WO2023155277A1 - Infrared shielding type eva hot melt adhesive film and preparation method therefor - Google Patents

Infrared shielding type eva hot melt adhesive film and preparation method therefor Download PDF

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Publication number
WO2023155277A1
WO2023155277A1 PCT/CN2022/084178 CN2022084178W WO2023155277A1 WO 2023155277 A1 WO2023155277 A1 WO 2023155277A1 CN 2022084178 W CN2022084178 W CN 2022084178W WO 2023155277 A1 WO2023155277 A1 WO 2023155277A1
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adhesive film
melt adhesive
agent
infrared shielding
parts
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PCT/CN2022/084178
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French (fr)
Chinese (zh)
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宾家荃
宾家齐
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广东汇齐新材料有限公司
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Publication of WO2023155277A1 publication Critical patent/WO2023155277A1/en

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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
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04—Homopolymers or copolymers of ethene
    • C09J123/08—Copolymers of ethene
    • C09J123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C09J123/0853—Vinylacetate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/35—Heat-activated
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/304—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C

Definitions

  • the invention relates to the technical field of EVA hot-melt adhesives, in particular to an infrared shielding EVA hot-melt adhesive film and a preparation method thereof.
  • EVA hot melt adhesive is a new type of synthetic adhesive made of ethylene-vinyl acetate thermoplastic polymer as the main material, and other polymer materials such as tackifiers, waxes, plasticizers, antioxidants, fillers, etc. by melting and blending. It is convenient for safe transportation and storage, low energy consumption, and easy operation.
  • the adhesive is softened and melted in a fluid state by heating to coat the bonding interface, and the bonding is realized by cooling and solidifying within a short time after being separated from the heat source.
  • the sun is the strongest infrared radiation source in nature, but in the production environment, the infrared radiation sources mainly include furnaces, molten metal and glass, strong infrared light sources, baking and heating equipment, etc.
  • the infrared radiation sources mainly include furnaces, molten metal and glass, strong infrared light sources, baking and heating equipment, etc.
  • infrared radiation sources such as furnaces, molten metal and glass, strong infrared light sources, baking and heating equipment, etc.
  • infrared radiation sources such as furnaces, molten metal and glass, strong infrared light sources, baking and heating equipment, etc.
  • Some special occupations are engaged in the above-mentioned work and are easily exposed to infrared rays. Exposure to infrared rays requires shielding and protection against infrared rays.
  • an infrared shielding EVA hot-melt adhesive film which improves the infrared shielding protection work of textiles by compounding the EVA hot-melt adhesive film with textiles, and also provides an infrared shielding EVA Preparation method of hot melt adhesive film.
  • An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
  • EVA main resin 60-80 parts; infrared shielding agent 10-30 parts; cooling agent 5-10 parts; silane coupling agent 8-15 parts; co-solvent 2-6 parts; inorganic flame retardant 0.1 part -1 part; 3 parts-10 parts of tackifier; 0.1 part-1 part of initiator; 0.01 part-1 part of antioxidant; wherein, the melting index of the EVA main resin is 200g/10min -300g/10min. EVA main resin with higher melting index is easy to wrap various materials, so that it has better dispersion performance.
  • the above-mentioned infrared shielding EVA hot melt adhesive film shields or absorbs infrared rays through the action of an infrared shielding agent, converts light energy into heat energy, and then through the action of a cooling agent, heat is separated from the surface or quickly dissipated to improve the quality of textiles.
  • Infrared shielding and protection work through the role of inorganic flame retardants, improve the flame retardant performance of the product; through the role of silane coupling agents, the silane coupling agent is interposed between EVA main resin and infrared shielding agent, cooling agent, inorganic resistance Between the fuel, a bonding layer of organic matrix-silane coupling agent-inorganic matrix is formed to improve the compatibility of various materials, and at the same time, it can improve the adhesive performance of the adhesive film and textile materials, and can greatly improve the high temperature resistance of EVA. .
  • the infrared shielding agent is one or more of polyaniline, copper sulfide, and pyreneimide.
  • the infrared shielding agent is composed of copper sulfide and polyaniline or pyreneimide with a mass ratio of 1: (4-5), wherein the copper sulfide is copper sulfide nanoparticles, copper sulfide nanospheres one or both.
  • Polyaniline can absorb infrared rays and convert light energy into heat energy.
  • the anion radical of pyreneimide has strong near-infrared absorption characteristics. Copper sulfide has a good infrared absorption effect. When combined with polyaniline or pyreneimide, Form two kinds of infrared absorption effects such as organic and inorganic.
  • the cooling agent is one or more of graphene oxide, graphene, and carbon nanotubes.
  • the heat dissipation agent is composed of graphene and carbon nanotubes with a mass ratio of 1:2, and the combination of the two forms a criss-cross heat dissipation system.
  • the silane coupling agent is one or more of vinylsilane, aminosilane, and methacryloxysilane.
  • the co-solvent is one or more of ethylene glycol monobutyl ether, propylene glycol monobutyl ether, diethylene glycol monobutyl ether, and butanol. Improve the dispersion performance of cooling agent or inorganic flame retardant.
