中一个实施例中，水基载体与功能相的重量比为1：(2～5)，在上述范围内，有利于促进水基载体与功能相之间的相容性，同时提高发热效果。
在其中一个实施例中，水溶性粘结剂与水的重量比为(15～30)：100。在上述范围内，能够使得水基载体具有适宜的粘度和保水性，既有利于功能相的分散，同时确保在加工为发热线路时满足工艺要求，改善发热效果。
在其中一个实施例中，水溶性粘结剂为选自改性淀粉、甲基纤维素、羟甲基纤维素和羧甲基纤维素中的至少一种。
在其中一个实施例中，水溶性粘结剂为改性淀粉和甲基纤维素。采用改性淀粉和甲基纤维素组合作为水性粘结剂能够进一步优化水基载体的微观结构，到达水基载体的悬浮性和保水性同步的效果。进一步地，改性淀粉与甲基纤维素的重量比为1：(1～3)。
具体地，改性淀粉是指利用物理、化学或酶法处理对淀粉分子进行改性得 到的物质。通过在淀粉分子上引入新的官能团或改变淀粉分子大小和淀粉颗粒性质，能够改变其特性。进一步地，改性淀粉的重均分子量可以为10000～80000。具体地，改性淀粉包括预糊化淀粉、交联淀粉和醚化淀粉的至少一种。
具体地，甲基纤维素的结构式为：
Figure PCTCN2020093947-appb-000001
其中，R为-H或-CH 3。进一步地，甲基纤维素的重均分子量可以为20000～100000。
导电材料为具有导电性的物质，可以为各种金属材料，只要满足其在常温下不与水发生化学反应即可。
在其中一个实施例中，导电材料为不锈钢、镍铬合金和铁铬铝合金中的至少一种。
在其中一个实施例中，导电材料为粉体。
在其中一个实施例中，功能相还包括表面改性剂，用于对导电材料进行表面改性，以进一步提高功能相与水基载体之间的相容性。
在其中一个实施例中，表面改性剂包括微晶纤维素、羟甲基纤维素和羧甲基纤维素中的至少一种。上述种类的表面改性剂能够促进导电材料与水基载体之间的充分混合。
在其中一个实施例中，表面改性剂与导电材料的重量比为(3～8)：100。
在其中一个实施例中，发热电子浆料组合物还包括功能添加剂，用于改善发热电子浆料的功能性，优化产品性能，延长产品的使用寿命。
在其中一个实施例中，功能添加剂包括触变剂和防腐剂中的至少一种。
具体地，触变剂为用于提高水基载体的触变性的功能添加剂。在其中一个实施例中，触变剂为选自氢化蓖麻油、油酸和硬脂酸中的至少一种。进一步地，以100重量份的水基载体为基准，触变剂的含量为0.3～1重量份。
具体地，防腐剂为用于防止水基载体发霉腐败的功能添加剂。在其中一个实施例中，防腐剂为选自苯甲酸钠、山梨酸盐、脱氢乙酸盐和硝酸铵中的至少一种。进一步地，以100重量份的水基载体为基准，防腐剂的含量为0.2～0.8重量份。
请参阅图1，一种制备发热电子浆料的方法，该方法包括以下步骤：
S101：将水溶性粘结剂与水混合，进行第一加热处理，得到水基载体。
在其中一个实施例中，第一加热处理的条件包括：温度为80℃～90℃，时间为4h～6h。
在其中一个实施例中，第一加热处理在水浴条件下进行。进一步地，第一加热处理在搅拌的条件下进行，搅拌的转速可以为200转/分钟～400转/分钟。
在其中一个实施例中，在将水基载体与功能相混合前，先将导电材料与表面改性剂混合，得到功能相。即，先将导电材料与表面改性剂混合，得到功能相，然后再将水基载体与功能相混合。导电材料与表面改性剂混合的过程中，表面改性剂对导电材料进行表面改性，使得表面改性后的导电材料在于水基载体混合时具有更好的相容性。为了促进表面改性，功能相与表面改性剂混合的过程可以在搅拌的条件下进行，搅拌的转速可以为200转/分钟～400转/分钟，搅拌的时间可以为4h～6h。
S102：将水基载体与功能相混合，进行第二加热处理，得到发热电子浆料。
在其中一个实施例中，将水基载体与功能相混合后，再与功能添加剂混合，然后再进行第二加热处理。
在其中一个实施例中，第二加热处理的条件包括：温度为80℃～90℃，时间为6h～8h。
在其中一个实施例中，第二加热处理在水浴条件下进行。进一步地，第二加热处理在搅拌的条件下进行，搅拌的转速可以为200转/分钟～400转/分钟。
