WO2024021179A1 - Thermocuring crosslinking-type hot melt adhesive film and preparation method therefor - Google Patents

Thermocuring crosslinking-type hot melt adhesive film and preparation method therefor Download PDF

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Publication number
WO2024021179A1
WO2024021179A1 PCT/CN2022/112141 CN2022112141W WO2024021179A1 WO 2024021179 A1 WO2024021179 A1 WO 2024021179A1 CN 2022112141 W CN2022112141 W CN 2022112141W WO 2024021179 A1 WO2024021179 A1 WO 2024021179A1
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adhesive film
cross
parts
melt adhesive
hot melt
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PCT/CN2022/112141
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French (fr)
Chinese (zh)
Inventor
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 WO2024021179A1 publication Critical patent/WO2024021179A1/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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • 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
    • 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
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron

Definitions

  • the invention relates to the field of hot-melt adhesive film materials, and in particular to a thermally cured cross-linked hot-melt adhesive film and a preparation method thereof.
  • Hot melt adhesive film is made of hot melt adhesive into a film of a certain thickness, placed between adherends, and bonded by heating and pressure. It helps industrial production achieve modularization, improves production efficiency, and saves glue. material, and is widely used in the clothing, textile, automobile, and electronics industries due to its solvent-free, pollution-free, and fast curing speed. With the development of industry, the performance requirements for hot melt adhesive films are becoming higher and higher.
  • the present invention provides a thermally cured cross-linked hot melt adhesive film with excellent high temperature resistance and thermal conductivity.
  • the invention provides a method for preparing a thermally cured cross-linked hot melt adhesive film, which has a simple and convenient process.
  • the present invention adopts the following technical solutions.
  • a heat-curing cross-linked hot melt adhesive film including the following components by weight: 50-70 parts by weight of TPU; 40-60 parts by composite cross-linking agent; 15-25 parts by phenolic resin; 5-10 parts by temperature-resistant filler; thermal conductivity 5-10 parts of filler; 3-8 parts of light stabilizer.
  • the composite cross-linking agent is composed of a main cross-linking agent and an auxiliary cross-linking agent with a mass ratio of 1-2:1.
  • the main cross-linking agent is di-tert-butyl peroxide, dicumyl peroxide, tert-butyl cumyl peroxide, 1,1-di-tert-butyl peroxide
  • the main cross-linking agent is di-tert-butyl peroxide, dicumyl peroxide, tert-butyl cumyl peroxide, 1,1-di-tert-butyl peroxide.
  • auxiliary cross-linking agent is N, N’-methylene bisacrylamide.
  • the phenolic resin is one of phenolic-epoxy resin, phenolic epoxy vinyl resin, phenol type novolac epoxy resin, and o-cresol type novolac epoxy resin.
  • thermo-resistant filler is one of mica powder, quartz powder, alumina or fumed silica.
  • thermally conductive filler is one of graphene nanosheets, expanded graphite, multi-walled carbon nanotubes, and hexagonal boron nitride.
  • the light stabilizer is N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,6-hexanediamine, bis( One of 2,2,6,6-tetramethyl-4-piperidinyl) subebate and bis-2,2,6,6-tetramethylpiperidinol subebate.
  • a method for preparing a thermally cured cross-linked hot melt adhesive film including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
  • the stirring speed is 450-600r/min
  • the stirring time is 10-20min
  • the casting temperature is 100-120°C
  • the thickness of the thermally cured cross-linked hot melt adhesive film is 0.1 -0.25mm.
  • the present invention uses a multi-component cross-linking agent, and the main cross-linking agent and the auxiliary cross-linking agent are used in combination, so that each component can exert a good synergistic effect, thereby ensuring that the production is minimized on the basis of rapid cross-linking.
  • cost the system combination of phenolic resin and temperature-resistant fillers greatly enhances the temperature resistance of the film and improves corrosion resistance; by adding thermally conductive fillers, the film has better whisker channels inside, speeding up its thermal conductivity; light
  • stabilizers can ensure the aging resistance of the film; the proportion and total amount of various additives added do not change much compared to the conventional formula, but the reaction speed is fast, the degree of curing is high, and the thermal conductivity is significantly improved.
  • a heat-curing cross-linked hot melt adhesive film including the following components by weight: 50-70 parts by weight of TPU; 40-60 parts by composite cross-linking agent; 15-25 parts by phenolic resin; 5-10 parts by temperature-resistant filler; thermal conductivity 5-10 parts of filler; 3-8 parts of light stabilizer.
  • the composite cross-linking agent is composed of a main cross-linking agent and an auxiliary cross-linking agent with a mass ratio of 1-2:1.
  • the main cross-linking agent is di-tert-butyl peroxide, dicumyl peroxide, tert-butyl cumyl peroxide, 1,1-di-tert-butyl peroxide-3,3, One of 5-trimethylcyclohexane.
  • auxiliary cross-linking agent is N,N’-methylenebisacrylamide.