  • the inorganic flame retardant is one or both of magnesium hydroxide and aluminum hydroxide;
  • the tackifier is one or both of rosin resin, carbon pentahydrogenated petroleum resin, and terpene resin. more than one species.
  • the mass ratio of the EVA host resin to the infrared shielding agent and silane coupling agent is 1:(0.2-0.4):(0.1-0.2). Further preferably, the mass ratio of the EVA host resin to the infrared shielding agent and silane coupling agent is 1:0.3:0.2.
  • the initiator is one or both of benzoyl peroxide, diacetyl peroxide, tert-butyl peroxybenzoate, 2,4-dichlorobenzoyl peroxide and lauryl peroxide.
  • the antioxidant is tetrakis [ ⁇ -(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester, three [2.4-di-tert-butylphenyl] phosphite, One or more of 4,4'-thiobis(6-tert-butyl-3-methylphenol).
  • a method for preparing an infrared shielding EVA hot-melt adhesive film comprising the following preparation steps.
  • the preparation method of the infrared shielding EVA hot-melt adhesive film includes the following preparation steps.
  • the infrared-shielding EVA hot-melt adhesive film of the present invention shields or absorbs infrared rays through the action of an infrared shielding agent, converts light energy into heat energy, and then through the action of a cooling agent, heat is separated on the surface or quickly dissipated, thereby improving the quality of textiles.
  • Infrared shielding and protection work through the role of inorganic flame retardants, improve the flame retardant performance of the product; through the role of silane coupling agents, the silane coupling agent is interposed between EVA main resin and infrared shielding agent, cooling agent, inorganic resistance Between the fuel, a bonding layer of organic matrix-silane coupling agent-inorganic matrix is formed to improve the compatibility of various materials, and at the same time, it can improve the adhesive performance of the adhesive film and textile materials, and can greatly improve the high temperature resistance of EVA. .
  • the melt index of the EVA main resin is 200g/10min;
  • the infrared shielding agent is composed of copper sulfide and polyaniline or pyreneimide with a mass ratio of 1:4, and the copper sulfide is copper sulfide Nanoparticles;
  • the cooling agent is composed of graphene and carbon nanotubes with a mass ratio of 1:2;
  • the silane coupling agent is vinylsilane;
  • the co-solvent is composed of ethylene glycol monobutyl ether and butanol with a mass ratio of 1:1 ;
  • the inorganic flame retardant is magnesium hydroxide;
  • the tackifier is rosin resin;
  • the initiator is benzoyl peroxide;
  • the antioxidant is tetrakis[ ⁇ -(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester.
  • An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
  • EVA main resin 60 parts of EVA main resin; 10 parts of infrared shielding agent; 5 parts of cooling agent; 8 parts of silane coupling agent; 2 parts of cosolvent; 0.1 part of inorganic flame retardant; 3 parts of tackifier; share.
  • the preparation method of the infrared shielding type EVA hot melt adhesive film comprises the following preparation steps.
  • An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
  • the preparation method of the infrared shielding type EVA hot melt adhesive film comprises the following preparation steps.
  • An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
  • EVA main resin 80 parts of EVA main resin; 30 parts of infrared shielding agent; 10 parts of cooling agent; 15 parts of silane coupling agent; 6 parts of cosolvent; 1 part of inorganic flame retardant; 10 parts of tackifier; share.
  • the preparation method of the infrared shielding type EVA hot melt adhesive film comprises the following preparation steps.
  • Example 1 the EVA hot-melt adhesive film of Comparative Example 1 does not contain a cooling agent.
  • Other ingredients and preparation methods are the same as in Example 1, and will not be repeated here.
  • Example 2 Different from Example 1, the EVA hot-melt adhesive film of Comparative Example 2 does not contain co-solvent. Other ingredients and preparation methods are the same as in Example 1, and will not be repeated here.
  • melt index of the EVA main resin in the EVA hot-melt adhesive film of Comparative Example 3 is 100 g/10min.
  • Other ingredients and preparation methods are the same as in Example 1, and will not be repeated here.
  • the EVA hot-melt adhesive film of embodiment and comparative example is compounded with textile, and the thickness of adhesive film is 0.2mm, carries out following test, and heat resistance test standard is HG/T 5052-2016; the thermal conductivity test standard is GB/T 10295-2008.
  • the transmittance (NIR) of the sample in the near-infrared region was measured by a U4110 spectrophotometer of Hitachi, Japan, and then calculated.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

Disclosed are an infrared shielding type EVA hot melt adhesive film and a preparation method therefor. The hot melt adhesive film comprises 60-80 parts of an EVA main body resin; 10-30 parts of an infrared shielding agent; 5-10 parts of a heat dissipation agent; 8-15 parts of a silane coupling agent; 2-6 parts of cosolvent; 0.1-1 parts of an inorganic flame retardant; 3-10 parts of a tackifier; 0.1-1 parts of an initiator; and 0.01-1 parts of an antioxidant. By means of the action of the infrared shielding agent, infrared rays are shielded or absorbed and light energy is converted into thermal energy, then the thermal energy is isolated on a surface by means of the action of the heat dissipation agent, and shielding and protection against infrared rays are improved; the flame retardancy of a product is improved by means of the action of the inorganic flame retardant; by means of the action of the silane coupling agent, the silane coupling agent is sandwiched between the EVA main body resin and the infrared shielding agent, an organic substrate-silane coupling agent-inorganic substrate bonded layer is formed, and the compatibility of each material is improved.