在上述方法中，水溶性粘结剂、功能相、表面改性剂、功能添加剂等各原料的种类和用量参见上文描述，此处不再赘述。
通过上述方法，先将水溶性粘结剂与水混合在适宜的加热条件下制备水基载体，再将所得的水基载体与功能相和可选的功能添加剂混合反应，最终制备得到发热电子浆料。
由上述方法制备得到的发热电子浆料。该发热电子浆料不含有机溶剂，在后续加工为发热线路的过程中不会产生刺激性气味，减小环境污染，避免影响操作人员的身体健康。
一种电子烟发热体，该电子烟发热体包括基体和形成在基体上的发热线路，发热线路由上述发热电子浆料制成。
请参阅图2，一种电子烟发热体的制备方法，该方法包括以下步骤：
S201：将发热电子浆料丝网印刷于基体上，得到印刷有发热电子浆料的基体。
在其中一个实施例中，基体为多孔陶瓷基体或复合氧化铝陶瓷基体。
在其中一个实施例中，丝网印刷的条件包括：印刷压力为0.1MPa～0.6Mpa。
S202：将印刷有发热电子浆料的基体进行干燥以使发热电子浆料固化，得到固化干燥后的基体。
在其中一个实施例中，干燥的条件包括：温度为80℃～100℃，时间为30min～45min。
在其中一个实施例中，干燥在电热固化炉中进行。
S203：将固化干燥后的基体进行烧结，得到电子烟发热体。
在其中一个实施例中，烧结的条件包括：温度为800℃～1200℃，时间为60min～120min。
在其中一个实施例中，烧结在烧结炉中进行。烧结完成后，已固化的发热电子浆料在基体上形成发热线路。
在上述制备电子烟发热体的工艺过程中，尤其是在固化、烧结过程中，由于发热电子浆料不含有机溶剂，从而无刺激性气味产生，提高操作人员的工作舒适度，避免损伤操作人员的身体健康，同时省去了额外的洁净工序，从而明显降低生产成本，节能减排。
一种电子烟，该电子烟包括上述电子烟发热体。
下面通过具体的实施例进一步说明本发明，但不用于限制本发明。
实施例中，改性淀粉为预糊化淀粉，购自上海源聚生物科技，商品号为Y0365，重均分子量为50000。甲基纤维素购自盖德化工，CAS：9004-67-5，重均分子量为30000。不锈钢粉购自阿拉丁，商品号为S118293。微晶纤维素购自源叶生物，商品号为S25132。氢化蓖麻油购自方富(广州)高新材料，CAS：8001-78-3。苯甲酸钠购自艾科试剂，CAS：532-32-1。
实施例1～6用于说明发热电子浆料及其制备方法。
实施例1
(1)将改性淀粉与甲基纤维素按重量比为1:2加入85℃的水中，改性淀粉和甲基纤维素的总重量与水的重量比为20:100，在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行第一加热处理5h，过200目筛后得到水基载体。
(2)将不锈钢粉过200目筛，与微晶纤维素按重量比为100:6混合常温下 搅拌混合(搅拌转速250转/分钟)5h，得到功能相。
(3)按水基载体与功能相重量比为1:4混合，加入氢化蓖麻油和苯甲酸钠，以100重量份的水基载体为基准，氢化蓖麻油的用量为0.5重量份，苯甲酸钠的用量为0.5重量份，然后在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行第二加热处理7h，过200目筛后得到发热电子浆料。
实施例2
本实施例的发热电子浆料制备过程与实施例1大致相同，区别在于，本实施例的步骤(1)中，水溶性粘结剂仅采用甲基纤维素，具体地，步骤(1)为：将甲基纤维素加入85℃的水中，甲基纤维素与水的重量比为20:100，在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行第一加热处理5h，过200目筛后得到水基载体。
实施例3
本实施例的发热电子浆料制备过程与实施例1大致相同，区别在于，本实施例的步骤(1)中，水溶性粘结剂仅采用改性淀粉，具体地，步骤(1)为：将改性淀粉加入85℃的水中，改性淀粉与水的重量比为20:100，在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行第一加热处理5h，过200目筛后得到水基载体。