  • the phenolic resin is one of phenolic-epoxy resin, phenolic epoxy vinyl resin, phenol type novolac epoxy resin, and o-cresol type novolac epoxy resin.
  • the temperature-resistant filler is one of mica powder, quartz powder, alumina or fumed silica.
  • thermally conductive filler is one of graphene nanosheets, expanded graphite, multi-walled carbon nanotubes, and hexagonal boron nitride.
  • the light stabilizer is N,N-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,6-hexanediamine, bis(2,2,6, One of 6-tetramethyl-4-piperidinyl) subebate and bis-2,2,6,6-tetramethylpiperidinol subebate.
  • a method for preparing a thermally cured cross-linked hot melt adhesive film including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
  • the stirring speed is 450-600r/min
  • the stirring time is 10-20min
  • the casting temperature is 100-120°C
  • the thickness of the thermosetting cross-linked hot melt adhesive film is 0.1-0.25mm.
  • a method for preparing a thermally cured cross-linked hot melt adhesive film including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
  • the heat-curing cross-linked hot melt adhesive film includes the following components by weight: 50 parts of TPU; 40 parts of composite cross-linking agent; 15 parts of phenolic resin; 5 parts of temperature-resistant filler; 5 parts of thermally conductive filler; 3 parts of light stabilizer .
  • the stirring speed is 450 r/min
  • the stirring time is 10 minutes
  • the casting temperature is 100°C
  • the thickness of the thermally cured cross-linked hot melt adhesive film is 0.1 mm.
  • a method for preparing a thermally cured cross-linked hot melt adhesive film including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
  • the heat-curing cross-linked hot melt adhesive film includes the following components by weight: 55 parts of TPU; 45 parts of composite cross-linking agent; 20 parts of phenolic resin; 8 parts of temperature-resistant filler; 5 parts of thermally conductive filler; 3 parts of light stabilizer .
  • the stirring speed is 450 r/min, the stirring time is 15 minutes; the casting temperature is 100°C; and the thickness of the thermally cured cross-linked hot melt adhesive film is 0.1 mm.
  • a method for preparing a thermally cured cross-linked hot melt adhesive film including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
  • the heat-curing cross-linked hot melt adhesive film includes the following components by weight: 60 parts of TPU; 55 parts of composite cross-linking agent; 20 parts of phenolic resin; 7 parts of temperature-resistant fillers; 8 parts of thermally conductive fillers; 6 parts of light stabilizer .
  • the stirring speed is 500 r/min, the stirring time is 15 minutes; the casting temperature is 110°C; and the thickness of the thermally cured cross-linked hot melt adhesive film is 0.2 mm.
  • a method for preparing a thermally cured cross-linked hot melt adhesive film including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
  • thermosetting cross-linked hot melt adhesive film includes the following components by weight: 70 parts of TPU; 60 parts of composite cross-linking agent; 25 parts of phenolic resin; 10 parts of temperature-resistant filler; 10 parts of thermally conductive filler; 8 parts of light stabilizer .
  • the stirring speed is 600 r/min, the stirring time is 20 minutes; the casting temperature is 120°C; and the thickness of the thermally cured cross-linked hot melt adhesive film is 0.25 mm.
  • Example 1 Repeat the preparation method of Example 1 according to the specified parts of each component, but do not add and use phenolic resin and temperature-resistant filler.
  • Example 1 Repeat the preparation method of Example 1 according to the specified portions of each component, but do not add or use the thermally conductive filler.
  • Comparative Example 3 uses an uncured cross-linked adhesive film.
  • Sample structure film/back plate.
  • Lamination process 140°C, vacuum for 4min30s, pressurization for 12s, lamination for 5min.
  • Test conditions Tensile speed is 100mm/min.
  • Performance meter method observe the peeling strength of the film and backing board.
  • Test Examples 1-4 and Comparative Examples 1-2 according to the experimental method of GB/T2423.3-2006.
  • Test conditions temperature 85°C, humidity 85%, 1000h.
  • Sample composition composed of back plate, film, and glass.
  • Lamination conditions 140°C, vacuum for 4 minutes and 30 seconds, pressurization for 12 seconds, and lamination for 5 minutes.
  • Performance characterization method A. The yellowing index ( ⁇ Y1) is analyzed in accordance with GB2409-80 "Plastic Yellowness Index Test Method"; B. Observe whether the sample has bubbles, degumming and other phenomena.
  • the present invention uses a multi-component cross-linking agent, and the main cross-linking agent and the auxiliary cross-linking agent are used in combination, so that each component can exert a good synergistic effect, thereby ensuring that the production is minimized on the basis of rapid cross-linking.
  • cost the system combination of phenolic resin and temperature-resistant fillers greatly enhances the temperature resistance of the film and improves corrosion resistance; by adding thermally conductive fillers, the film has better whisker channels inside, speeding up its thermal conductivity; light
  • stabilizers can ensure the aging resistance of the film; the proportion and total amount of various additives added do not change much compared to the conventional formula, but the reaction speed is fast, the degree of curing is high, and the thermal conductivity is significantly improved.