Description

一种红外屏蔽型EVA热熔胶膜及其制备方法A kind of infrared shielding type EVA hot-melt adhesive film and preparation method thereof
相关申请的交叉引用。Cross-references to related applications.
本申请要求于2022年2月15日提交中国专利局，申请号为202210139079.0，发明名称为“一种红外屏蔽型EVA热熔胶膜及其制备方法”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。This application claims the priority of the Chinese patent application submitted to the China Patent Office on February 15, 2022, the application number is 202210139079.0, and the invention title is "An infrared shielding EVA hot-melt adhesive film and its preparation method", the entire content of which Incorporated in this application by reference.
技术领域technical field
本发明涉及EVA热熔胶技术领域，尤其涉及一种红外屏蔽型EVA热熔胶膜及其制备方法。The invention relates to the technical field of EVA hot-melt adhesives, in particular to an infrared shielding EVA hot-melt adhesive film and a preparation method thereof.
背景技术Background technique
EVA热熔胶是以乙烯-醋酸乙烯热塑性聚合物为主体材料，与增粘剂、蜡类、增塑剂、抗氧剂、填料等其它高分子材料通过熔融共混合成的新型合成胶粘剂。它运输安全贮存便利，耗能较低，操作简易，利用加热的方法使胶粘剂软化熔融处于流态对粘接界面进行涂布，在脱离热源的很短时间内借冷却固化即实现粘接。EVA hot melt adhesive is a new type of synthetic adhesive made of ethylene-vinyl acetate thermoplastic polymer as the main material, and other polymer materials such as tackifiers, waxes, plasticizers, antioxidants, fillers, etc. by melting and blending. It is convenient for safe transportation and storage, low energy consumption, and easy operation. The adhesive is softened and melted in a fluid state by heating to coat the bonding interface, and the bonding is realized by cooling and solidifying within a short time after being separated from the heat source.
自然界的红外线辐射源以太阳为最强，但在生产环境中，主要以熔炉、熔融态金属和玻璃、强红外线光源、烘烤和加热设备等为主的红外线辐射源，一些特殊职业从事上述的工作，容易接触到红外线，因此，特殊职业工作者长期接触红外线需要对红外线进行屏蔽防护工作。The sun is the strongest infrared radiation source in nature, but in the production environment, the infrared radiation sources mainly include furnaces, molten metal and glass, strong infrared light sources, baking and heating equipment, etc. Some special occupations are engaged in the above-mentioned Work, it is easy to be exposed to infrared rays, therefore, workers in special occupations who are exposed to infrared rays for a long time need to shield and protect infrared rays.
技术问题technical problem
在生产环境中，主要以熔炉、熔融态金属和玻璃、强红外线光源、烘烤和加热设备等为主的红外线辐射源，一些特殊职业从事上述的工作，容易接触到红外线，特殊职业工作者长期接触红外线需要对红外线进行屏蔽防护工作。In the production environment, there are mainly infrared radiation sources such as furnaces, molten metal and glass, strong infrared light sources, baking and heating equipment, etc. Some special occupations are engaged in the above-mentioned work and are easily exposed to infrared rays. Exposure to infrared rays requires shielding and protection against infrared rays.
技术解决方案technical solution
根据本申请的各种实施例，提供一种红外屏蔽型EVA热熔胶膜，其通过将EVA热熔胶膜与纺织品复合，提高纺织品的红外线的屏蔽防护工作，还提供一种红外屏蔽型EVA热熔胶膜的制备方法。According to various embodiments of the present application, an infrared shielding EVA hot-melt adhesive film is provided, which improves the infrared shielding protection work of textiles by compounding the EVA hot-melt adhesive film with textiles, and also provides an infrared shielding EVA Preparation method of hot melt adhesive film.
一种红外屏蔽型EVA热熔胶膜，包括如下重量份的组分。An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
EVA主体树脂 60份-80份；红外线屏蔽剂10份-30份；散热剂5份-10份；硅烷偶联剂8份-15份；助溶剂2份-6份；无机阻燃剂0.1份-1份；增粘剂3份-10份；引发剂0.1份-1份；抗氧化剂0.01份-1份；其中，所述EVA主体树脂的的熔指为200g/10min -300g/10min。熔指较高的EVA主体树脂容易对各物料进行包裹，使其分散性能更好。EVA main resin 60-80 parts; infrared shielding agent 10-30 parts; cooling agent 5-10 parts; silane coupling agent 8-15 parts; co-solvent 2-6 parts; inorganic flame retardant 0.1 part -1 part; 3 parts-10 parts of tackifier; 0.1 part-1 part of initiator; 0.01 part-1 part of antioxidant; wherein, the melting index of the EVA main resin is 200g/10min -300g/10min. EVA main resin with higher melting index is easy to wrap various materials, so that it has better dispersion performance.