实施例4
本实施例的发热电子浆料制备过程与实施例1大致相同，区别在于，本实施例的步骤(2)中，不采用表面改性剂微晶纤维素，具体地，步骤(2)为：将不锈钢粉过200目筛，得到功能相。
实施例5
本实施例的发热电子浆料制备过程与实施例1大致相同，区别在于，本实 施例的步骤(3)中，不加入功能添加剂，具体地，步骤(3)为：按水基载体与功能相重量比为1:4混合，然后在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行第二加热处理7h，过200目筛后得到发热电子浆料。
实施例6
(1)将改性淀粉与甲基纤维素按重量比为1:4加入85℃的水中，改性淀粉和甲基纤维素的总重量与水的重量比为10:100，在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行第一加热处理5h，过200目筛后得到水基载体。
(2)将不锈钢粉过200目筛，与微晶纤维素按重量比为100:10混合常温下高速混合(搅拌转速250转/分钟)5h，得到功能相。
(3)按水基载体与功能相重量比为1:1混合，加入氢化蓖麻油和苯甲酸钠，以100重量份的水基载体为基准，氢化蓖麻油的用量为0.5重量份，苯甲酸钠的用量为0.5重量份，然后在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行第二加热处理7h，过200目筛后得到发热电子浆料。
对比例1
本对比例的发热电子浆料采用有机溶剂，具体制备过程为：
(1)将乙基纤维素与松油醇按重量比为1:25混合后，在90℃水浴搅拌(搅拌转速250转/分钟)条件下进行加热处理12h，过200目筛，得到有机载体。
(2)将不锈钢粉过200目筛，得到功能相。
(3)按有机载体与功能相重量比为1:4混合，在85℃水浴搅拌(搅拌转速250转/分钟)条件下进行加热处理7h，过200目筛后得到发热电子浆料。
实施例7～12用于说明采用实施例1～6的发热电子浆料制备电子烟发热体的过程。
实施例7
采用实施例1的发热电子浆料，在温度为23～27℃，湿度为40～60，印刷压力为0.5MPa条件下丝网印刷于多孔陶瓷基体上，然后送入电热固化炉中在90℃下干燥40min以使发热电子浆料固化，最后送入烧结炉中，在1000～1020℃下烧结1h，已固化的发热电子浆料在多孔陶瓷基体上形成发热线路，得到电子烟发热体。
制备过程中无刺激性气味产生，提高了操作人员的工作舒适度，避免损伤操作人员的身体健康，同时省去了额外的洁净工序，降低生产成本，节能减排。
实施例8～12
采用与实施例7大致相同的方法制备电子烟发热体，区别在于，分别采用实施例2～6的发热电子浆料替换实施例1的发热电子浆料。
制备过程中无刺激性气味产生，提高了操作人员的工作舒适度，避免损伤操作人员的身体健康，同时省去了额外的洁净工序，降低生产成本，节能减排。
对比例2
采用与实施例7大致相同的方法制备电子烟发热体，区别在于，采用对比例1的发热电子浆料替换实施例1的发热电子浆料。
制备过程中，由于有机溶剂挥发产生剧烈刺激性气味，威胁操作人员的身体健康，开启强排风后，刺激性气味仍不能彻底根除，且生产成本增大。
测试例
采用电桥仪测试实施例7～12和对比例2制备的电子烟发热体的初始电阻及抽吸1000口后的电阻，结果列于表1。
表1
  初始电阻(欧姆) 抽吸1000口后电阻(欧姆)
实施例7 1.019 1.108
实施例8 1.126 1.204
实施例9 1.098 1.136
实施例10 1.134 1.184
实施例11 1.158 1.209
实施例12 1.176 1.220
对比例2 1.154 1.216
由表1可见，本发明的电子烟发热体具有较低的电阻，且长时间使用下电阻无明显升高，证明采用本发明的发热电子浆料组合物制备的电子烟发热体具有良好的发热性能。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (20)