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

Abstract

A thermocuring crosslinking-type hot melt adhesive film, comprising the following components in parts by weight: 50-70 parts of TPU; 40-60 parts of a composite crosslinking agent; 15-25 parts of a phenolic resin; 5-10 parts of a temperature-resistant filler; 5-10 parts of a heat-conducting filler; and 3-8 parts of a light stabilizer. A multi-component crosslinking agent is used, and a main crosslinking agent and an auxiliary crosslinking agent are matched for use, such that the components generate a relatively good synergistic effect, thereby maximally reducing the production cost on the basis of ensuring rapid crosslinking; the systematic combination of a phenolic resin and a temperature-resistant filler greatly enhances the temperature resistance of the adhesive film and improves the corrosion resistance thereof; by adding a heat-conducting filler, a relatively good whisker channel is formed in the adhesive film, such that the heat conduction efficiency of the adhesive film is improved; by adding a light stabilizer, the aging resistance of the adhesive film can be ensured; and compared with a conventional formula, addition proportions and the total amount of various auxiliaries are not changed much, but the reaction speed is high, the curing degree is high, and the thermal conductivity is obviously improved.

Description

热固化交联型热熔胶膜及其制备方法Thermal curing cross-linked 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7月25日提交中国专利局，申请号为202210879692.6，发明名称为“一种热固化交联型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 requests the priority of the Chinese patent application submitted to the China Patent Office on July 25, 2022, with the application number 202210879692.6, and the invention name is "A thermosetting cross-linked hot melt adhesive film and its preparation method", all of which The contents are incorporated into this application by reference.
技术领域Technical field
本发明涉及热熔胶膜材料领域，特别是涉及一种热固化交联型热熔胶膜及其制备方法。The invention relates to the field of hot-melt adhesive film materials, and in particular to a thermally cured cross-linked hot-melt adhesive film and a preparation method thereof.
背景技术Background technique
热熔胶膜是将热熔胶制成一定厚度的薄膜，置于被粘物之间，通过加热加压实施粘接，它帮助了工业生产实现模块化，提高生产效率的同时还节省了胶料，同时以其无溶剂、无污染、固化速度快等优点广泛应用在服装、纺织、汽车、电子行业。随着工业的发展，对热熔胶膜的性能要求也越来越高。Hot melt adhesive film is made of hot melt adhesive into a film of a certain thickness, placed between adherends, and bonded by heating and pressure. It helps industrial production achieve modularization, improves production efficiency, and saves glue. material, and is widely used in the clothing, textile, automobile, and electronics industries due to its solvent-free, pollution-free, and fast curing speed. With the development of industry, the performance requirements for hot melt adhesive films are becoming higher and higher.
技术问题technical problem
目前的热熔胶膜存在耐高温性能、导热效果不佳等缺陷，因此，亟需一种性能优异的热固化交联型热熔胶膜。Current hot melt adhesive films have shortcomings such as high temperature resistance and poor thermal conductivity. Therefore, there is an urgent need for a thermally cured cross-linked hot melt adhesive film with excellent performance.
技术解决方案Technical solutions
为解决上述技术问题，本发明提供一种耐高温性能、导热效果优异的热固化交联型热熔胶膜。In order to solve the above technical problems, the present invention provides a thermally cured cross-linked hot melt adhesive film with excellent high temperature resistance and thermal conductivity.
本发明提供一种热固化交联型热熔胶膜的制备方法，工艺简单便捷。The invention provides a method for preparing a thermally cured cross-linked hot melt adhesive film, which has a simple and convenient process.
本发明采用如下技术方案。The present invention adopts the following technical solutions.
一种热固化交联型热熔胶膜，包括如下重量份的组分：TPU50-70份；复合交联剂40-60份；酚醛树脂15-25份；耐温填料5-10份；导热填料5-10份；光稳定剂3-8份。A heat-curing cross-linked hot melt adhesive film, including the following components by weight: 50-70 parts by weight of TPU; 40-60 parts by composite cross-linking agent; 15-25 parts by phenolic resin; 5-10 parts by temperature-resistant filler; thermal conductivity 5-10 parts of filler; 3-8 parts of light stabilizer.
对上述技术方案的进一步改进为，所述复合交联剂由主交联剂和辅交联剂以质量比为1-2：1组成。A further improvement to the above technical solution is that the composite cross-linking agent is composed of a main cross-linking agent and an auxiliary cross-linking agent with a mass ratio of 1-2:1.
对上述技术方案的进一步改进为，所述主交联剂为二叔丁基过氧化物、二枯基过氧化物、叔丁基枯基过氧化物、1,1-二叔丁基过氧化物-3,3,5-三甲基环己烷中的一种。A further improvement to the above technical solution is that the main cross-linking agent is di-tert-butyl peroxide, dicumyl peroxide, tert-butyl cumyl peroxide, 1,1-di-tert-butyl peroxide One of the substances -3,3,5-trimethylcyclohexane.