上述的红外屏蔽型EVA热熔胶膜通过红外线屏蔽剂的作用，将红外线屏蔽或者吸收，将光能转为热能，再通过散热剂的作用，将热量隔着在表面或快速散开，提高纺织品的红外线的屏蔽防护工作；通过无机阻燃剂的作用，提高产品的阻燃性能；通过硅烷偶联剂的作用，使硅烷偶联剂介于EVA主体树脂与红外线屏蔽剂、散热剂、无机阻燃剂之间，形成有机基体-硅烷偶联剂-无机基体的结合层，提高各物料的相容性，同时能够改善胶膜与纺织品材料的粘合性能，能够大大地提高EVA的耐高温性能。The above-mentioned infrared shielding EVA hot melt adhesive film shields or absorbs infrared rays through the action of an infrared shielding agent, converts light energy into heat energy, and then through the action of a cooling agent, heat is separated from the surface or quickly dissipated to improve the quality of textiles. Infrared shielding and protection work; through the role of inorganic flame retardants, improve the flame retardant performance of the product; through the role of silane coupling agents, the silane coupling agent is interposed between EVA main resin and infrared shielding agent, cooling agent, inorganic resistance Between the fuel, a bonding layer of organic matrix-silane coupling agent-inorganic matrix is formed to improve the compatibility of various materials, and at the same time, it can improve the adhesive performance of the adhesive film and textile materials, and can greatly improve the high temperature resistance of EVA. .
优选地，所述红外线屏蔽剂为聚苯胺、硫化铜、芘酰亚胺中的一种或两种以上。Preferably, the infrared shielding agent is one or more of polyaniline, copper sulfide, and pyreneimide.
优选地，所述红外线屏蔽剂由质量比为1：（4-5）的硫化铜与聚苯胺或芘酰亚胺所组成，其中，所述硫化铜为硫化铜纳米颗粒、硫化铜纳米球中的一种或两种。聚苯胺能够对红外线吸收，将光能转化为热能，芘酰亚胺的阴离子自由基具有强烈的近红外吸收特点，硫化铜具有较好的红外线吸收效果，与聚苯胺或芘酰亚胺配合，形成有机和无机等两种红外线吸收功效。Preferably, the infrared shielding agent is composed of copper sulfide and polyaniline or pyreneimide with a mass ratio of 1: (4-5), wherein the copper sulfide is copper sulfide nanoparticles, copper sulfide nanospheres one or both. Polyaniline can absorb infrared rays and convert light energy into heat energy. The anion radical of pyreneimide has strong near-infrared absorption characteristics. Copper sulfide has a good infrared absorption effect. When combined with polyaniline or pyreneimide, Form two kinds of infrared absorption effects such as organic and inorganic.
优选地，所述散热剂为氧化石墨烯、石墨烯、碳纳米管中的一种或两种以上。进一步优选地，所述散热剂由质量比为1:2的石墨烯、碳纳米管组成，通过两者结合，形成横纵交错的散热体系。Preferably, the cooling agent is one or more of graphene oxide, graphene, and carbon nanotubes. Further preferably, the heat dissipation agent is composed of graphene and carbon nanotubes with a mass ratio of 1:2, and the combination of the two forms a criss-cross heat dissipation system.
优选地，所述硅烷偶联剂为乙烯基硅烷、氨基硅烷、甲基丙烯酰氧基硅烷中的一种或两种以上。Preferably, the silane coupling agent is one or more of vinylsilane, aminosilane, and methacryloxysilane.
优选地，所述助溶剂为乙二醇单丁醚、丙二醇单丁醚、二乙二醇单丁醚、丁醇中的一种或两种以上。提高散热剂或者无机阻燃剂的分散性能。Preferably, the co-solvent is one or more of ethylene glycol monobutyl ether, propylene glycol monobutyl ether, diethylene glycol monobutyl ether, and butanol. Improve the dispersion performance of cooling agent or inorganic flame retardant.
优选地，所述无机阻燃剂为氢氧化镁、氢氧化铝中的一种或两种；所述增粘剂为松香树脂、碳五加氢石油树脂、萜烯树脂中的一种或者两种以上。Preferably, the inorganic flame retardant is one or both of magnesium hydroxide and aluminum hydroxide; the tackifier is one or both of rosin resin, carbon pentahydrogenated petroleum resin, and terpene resin. more than one species.
优选地，所述EVA主体树脂与所述红外线屏蔽剂、硅烷偶联剂的质量比为1：（0.2-0.4）：（0.1-0.2）。进一步优选地，所述EVA主体树脂与所述红外线屏蔽剂、硅烷偶联剂的质量比为1：0.3：0.2。Preferably, the mass ratio of the EVA host resin to the infrared shielding agent and silane coupling agent is 1:(0.2-0.4):(0.1-0.2). Further preferably, the mass ratio of the EVA host resin to the infrared shielding agent and silane coupling agent is 1:0.3:0.2.