  1. 一种发热电子浆料组合物，所述发热电子浆料组合物包括水基载体和功能相，所述水基载体包括水溶性粘结剂和水，所述功能相包括导电材料。
  2. 根据权利要求1所述的发热电子浆料组合物，其特征在于，所述水基载体与所述功能相的重量比为1：(2～5)；和/或，
    所述水溶性粘结剂与水的重量比为(15～30)：100。
  3. 根据权利要求1所述的发热电子浆料组合物，其特征在于，所述水溶性粘结剂为选自改性淀粉、甲基纤维素、羟甲基纤维素和羧甲基纤维素中的至少一种。
  4. 根据权利要求3所述的发热电子浆料组合物，其特征在于，所述水溶性粘结剂为改性淀粉和甲基纤维素，所述改性淀粉与甲基纤维素的重量比为1：(1～3)。
  5. 根据权利要求4所述的发热电子浆料组合物，其特征在于，所述改性淀粉的重均分子量为10000～80000；和/或，
    所述甲基纤维素的重均分子量为20000～100000。
  6. 根据权利要求1所述的发热电子浆料组合物，其特征在于，所述导电材料为不锈钢、镍铬合金和铁铬铝合金中的至少一种。
  7. 根据权利要求1所述的发热电子浆料组合物，其特征在于，所述功能相还包括表面改性剂，所述表面改性剂包括微晶纤维素、羟甲基纤维素和羧甲基纤维素中的至少一种。
  8. 根据权利要求7所述的发热电子浆料组合物，其特征在于，所述表面改性剂与所述导电材料的重量比为(3～8)：100。
  9. 根据权利要求1所述的发热电子浆料组合物，其特征在于，所述组合物还 包括功能添加剂，所述功能添加剂包括触变剂和防腐剂中的至少一种。
  10. 根据权利要求9所述的发热电子浆料组合物，其特征在于，以100重量份的所述水基载体为基准，所述触变剂的含量为0.3～1重量份；和/或，
    以100重量份的水基载体为基准，防腐剂的含量为0.2～0.8重量份。
  11. 一种制备发热电子浆料的方法，所述方法包括以下步骤：
    将水溶性粘结剂与水混合，进行第一加热处理，得到水基载体；及
    将所述水基载体与功能相混合，进行第二加热处理，得到发热电子浆料；
    其中，所述功能相包括导电材料。
  12. 根据权利要求11所述的方法，其特征在于，所述第一加热处理的条件包括：温度为80℃～90℃，时间为4h～6h；和/或，
    所述水溶性粘结剂与水的重量比为(15～30)：100；和/或，
    所述水溶性粘结剂为选自改性淀粉、甲基纤维素、羟甲基纤维素和羧甲基纤维素中的至少一种。
  13. 根据权利要求11所述的方法，其特征在于，在将所述水基载体与功能相混合前，先将所述导电材料与表面改性剂混合，得到所述功能相；所述表面改性剂包括微晶纤维素、羟甲基纤维素和羧甲基纤维素中的至少一种。
  14. 根据权利要求13所述的方法，其特征在于，所述表面改性剂与所述导电材料的重量比为(3～8)：100。
  15. 根据权利要求11所述的方法，其特征在于，所述水基载体与所述功能相的重量比为1：(2～5)；和/或，
    所述第二加热处理的条件包括：温度为80℃～90℃，时间为6h～8h。
  16. 根据权利要求11所述的方法，其特征在于，所述导电材料为不锈钢、镍铬合金和铁铬铝合金中的至少一种。
  17. 根据权利要求11所述的方法，其特征在于，将所述水基载体与功能相混合后，再与功能添加剂混合，然后再进行所述第二加热处理；所述功能添加剂包括触变剂和防腐剂中的至少一种。
  18. 由权利要求11～17任意一项所述的制备发热电子浆料的方法制备得到的发热电子浆料。
  19. 一种电子烟发热体，所述电子烟发热体包括基体和形成在所述基体上的发热线路，所述发热线路由权利要求18所述的发热电子浆料制成。
  20. 一种电子烟，所述电子烟包括权利要求19所述的电子烟发热体。
PCT/CN2020/093947 2019-06-20 2020-06-02 发热电子浆料组合物、发热电子浆料及其制备方法、电子烟发热体和电子烟 WO2020253519A1 (zh)

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