对上述技术方案的进一步改进为，所述辅交联剂为N,N’-亚甲基双丙烯酰胺。A further improvement to the above technical solution is that the auxiliary cross-linking agent is N, N’-methylene bisacrylamide.
对上述技术方案的进一步改进为，所述酚醛树脂为酚醛-环氧树脂、酚醛环氧乙烯基树脂、苯酚型酚醛环氧树脂、邻甲酚型酚醛环氧树脂中的一种。A further improvement to the above technical solution is that the phenolic resin is one of phenolic-epoxy resin, phenolic epoxy vinyl resin, phenol type novolac epoxy resin, and o-cresol type novolac epoxy resin.
对上述技术方案的进一步改进为，所述耐温填料为云母粉、石英粉、氧化铝或气相白炭黑中的一种。A further improvement to the above technical solution is that the temperature-resistant filler is one of mica powder, quartz powder, alumina or fumed silica.
对上述技术方案的进一步改进为，所述导热填料为石墨烯纳米片、膨胀石墨、多壁碳纳米管、六方氮化硼中的一种。A further improvement to the above technical solution is that the thermally conductive filler is one of graphene nanosheets, expanded graphite, multi-walled carbon nanotubes, and hexagonal boron nitride.
对上述技术方案的进一步改进为，所述光稳定剂为N,N-双(2,2,6,6-四甲基-4-哌啶基)-1,6-己二胺、双(2,2,6,6-四甲基-4-哌啶基)葵二酸酯和葵二酸双2,2,6,6-四甲基哌啶醇酯中的一种。A further improvement to the above technical solution is that the light stabilizer is N,N-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,6-hexanediamine, bis( One of 2,2,6,6-tetramethyl-4-piperidinyl) subebate and bis-2,2,6,6-tetramethylpiperidinol subebate.
一种热固化交联型热熔胶膜的制备方法，包括如下步骤：按配比将各组分添加至搅拌机中进行搅拌，待搅拌后，投入至流延机中进行流延，再经过塑化挤出、拉伸、热固化、牵引、收卷，制得热固化交联型热熔胶膜。A method for preparing a thermally cured cross-linked hot melt adhesive film, including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
对上述技术方案的进一步改进为，搅拌的转速为450-600r/min，搅拌的时间为10-20min；流延的温度为100-120℃；热固化交联型热熔胶膜的厚度为0.1-0.25mm。Further improvements to the above technical solution are as follows: the stirring speed is 450-600r/min, the stirring time is 10-20min; the casting temperature is 100-120°C; the thickness of the thermally cured cross-linked hot melt adhesive film is 0.1 -0.25mm.
有益效果beneficial effects
本发明采用多组分交联剂，由主交联剂与辅交联剂搭配使用，使其各组分之间发挥较好的协同作用，从而保证在快速交联的基础上最大限度降低生产成本；酚醛树脂和耐温填料的体系结合大大增强了胶膜的耐温性能，提高了耐腐蚀性；通过添加导热填料，使胶膜内部拥有较好的晶须通道，加快其导热效率；光稳定剂的添加则可以保证胶膜的耐老化性能；各种助剂添加的比例和总量相对常规配方变化不大，但反应速度快，固化程度高，导热率有明显提升。The present invention uses a multi-component cross-linking agent, and the main cross-linking agent and the auxiliary cross-linking agent are used in combination, so that each component can exert a good synergistic effect, thereby ensuring that the production is minimized on the basis of rapid cross-linking. cost; the system combination of phenolic resin and temperature-resistant fillers greatly enhances the temperature resistance of the film and improves corrosion resistance; by adding thermally conductive fillers, the film has better whisker channels inside, speeding up its thermal conductivity; light The addition of stabilizers can ensure the aging resistance of the film; the proportion and total amount of various additives added do not change much compared to the conventional formula, but the reaction speed is fast, the degree of curing is high, and the thermal conductivity is significantly improved.
本发明的实施方式Embodiments of the invention
下面结合具体实施方式，对本发明做进一步描述，需要说明的是，在不相冲突的前提下，以下描述的各实施例之间或各技术特征之间可以任意组合形成新的实施例。The present invention will be further described below in conjunction with specific implementation modes. It should be noted that, provided there is no conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments.
一种热固化交联型热熔胶膜，包括如下重量份的组分：TPU50-70份；复合交联剂40-60份；酚醛树脂15-25份；耐温填料5-10份；导热填料5-10份；光稳定剂3-8份。A heat-curing cross-linked hot melt adhesive film, including the following components by weight: 50-70 parts by weight of TPU; 40-60 parts by composite cross-linking agent; 15-25 parts by phenolic resin; 5-10 parts by temperature-resistant filler; thermal conductivity 5-10 parts of filler; 3-8 parts of light stabilizer.