优选地，所述引发剂为过氧化苯甲酰、过氧化二乙酰、过氧化苯甲酸叔丁酯、2,4-二氯过氧化苯甲酰、过氧化十二酰中的一种或者两种以上；所述抗氧剂为四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯、三[2.4-二叔丁基苯基]亚磷酸酯、4,4'-硫代双(6-叔丁基-3-甲基苯酚）中的一种或者两种以上。Preferably, the initiator is one or both of benzoyl peroxide, diacetyl peroxide, tert-butyl peroxybenzoate, 2,4-dichlorobenzoyl peroxide and lauryl peroxide. more than one species; the antioxidant is tetrakis [β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester, three [2.4-di-tert-butylphenyl] phosphite, One or more of 4,4'-thiobis(6-tert-butyl-3-methylphenol).
一种红外屏蔽型EVA热熔胶膜的制备方法，包括如下制备步骤。A method for preparing an infrared shielding EVA hot-melt adhesive film, comprising the following preparation steps.
S1：将EVA主体树脂、硅烷偶联剂、助溶剂、无机阻燃剂、引发剂、抗氧化剂和增粘剂加入到高速混合机中高速搅拌混合，边搅拌边加入红外线屏蔽剂和散热剂，混合均匀，得到混合物料。S1: Add EVA main resin, silane coupling agent, co-solvent, inorganic flame retardant, initiator, antioxidant and tackifier to a high-speed mixer and mix at high speed, and add infrared shielding agent and cooling agent while stirring. Mix evenly to obtain a mixed material.
S2：将混合物料投入螺杆挤出机中熔融挤出，经延流、冷却、牵引及收卷的步骤，得到红外屏蔽型EVA热熔胶膜。S2: Put the mixed material into the screw extruder to melt and extrude, and go through the steps of spreading, cooling, pulling and winding to obtain an infrared shielding EVA hot-melt adhesive film.
优选地，该红外屏蔽型EVA热熔胶膜的制备方法包括如下制备步骤。Preferably, the preparation method of the infrared shielding EVA hot-melt adhesive film includes the following preparation steps.
S1：将EVA主体树脂、硅烷偶联剂、助溶剂、无机阻燃剂、引发剂、抗氧化剂和增粘剂加入到高速混合机中高速搅拌混合，混合20min-40min后，边搅拌边加入红外线屏蔽剂和散热剂，混合均匀30min-40min，得到混合物料。S1: Add EVA main resin, silane coupling agent, co-solvent, inorganic flame retardant, initiator, antioxidant and tackifier to a high-speed mixer and mix at high speed. After mixing for 20min-40min, add infrared rays while stirring The shielding agent and cooling agent are mixed uniformly for 30min-40min to obtain the mixed material.
S2：将混合物料投入螺杆挤出机中在120℃-140℃下熔融挤出，经延流、冷却、牵引及收卷的步骤，得到红外屏蔽型EVA热熔胶膜。S2: Put the mixed material into a screw extruder and melt and extrude it at 120°C-140°C. After the steps of casting, cooling, drawing and winding, an infrared shielding EVA hot-melt adhesive film is obtained.
有益效果Beneficial effect
本发明的红外屏蔽型EVA热熔胶膜通过红外线屏蔽剂的作用，将红外线屏蔽或者吸收，将光能转为热能，再通过散热剂的作用，将热量隔在表面或快速散开，提高纺织品的红外线的屏蔽防护工作；通过无机阻燃剂的作用，提高产品的阻燃性能；通过硅烷偶联剂的作用，使硅烷偶联剂介于EVA主体树脂与红外线屏蔽剂、散热剂、无机阻燃剂之间，形成有机基体-硅烷偶联剂-无机基体的结合层，提高各物料的相容性，同时能够改善胶膜与纺织品材料的粘合性能，能够大大地提高EVA的耐高温性能。The infrared-shielding EVA hot-melt adhesive film of the present invention shields or absorbs infrared rays through the action of an infrared shielding agent, converts light energy into heat energy, and then through the action of a cooling agent, heat is separated on the surface or quickly dissipated, thereby improving the quality of textiles. Infrared shielding and protection work; through the role of inorganic flame retardants, improve the flame retardant performance of the product; through the role of silane coupling agents, the silane coupling agent is interposed between EVA main resin and infrared shielding agent, cooling agent, inorganic resistance Between the fuel, a bonding layer of organic matrix-silane coupling agent-inorganic matrix is formed to improve the compatibility of various materials, and at the same time, it can improve the adhesive performance of the adhesive film and textile materials, and can greatly improve the high temperature resistance of EVA. .
本发明的实施方式Embodiments of the present invention
为了便于理解本发明，下面将对本发明进行更全面的描述。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。In order to facilitate the understanding of the present invention, the following will describe the present invention more fully. However, the present invention can be embodied in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.
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。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention.
以下实施例中若无特别说明，EVA主体树脂的的熔指为200g/10min；红外线屏蔽剂由质量比为1：4的硫化铜与聚苯胺或芘酰亚胺所组成，硫化铜为硫化铜纳米颗粒；散热剂由质量比为1:2的石墨烯、碳纳米管组成；硅烷偶联剂为乙烯基硅烷；助溶剂由质量比为1:1的乙二醇单丁醚与丁醇组成；无机阻燃剂为氢氧化镁；增粘剂为松香树脂；引发剂为过氧化苯甲酰；抗氧剂为四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯。Unless otherwise specified in the following examples, the melt index of the EVA main resin is 200g/10min; the infrared shielding agent is composed of copper sulfide and polyaniline or pyreneimide with a mass ratio of 1:4, and the copper sulfide is copper sulfide Nanoparticles; the cooling agent is composed of graphene and carbon nanotubes with a mass ratio of 1:2; the silane coupling agent is vinylsilane; the co-solvent is composed of ethylene glycol monobutyl ether and butanol with a mass ratio of 1:1 ; The inorganic flame retardant is magnesium hydroxide; the tackifier is rosin resin; the initiator is benzoyl peroxide; the antioxidant is tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester.
实施例1。Example 1.
一种红外屏蔽型EVA热熔胶膜，包括如下重量份的组分。An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
EVA主体树脂 60份；红外线屏蔽剂10份；散热剂5份；硅烷偶联剂8份；助溶剂2份；无机阻燃剂0.1份；增粘剂3份；引发剂0.1份；抗氧化剂0.01份。60 parts of EVA main resin; 10 parts of infrared shielding agent; 5 parts of cooling agent; 8 parts of silane coupling agent; 2 parts of cosolvent; 0.1 part of inorganic flame retardant; 3 parts of tackifier; share.
该红外屏蔽型EVA热熔胶膜的制备方法包括如下制备步骤。The preparation method of the infrared shielding type EVA hot melt adhesive film comprises the following preparation steps.
S1：将EVA主体树脂、硅烷偶联剂、助溶剂、无机阻燃剂、引发剂、抗氧化剂和增粘剂加入到高速混合机中高速搅拌混合，混合20min后，边搅拌边加入红外线屏蔽剂和散热剂，混合均匀30min，得到混合物料。S1: Add EVA main resin, silane coupling agent, co-solvent, inorganic flame retardant, initiator, antioxidant and tackifier to a high-speed mixer and mix at high speed. After mixing for 20 minutes, add infrared shielding agent while stirring and cooling agent, mixed evenly for 30 minutes to obtain a mixed material.
S2：将混合物料投入螺杆挤出机中在120℃下熔融挤出，经延流、冷却、牵引及收卷的步骤，得到红外屏蔽型EVA热熔胶膜。S2: put the mixed material into a screw extruder and melt and extrude it at 120°C, and go through the steps of spreading, cooling, pulling and winding to obtain an infrared shielding EVA hot-melt adhesive film.
实施例2。Example 2.
一种红外屏蔽型EVA热熔胶膜，包括如下重量份的组分。An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
EVA主体树脂 70份；红外线屏蔽剂20份；散热剂7份；硅烷偶联剂12份；助溶剂4份；无机阻燃剂0.5份；增粘剂7份；引发剂0.5份；抗氧化剂0.5份。70 parts of EVA main resin; 20 parts of infrared shielding agent; 7 parts of cooling agent; 12 parts of silane coupling agent; 4 parts of cosolvent; 0.5 parts of inorganic flame retardant; share.
该红外屏蔽型EVA热熔胶膜的制备方法包括如下制备步骤。The preparation method of the infrared shielding type EVA hot melt adhesive film comprises the following preparation steps.
S1：将EVA主体树脂、硅烷偶联剂、助溶剂、无机阻燃剂、引发剂、抗氧化剂和增粘剂加入到高速混合机中高速搅拌混合，混合20min后，边搅拌边加入红外线屏蔽剂和散热剂，混合均匀30min，得到混合物料。S1: Add EVA main resin, silane coupling agent, co-solvent, inorganic flame retardant, initiator, antioxidant and tackifier to a high-speed mixer and mix at high speed. After mixing for 20 minutes, add infrared shielding agent while stirring and cooling agent, mixed evenly for 30 minutes to obtain a mixed material.
S2：将混合物料投入螺杆挤出机中在120℃下熔融挤出，经延流、冷却、牵引及收卷的步骤，得到红外屏蔽型EVA热熔胶膜。S2: put the mixed material into a screw extruder and melt and extrude it at 120°C, and go through the steps of spreading, cooling, pulling and winding to obtain an infrared shielding EVA hot-melt adhesive film.
实施例3。Example 3.
一种红外屏蔽型EVA热熔胶膜，包括如下重量份的组分。An infrared shielding EVA hot-melt adhesive film comprises the following components in parts by weight.
EVA主体树脂80份；红外线屏蔽剂30份；散热剂10份；硅烷偶联剂15份；助溶剂6份；无机阻燃剂1份；增粘剂10份；引发剂1份；抗氧化剂1份。80 parts of EVA main resin; 30 parts of infrared shielding agent; 10 parts of cooling agent; 15 parts of silane coupling agent; 6 parts of cosolvent; 1 part of inorganic flame retardant; 10 parts of tackifier; share.
该红外屏蔽型EVA热熔胶膜的制备方法包括如下制备步骤。The preparation method of the infrared shielding type EVA hot melt adhesive film comprises the following preparation steps.