进一步地，所述复合交联剂由主交联剂和辅交联剂以质量比为1-2：1组成。Further, the composite cross-linking agent is composed of a main cross-linking agent and an auxiliary cross-linking agent with a mass ratio of 1-2:1.
进一步地，所述主交联剂为二叔丁基过氧化物、二枯基过氧化物、叔丁基枯基过氧化物、1,1-二叔丁基过氧化物-3,3,5-三甲基环己烷中的一种。Further, the main cross-linking agent is di-tert-butyl peroxide, dicumyl peroxide, tert-butyl cumyl peroxide, 1,1-di-tert-butyl peroxide-3,3, One of 5-trimethylcyclohexane.
进一步地，所述辅交联剂为N,N’-亚甲基双丙烯酰胺。Further, the auxiliary cross-linking agent is N,N’-methylenebisacrylamide.
进一步地，所述酚醛树脂为酚醛-环氧树脂、酚醛环氧乙烯基树脂、苯酚型酚醛环氧树脂、邻甲酚型酚醛环氧树脂中的一种。Further, the phenolic resin is one of phenolic-epoxy resin, phenolic epoxy vinyl resin, phenol type novolac epoxy resin, and o-cresol type novolac epoxy resin.
进一步地，所述耐温填料为云母粉、石英粉、氧化铝或气相白炭黑中的一种。Further, the temperature-resistant filler is one of mica powder, quartz powder, alumina or fumed silica.
进一步地，所述导热填料为石墨烯纳米片、膨胀石墨、多壁碳纳米管、六方氮化硼中的一种。Further, the thermally conductive filler is one of graphene nanosheets, expanded graphite, multi-walled carbon nanotubes, and hexagonal boron nitride.
进一步地，所述光稳定剂为N,N-双(2,2,6,6-四甲基-4-哌啶基)-1,6-己二胺、双(2,2,6,6-四甲基-4-哌啶基)葵二酸酯和葵二酸双2,2,6,6-四甲基哌啶醇酯中的一种。Further, the light stabilizer is N,N-bis(2,2,6,6-tetramethyl-4-piperidinyl)-1,6-hexanediamine, bis(2,2,6, One of 6-tetramethyl-4-piperidinyl) subebate and bis-2,2,6,6-tetramethylpiperidinol subebate.
一种热固化交联型热熔胶膜的制备方法，包括如下步骤：按配比将各组分添加至搅拌机中进行搅拌，待搅拌后，投入至流延机中进行流延，再经过塑化挤出、拉伸、热固化、牵引、收卷，制得热固化交联型热熔胶膜。A method for preparing a thermally cured cross-linked hot melt adhesive film, including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
进一步地，搅拌的转速为450-600r/min，搅拌的时间为10-20min；流延的温度为100-120℃；热固化交联型热熔胶膜的厚度为0.1-0.25mm。Further, the stirring speed is 450-600r/min, the stirring time is 10-20min; the casting temperature is 100-120°C; the thickness of the thermosetting cross-linked hot melt adhesive film is 0.1-0.25mm.
实施例1。Example 1.
一种热固化交联型热熔胶膜的制备方法，包括如下步骤：按配比将各组分添加至搅拌机中进行搅拌，待搅拌后，投入至流延机中进行流延，再经过塑化挤出、拉伸、热固化、牵引、收卷，制得热固化交联型热熔胶膜。A method for preparing a thermally cured cross-linked hot melt adhesive film, including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
所述热固化交联型热熔胶膜包括如下重量份的组分：TPU50份；复合交联剂40份；酚醛树脂15份；耐温填料5份；导热填料5份；光稳定剂3份。The heat-curing cross-linked hot melt adhesive film includes the following components by weight: 50 parts of TPU; 40 parts of composite cross-linking agent; 15 parts of phenolic resin; 5 parts of temperature-resistant filler; 5 parts of thermally conductive filler; 3 parts of light stabilizer .
进一步地，搅拌的转速为450r/min，搅拌的时间为10min；流延的温度为100℃；热固化交联型热熔胶膜的厚度为0.1mm。Further, the stirring speed is 450 r/min, the stirring time is 10 minutes, the casting temperature is 100°C, and the thickness of the thermally cured cross-linked hot melt adhesive film is 0.1 mm.
实施例2。Example 2.
一种热固化交联型热熔胶膜的制备方法，包括如下步骤：按配比将各组分添加至搅拌机中进行搅拌，待搅拌后，投入至流延机中进行流延，再经过塑化挤出、拉伸、热固化、牵引、收卷，制得热固化交联型热熔胶膜。A method for preparing a thermally cured cross-linked hot melt adhesive film, including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
所述热固化交联型热熔胶膜包括如下重量份的组分：TPU55份；复合交联剂45份；酚醛树脂20份；耐温填料8份；导热填料5份；光稳定剂3份。The heat-curing cross-linked hot melt adhesive film includes the following components by weight: 55 parts of TPU; 45 parts of composite cross-linking agent; 20 parts of phenolic resin; 8 parts of temperature-resistant filler; 5 parts of thermally conductive filler; 3 parts of light stabilizer .