S1：将EVA主体树脂、硅烷偶联剂、助溶剂、无机阻燃剂、引发剂、抗氧化剂和增粘剂加入到高速混合机中高速搅拌混合，混合20min后，边搅拌边加入红外线屏蔽剂和散热剂，混合均匀30min，得到混合物料。S1: Add EVA main resin, silane coupling agent, co-solvent, inorganic flame retardant, initiator, antioxidant and tackifier to a high-speed mixer and mix at high speed. After mixing for 20 minutes, add infrared shielding agent while stirring and cooling agent, mixed evenly for 30 minutes to obtain a mixed material.
S2：将混合物料投入螺杆挤出机中在120℃下熔融挤出，经延流、冷却、牵引及收卷的步骤，得到红外屏蔽型EVA热熔胶膜。S2: put the mixed material into a screw extruder and melt and extrude it at 120°C, and go through the steps of spreading, cooling, pulling and winding to obtain an infrared shielding EVA hot-melt adhesive film.
对比例1。Comparative example 1.
与实施例1不同的是，对比例1的EVA热熔胶膜中不含散热剂。其他成分和制备方法与实施例1相同，在此不再赘述。Different from Example 1, the EVA hot-melt adhesive film of Comparative Example 1 does not contain a cooling agent. Other ingredients and preparation methods are the same as in Example 1, and will not be repeated here.
对比例2。Comparative example 2.
与实施例1不同的是，对比例2的EVA热熔胶膜中不含助溶剂。其他成分和制备方法与实施例1相同，在此不再赘述。Different from Example 1, the EVA hot-melt adhesive film of Comparative Example 2 does not contain co-solvent. Other ingredients and preparation methods are the same as in Example 1, and will not be repeated here.
对比例3。Comparative example 3.
与实施例1不同的是，对比例3的EVA热熔胶膜中EVA主体树脂的的熔指为100 g/10min。其他成分和制备方法与实施例1相同，在此不再赘述。Different from Example 1, the melt index of the EVA main resin in the EVA hot-melt adhesive film of Comparative Example 3 is 100 g/10min. Other ingredients and preparation methods are the same as in Example 1, and will not be repeated here.
性能测试。Performance Testing.
对实施例和对比例的EVA热熔胶膜与纺织品复合，胶膜的厚度为0.2mm，进行如下测试，耐热性测试标准为HG∕T 5052-2016；导热系数测试标准为GB/T 10295-2008。样品在近红外区的透过率(NIR)由日本日立公司的U4110型分光光度计测试得到数据，经计算得到。The EVA hot-melt adhesive film of embodiment and comparative example is compounded with textile, and the thickness of adhesive film is 0.2mm, carries out following test, and heat resistance test standard is HG/T 5052-2016; the thermal conductivity test standard is GB/T 10295-2008. The transmittance (NIR) of the sample in the near-infrared region was measured by a U4110 spectrophotometer of Hitachi, Japan, and then calculated.
结果如下表所示。The results are shown in the table below.
表1。Table 1.
。 .
上述实施方式仅为本发明的优选实施方式，不能以此来限定本发明保护的范围，本领域的技术人员在本发明的基础上所做的任何非实质性的变化及替换均属于本发明所要求保护的范围。The above-mentioned embodiment is only a preferred embodiment of the present invention, and cannot be used to limit the protection scope of the present invention. Any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention belong to the scope of the present invention. Scope of protection claimed.

Claims (9)

  1. 一种红外屏蔽型EVA热熔胶膜，其特征在于，包括如下重量份的组分：An infrared shielding type EVA hot-melt adhesive film is characterized in that it comprises the following components by weight:
    EVA主体树脂 60份-80份；红外线屏蔽剂10份-30份；散热剂5份-10份；硅烷偶联剂8份-15份；助溶剂2份-6份；无机阻燃剂0.1份-1份；增粘剂3份-10份；引发剂0.1份-1份；抗氧化剂0.01份-1份；其中，所述EVA主体树脂的的熔指为200g/10min -300g/10min。EVA main resin 60-80 parts; infrared shielding agent 10-30 parts; cooling agent 5-10 parts; silane coupling agent 8-15 parts; co-solvent 2-6 parts; inorganic flame retardant 0.1 part -1 part; 3-10 parts of tackifier; 0.1-1 part of initiator; 0.01-1 part of antioxidant; wherein, the melt index of the EVA main resin is 200g/10min-300g/10min.
  2. 根据权利要求1所述的红外屏蔽型EVA热熔胶膜，其特征在于，所述红外线屏蔽剂为聚苯胺、硫化铜、芘酰亚胺中的一种或两种以上。The infrared-shielding EVA hot-melt adhesive film according to claim 1, wherein the infrared shielding agent is one or more of polyaniline, copper sulfide, and pyreneimide.
  3. 根据权利要求2所述的红外屏蔽型EVA热熔胶膜，其特征在于，所述红外线屏蔽剂由质量比为1：（4-5）的硫化铜与聚苯胺或芘酰亚胺所组成，其中，所述硫化铜为硫化铜纳米颗粒、硫化铜纳米球中的一种或两种。The infrared shielding EVA hot melt adhesive film according to claim 2, wherein the infrared shielding agent is composed of copper sulfide and polyaniline or pyreneimide with a mass ratio of 1: (4-5), Wherein, the copper sulfide is one or both of copper sulfide nanoparticles and copper sulfide nanospheres.
  4. 根据权利要求1所述的红外屏蔽型EVA热熔胶膜，其特征在于，所述散热剂为氧化石墨烯、石墨烯、碳纳米管中的一种或两种以上。The infrared-shielding EVA hot-melt adhesive film according to claim 1, wherein the cooling agent is one or more of graphene oxide, graphene, and carbon nanotubes.
  5. 根据权利要求1所述的红外屏蔽型EVA热熔胶膜，其特征在于，所述硅烷偶联剂为乙烯基硅烷、氨基硅烷、甲基丙烯酰氧基硅烷中的一种或两种以上。The infrared-shielding EVA hot-melt adhesive film according to claim 1, wherein the silane coupling agent is one or more of vinylsilane, aminosilane, and methacryloxysilane.
  6. 根据权利要求1所述的红外屏蔽型EVA热熔胶膜，其特征在于，所述助溶剂为乙二醇单丁醚、丙二醇单丁醚、二乙二醇单丁醚、丁醇中的一种或两种以上。The infrared shielding type EVA hot-melt adhesive film according to claim 1, wherein the cosolvent is one of ethylene glycol monobutyl ether, propylene glycol monobutyl ether, diethylene glycol monobutyl ether, butanol species or two or more.
  7. 根据权利要求1所述的红外屏蔽型EVA热熔胶膜，其特征在于，所述无机阻燃剂为氢氧化镁、氢氧化铝中的一种或两种；所述增粘剂为松香树脂、碳五加氢石油树脂、萜烯树脂中的一种或者两种以上。The infrared shielding type EVA hot-melt adhesive film according to claim 1, wherein the inorganic flame retardant is one or both of magnesium hydroxide and aluminum hydroxide; the tackifier is rosin resin One or more of C5 hydrogenated petroleum resins and terpene resins.
  8. 根据权利要求1所述的红外屏蔽型EVA热熔胶膜，其特征在于，所述EVA主体树脂与所述红外线屏蔽剂、硅烷偶联剂的质量比为1：（0.2-0.4）：（0.1-0.2）。The infrared shielding EVA hot melt adhesive film according to claim 1, characterized in that the mass ratio of the EVA main resin to the infrared shielding agent and the silane coupling agent is 1: (0.2-0.4): (0.1 -0.2).
  9. 一种如权利要求1-8任一项所述的红外屏蔽型EVA热熔胶膜的制备方法，其特征在于，包括如下制备步骤：A preparation method of the infrared shielding type EVA hot-melt adhesive film as claimed in any one of claims 1-8, characterized in that, comprising the following preparation steps:
    S1：将EVA主体树脂、硅烷偶联剂、助溶剂、无机阻燃剂、引发剂、抗氧化剂和增粘剂加入到高速混合机中高速搅拌混合，边搅拌边加入红外线屏蔽剂和散热剂，混合均匀，得到混合物料；S1: Add EVA main resin, silane coupling agent, co-solvent, inorganic flame retardant, initiator, antioxidant and tackifier to a high-speed mixer and mix at high speed, and add infrared shielding agent and cooling agent while stirring. Mix evenly to obtain a mixed material;
    S2：将混合物料投入螺杆挤出机中熔融挤出，经延流、冷却、牵引及收卷的步骤，得到红外屏蔽型EVA热熔胶膜。S2: Put the mixed material into the screw extruder to melt and extrude, and go through the steps of spreading, cooling, pulling and winding to obtain an infrared shielding EVA hot-melt adhesive film.
    10、根据权利要求9所述的红外屏蔽型EVA热熔胶膜的制备方法，其特征在于，包括如下制备步骤：10. The method for preparing an infrared-shielding EVA hot-melt adhesive film according to claim 9, characterized in that it comprises the following preparation steps:
    S1：将EVA主体树脂、硅烷偶联剂、助溶剂、无机阻燃剂、引发剂、抗氧化剂和增粘剂加入到高速混合机中高速搅拌混合，混合20min-40min后，边搅拌边加入红外线屏蔽剂和散热剂，混合均匀30min-40min，得到混合物料；S1: Add EVA main resin, silane coupling agent, co-solvent, inorganic flame retardant, initiator, antioxidant and tackifier to a high-speed mixer and mix at high speed. After mixing for 20min-40min, add infrared rays while stirring The shielding agent and cooling agent are mixed evenly for 30min-40min to obtain the mixed material;
    S2：将混合物料投入螺杆挤出机中在120℃-140℃下熔融挤出，经延流、冷却、牵引及收卷的步骤，得到红外屏蔽型EVA热熔胶膜。S2: Put the mixed material into a screw extruder and melt and extrude it at 120°C-140°C. After the steps of casting, cooling, drawing and winding, an infrared shielding EVA hot-melt adhesive film is obtained.
PCT/CN2022/084178 2022-02-15 2022-03-30 Infrared shielding type eva hot melt adhesive film and preparation method therefor WO2023155277A1 (en)

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