进一步地，搅拌的转速为450r/min，搅拌的时间为15min；流延的温度为100℃；热固化交联型热熔胶膜的厚度为0.1mm。Further, the stirring speed is 450 r/min, the stirring time is 15 minutes; the casting temperature is 100°C; and the thickness of the thermally cured cross-linked hot melt adhesive film is 0.1 mm.
实施例3。Example 3.
一种热固化交联型热熔胶膜的制备方法，包括如下步骤：按配比将各组分添加至搅拌机中进行搅拌，待搅拌后，投入至流延机中进行流延，再经过塑化挤出、拉伸、热固化、牵引、收卷，制得热固化交联型热熔胶膜。A method for preparing a thermally cured cross-linked hot melt adhesive film, including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
所述热固化交联型热熔胶膜包括如下重量份的组分：TPU60份；复合交联剂55份；酚醛树脂20份；耐温填料7份；导热填料8份；光稳定剂6份。The heat-curing cross-linked hot melt adhesive film includes the following components by weight: 60 parts of TPU; 55 parts of composite cross-linking agent; 20 parts of phenolic resin; 7 parts of temperature-resistant fillers; 8 parts of thermally conductive fillers; 6 parts of light stabilizer .
进一步地，搅拌的转速为500r/min，搅拌的时间为15min；流延的温度为110℃；热固化交联型热熔胶膜的厚度为0.2mm。Further, the stirring speed is 500 r/min, the stirring time is 15 minutes; the casting temperature is 110°C; and the thickness of the thermally cured cross-linked hot melt adhesive film is 0.2 mm.
实施例4。Example 4.
一种热固化交联型热熔胶膜的制备方法，包括如下步骤：按配比将各组分添加至搅拌机中进行搅拌，待搅拌后，投入至流延机中进行流延，再经过塑化挤出、拉伸、热固化、牵引、收卷，制得热固化交联型热熔胶膜。A method for preparing a thermally cured cross-linked hot melt adhesive film, including the following steps: adding each component to a mixer according to the proportion and stirring, after stirring, putting it into a casting machine for casting, and then plasticizing Extrusion, stretching, heat curing, traction, and winding are carried out to prepare a heat curing cross-linked hot melt adhesive film.
所述热固化交联型热熔胶膜包括如下重量份的组分：TPU70份；复合交联剂60份；酚醛树脂25份；耐温填料10份；导热填料10份；光稳定剂8份。The thermosetting cross-linked hot melt adhesive film includes the following components by weight: 70 parts of TPU; 60 parts of composite cross-linking agent; 25 parts of phenolic resin; 10 parts of temperature-resistant filler; 10 parts of thermally conductive filler; 8 parts of light stabilizer .
进一步地，搅拌的转速为600r/min，搅拌的时间为20min；流延的温度为120℃；热固化交联型热熔胶膜的厚度为0.25mm。Further, the stirring speed is 600 r/min, the stirring time is 20 minutes; the casting temperature is 120°C; and the thickness of the thermally cured cross-linked hot melt adhesive film is 0.25 mm.
对比例1。Comparative Example 1.
按照指定的各组分份数重复实施例1的制备方法，但不添加使用酚醛树脂和耐温填料。Repeat the preparation method of Example 1 according to the specified parts of each component, but do not add and use phenolic resin and temperature-resistant filler.
对比例2。Comparative Example 2.
按照指定的各组分份数重复实施例1的制备方法，但不添加使用导热填料。Repeat the preparation method of Example 1 according to the specified portions of each component, but do not add or use the thermally conductive filler.
对比例3。Comparative Example 3.
对比例3采用未固化交联的胶膜。Comparative Example 3 uses an uncured cross-linked adhesive film.
效果评价及性能检测。Effect evaluation and performance testing.
一、剥离强度测试。1. Peel strength test.
按照GB/T2792-1998《压敏胶粘带剥离试验》标准对实施例1-4和对比例1-2进行剥离强度的测试。The peel strength of Examples 1-4 and Comparative Examples 1-2 was tested in accordance with the standard of GB/T2792-1998 "Pressure Sensitive Adhesive Tape Peeling Test".
样品结构：胶膜/背板。层压工艺：140℃，抽真空4min30s，加压12s，层压5min。试验条件：拉伸速度为100mm/min。性能表针方法：观察胶膜与背板的剥离强度大小。Sample structure: film/back plate. Lamination process: 140℃, vacuum for 4min30s, pressurization for 12s, lamination for 5min. Test conditions: Tensile speed is 100mm/min. Performance meter method: observe the peeling strength of the film and backing board.
二、耐湿热老化性能测试。2. Humidity and heat aging resistance test.
按照GB/T2423.3-2006的实验方法对实施例1-4和对比例1-2进行测试。Test Examples 1-4 and Comparative Examples 1-2 according to the experimental method of GB/T2423.3-2006.
试验条件：温度85℃，湿度85％，1000h。样品组成：依次由背板，胶膜，玻璃构成。层压条件：140℃，抽真空4min30s，加压12s，层压5min。性能表征方法：A黄变指数(△Y1)按照GB2409-80《塑料黄色指数试验方法》进行分析；B：观察样品是否有气泡、脱胶等现象产生。Test conditions: temperature 85℃, humidity 85%, 1000h. Sample composition: composed of back plate, film, and glass. Lamination conditions: 140°C, vacuum for 4 minutes and 30 seconds, pressurization for 12 seconds, and lamination for 5 minutes. Performance characterization method: A. The yellowing index (△Y1) is analyzed in accordance with GB2409-80 "Plastic Yellowness Index Test Method"; B. Observe whether the sample has bubbles, degumming and other phenomena.
三、交联度测试。3. Cross-linking degree test.
采用二甲苯萃取胶膜样品中未交联部分，称取萃取前后样品的重量W，用来表示交联度。实施例1-4和对比例1-2的胶膜经过140℃，抽真空4min30s，加压12s，层压5min的工艺进行层压制得。然后使用剪刀将其剪成直径约3mm左右的颗粒，放入钢丝网中，用细线绑紧，投入到二甲苯溶剂中进行萃取(萃取温度为140℃，萃取时间为10h)，最后萃取完后进行烘干(烘干温度140℃)，称量萃取前后的重量差，计算出交联度。Use xylene to extract the uncrosslinked part of the film sample, and weigh the weight W of the sample before and after extraction to express the degree of crosslinking. The adhesive films of Examples 1-4 and Comparative Examples 1-2 were laminated at 140°C, vacuumed for 4 minutes and 30 seconds, pressurized for 12 seconds, and laminated for 5 minutes. Then use scissors to cut it into particles with a diameter of about 3mm, put it into a steel mesh, tie it tightly with a thin wire, put it into xylene solvent for extraction (extraction temperature is 140°C, extraction time is 10h), and finally the extraction is completed After drying (drying temperature 140°C), weigh the weight difference before and after extraction to calculate the cross-linking degree.
四、导热性能测试。4. Thermal conductivity test.
采用稳态平板法测量材料的热导率，使用平板导热仪对实施例1-4和对比例1-2进行测试，将胶膜样品制备成270×270mm2的试样，并分别读取试件的电功率W，电压U，电流I，热面温度t1和冷面温度t2的值。Use the steady-state plate method to measure the thermal conductivity of the material. Use a plate thermal conductivity meter to test Examples 1-4 and Comparative Examples 1-2. Prepare the film sample into a 270×270mm2 sample, and read the test pieces respectively. The values of electric power W, voltage U, current I, hot surface temperature t1 and cold surface temperature t2.
测试结果如表1所示。The test results are shown in Table 1.
表1。Table 1.
。 .
本发明采用多组分交联剂，由主交联剂与辅交联剂搭配使用，使其各组分之间发挥较好的协同作用，从而保证在快速交联的基础上最大限度降低生产成本；酚醛树脂和耐温填料的体系结合大大增强了胶膜的耐温性能，提高了耐腐蚀性；通过添加导热填料，使胶膜内部拥有较好的晶须通道，加快其导热效率；光稳定剂的添加则可以保证胶膜的耐老化性能；各种助剂添加的比例和总量相对常规配方变化不大，但反应速度快，固化程度高，导热率有明显提升。The present invention uses a multi-component cross-linking agent, and the main cross-linking agent and the auxiliary cross-linking agent are used in combination, so that each component can exert a good synergistic effect, thereby ensuring that the production is minimized on the basis of rapid cross-linking. cost; the system combination of phenolic resin and temperature-resistant fillers greatly enhances the temperature resistance of the film and improves corrosion resistance; by adding thermally conductive fillers, the film has better whisker channels inside, speeding up its thermal conductivity; light The addition of stabilizers can ensure the aging resistance of the film; the proportion and total amount of various additives added do not change much compared to the conventional formula, but the reaction speed is fast, the degree of curing is high, and the thermal conductivity is significantly improved.
以上对本发明创造的实施例进行了详细说明，但所述内容仅为本发明创造的较佳实施例，不能被认为用于限定本发明创造的实施范围。凡依本发明创造申请范围所作的均等变化与改进等，均归属于本发明创造的专利涵盖范围之内。The embodiments of the present invention have been described in detail above, but the contents described are only preferred embodiments of the present invention and cannot be considered to limit the implementation scope of the present invention. All equivalent changes and improvements made in accordance with the application scope of this invention shall fall within the scope of the patent covered by this invention.

Claims (10)

  1. 一种热固化交联型热熔胶膜，其特征在于，包括如下重量份的组分：TPU50-70份；复合交联剂40-60份；酚醛树脂15-25份；耐温填料5-10份；导热填料5-10份；光稳定剂3-8份。A thermally cured cross-linked hot melt adhesive film, characterized by including the following components by weight: 50-70 parts of TPU; 40-60 parts of composite cross-linking agent; 15-25 parts of phenolic resin; 5-5 parts of temperature-resistant filler 10 parts; thermally conductive filler 5-10 parts; light stabilizer 3-8 parts.
  2. 根据权利要求1所述的热固化交联型热熔胶膜，其特征在于，所述复合交联剂由主交联剂和辅交联剂以质量比为1-2：1组成。The thermosetting cross-linked hot melt adhesive film according to claim 1, characterized in that the composite cross-linking agent is composed of a main cross-linking agent and an auxiliary cross-linking agent with a mass ratio of 1-2:1.
  3. 根据权利要求2所述的热固化交联型热熔胶膜，其特征在于，所述主交联剂为二叔丁基过氧化物、二枯基过氧化物、叔丁基枯基过氧化物、1,1-二叔丁基过氧化物-3,3,5-三甲基环己烷中的一种。The thermally cured cross-linked hot melt adhesive film according to claim 2, characterized in that the main cross-linking agent is di-tert-butyl peroxide, dicumyl peroxide, or tert-butyl cumyl peroxide. substance, one of 1,1-di-tert-butyl peroxide-3,3,5-trimethylcyclohexane.
  4. 根据权利要求2所述的热固化交联型热熔胶膜，其特征在于，所述辅交联剂为N,N’-亚甲基双丙烯酰胺。The thermosetting cross-linked hot melt adhesive film according to claim 2, characterized in that the auxiliary cross-linking agent is N, N’-methylene bisacrylamide.
  5. 根据权利要求1所述的热固化交联型热熔胶膜，其特征在于，所述酚醛树脂为酚醛-环氧树脂、酚醛环氧乙烯基树脂、苯酚型酚醛环氧树脂、邻甲酚型酚醛环氧树脂中的一种。The thermosetting cross-linked hot melt adhesive film according to claim 1, characterized in that the phenolic resin is phenolic-epoxy resin, phenolic epoxy vinyl resin, phenol type phenolic epoxy resin, o-cresol type A type of phenolic epoxy resin.
  6. 根据权利要求1所述的热固化交联型热熔胶膜，其特征在于，所述耐温填料为云母粉、石英粉、氧化铝或气相白炭黑中的一种。The thermally cured cross-linked hot melt adhesive film according to claim 1, wherein the temperature-resistant filler is one of mica powder, quartz powder, alumina or fumed silica.
  7. 根据权利要求1所述的热固化交联型热熔胶膜，其特征在于，所述导热填料为石墨烯纳米片、膨胀石墨、多壁碳纳米管、六方氮化硼中的一种。The thermally cured cross-linked hot melt adhesive film according to claim 1, wherein the thermally conductive filler is one of graphene nanosheets, expanded graphite, multi-walled carbon nanotubes, and hexagonal boron nitride.
  8. 根据权利要求1所述的热固化交联型热熔胶膜，其特征在于，所述光稳定剂为N,N-双(2,2,6,6-四甲基-4-哌啶基)-1,6-己二胺、双(2,2,6,6-四甲基-4-哌啶基)葵二酸酯和葵二酸双2,2,6,6-四甲基哌啶醇酯中的一种。The thermosetting cross-linked hot melt adhesive film according to claim 1, characterized in that the light stabilizer is N,N-bis(2,2,6,6-tetramethyl-4-piperidinyl) )-1,6-hexanediamine, bis(2,2,6,6-tetramethyl-4-piperidinyl)sebearate and bis2,2,6,6-tetramethylsebearate One of the piperidinol esters.
  9. 一种热固化交联型热熔胶膜的制备方法，其特征在于，包括如下步骤：按配比将各组分添加至搅拌机中进行搅拌，待搅拌后，投入至流延机中进行流延，再经过塑化挤出、拉伸、热固化、牵引、收卷，制得热固化交联型热熔胶膜。A method for preparing a thermally cured cross-linked hot melt adhesive film, which is characterized by including the following steps: adding each component to a mixer according to the proportion and stirring, and after stirring, putting it into a casting machine for casting, Then through plasticizing extrusion, stretching, heat curing, traction, and winding, a heat-curing cross-linked hot-melt adhesive film is obtained.
  10. 根据权利要求9所述的热固化交联型热熔胶膜的制备方法，其特征在于，搅拌的转速为450-600r/min，搅拌的时间为10-20min；流延的温度为100-120℃；热固化交联型热熔胶膜的厚度为0.1-0.25mm。The method for preparing a thermally cured cross-linked hot melt adhesive film according to claim 9, characterized in that the stirring speed is 450-600r/min, the stirring time is 10-20min; the casting temperature is 100-120 ℃; the thickness of the thermally cured cross-linked hot melt adhesive film is 0.1-0.25mm.
PCT/CN2022/112141 2022-07-25 2022-08-12 Thermocuring crosslinking-type hot melt adhesive film and preparation method therefor WO2024021179A1 (en)

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