Heat-conducting composition, epoxy glue heat-conducting component and epoxy glue

Abstract

The invention discloses a heat-conducting composition, an epoxy glue heat-conducting component and epoxy glue. The heat-conducting composition comprises 800-1200 parts of a heat-conducting filler, 40-60 parts of a flame retardant, 1-5 parts of a thixotropic agent and 1-5 parts of a surface treating agent, the heat-conducting filler is a surface-modified compound product; the flame retardant is a surface modified product. Through the mode, the heat-conducting composition, the epoxy glue heat-conducting component and the epoxy glue have high heat-conducting property and high flame-retardant property.

Description

Technical Field

[0001] The present application relates to the technical field of epoxy adhesives, and particularly to a heat-conducting composition, a heat-conducting component of an epoxy adhesive, and an epoxy adhesive. Background Art

[0002] With the development of science and technology, the global electronics industry has penetrated into various fields, and the demand and requirements for electronic products are getting higher and higher. Electronic products are constantly developing towards high performance and miniaturization. The number of components that need to be carried by electronic integrated circuits is increasing, resulting in a sharp rise in the heat dissipation of electronic components during operation, and reducing the service life of electronic components. Therefore, in order to ensure the life and reliability of components, the generated heat must be dissipated in time. Traditional packaging materials include ceramic packaging materials, technical packaging materials, and metal-based packaging materials, which have high thermal conductivity and high mechanical strength and meet the performance requirements of general electronic products. However, they have disadvantages such as complex processing, poor adhesiveness, and poor corrosion resistance, which limit their development in some precision electronic component fields.

[0003] Polymer heat-conducting adhesives are widely used in the field of electronic packaging due to their excellent electrical insulation, fatigue resistance, chemical stability, and easy processability. Polymer heat-conducting adhesives are usually studied with resin adhesives as the base. Commonly used resins include epoxy resins, silicone resins, and polyurethane resins, etc. The research of heat-conducting adhesives can be divided into intrinsic heat-conducting adhesives and filled heat-conducting adhesives according to their research methods.

[0004] Epoxy resin refers to the general name of a class of polymers containing more than two epoxy groups in the molecule. Due to the active chemical properties of the epoxy group, it can be ring-opened with a variety of compounds containing active hydrogen and cured and cross-linked into a network structure. Epoxy adhesives are prepared with epoxy resin as the matrix, and they have a series of advantages such as strong adhesiveness, small curing shrinkage, good corrosion resistance, and good process performance. However, the oxygen index of epoxy resin is relatively low, belonging to a flammable material, and epoxy resin is easy to drip and continue to burn spontaneously after leaving the fire, which is easy to cause a fire. Summary of the Invention

[0005] The heat-conducting composition, the heat-conducting component of the epoxy adhesive, and the epoxy adhesive provided by the present application can achieve a V0-level flame-retardant effect by adding a small amount of inorganic flame retardant to the composition, and at the same time, they also have high heat-conducting performance.

[0006] To solve the above technical problems, the first aspect of the present application provides a heat-conducting composition, including: 800-1200 parts of heat-conducting filler, 40-60 parts of flame retardant, 1-5 parts of thixotropic agent, 1-5 parts of surface treatment agent; the heat-conducting filler is a surface-modified compound product; the flame retardant is a surface-modified product.

[0007] Among them, the thermal conductive filler is alumina; the particle size of the alumina includes at least three kinds of large, medium and small particles, and their weight ratio is (6-9):(0.5-3):(0.5-3).

[0008] Among them, the flame retardant is selected from one or a combination of silica powder, magnesium oxide, aluminum hydroxide, magnesium hydroxide; the surface treatment agent includes one or a combination of γ-glycidoxypropyltrimethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, vinyltri-tert-butylperoxysilane, 3-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltriethoxysilane.

[0009] Among them, the weight ratio of the thermal conductive filler to the flame retardant is (8-12):(0.4-0.6).

[0010] Among them, the modification steps of the thermal conductive filler and the flame retardant include: adding a surface treatment agent to an ethanol aqueous solution with a pH value of 2-4 to completely hydrolyze the surface treatment agent; adding thermal conductive fillers and flame retardants with different particle sizes and stirring under preset conditions; drying the stirred reactants to obtain a mixture of surface-modified thermal conductive fillers and flame retardants; the amount of the surface treatment agent added is 3-5% of the total amount of the thermal conductive filler and the flame retardant.

[0011] To solve the above technical problems, a second aspect of the present application provides an epoxy adhesive thermal conductive component, which includes: 80-100 parts of epoxy resin, 5-15 parts of active diluent, 800-1200 parts of first thermal conductive filler, 40-60 parts of first flame retardant, 1-5 parts of thixotropic agent, 1-5 parts of first surface treatment agent; the first thermal conductive filler is a surface-modified compound product; the first flame retardant is a surface-modified product.

[0012] To solve the above technical problems, a third aspect of the present application provides an epoxy adhesive thermal conductive component, which includes: 80-110 parts of curing agent, 3-8 parts of accelerator, 800-1200 parts of second thermal conductive filler, 40-60 parts of second flame retardant, 1-5 parts of thixotropic agent, 1-5 parts of second surface treatment agent; the second thermal conductive filler is a surface-modified compound product; the second flame retardant is a surface-modified product.

[0013] Among them, the second surface treatment agent includes one or a combination of 3-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltriethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, vinyltri-tert-butylperoxysilane.

[0014] To solve the above technical problems, the fourth aspect of this application provides an epoxy adhesive, which includes component A and component B; Component A includes: 80-100 parts of epoxy resin, 5-15 parts of reactive diluent, 800-1200 parts of first thermal conductive filler, 40-60 parts of first flame retardant, 1-5 parts of thixotropic agent, 1-5 parts of first surface treatment agent; Component B includes: 80-110 parts of curing agent, 3-8 parts of accelerator, 800-1200 parts of second thermal conductive filler, 40-60 parts of second flame retardant, 1-5 parts of thixotropic agent, 1-5 parts of second surface treatment agent; The first thermal conductive filler and the second thermal conductive filler are surface-modified compound products; The first flame retardant and the second flame retardant are surface-modified products, and the components of the first surface treatment agent and the second surface treatment agent are different.

[0015] Among them, component A further includes 1-5 parts of defoaming agent and 0.5-2 parts of pigment, and component B further includes 1-5 parts of defoaming agent.

[0016] Compared with the prior art, the beneficial effects of the thermal conductive composition, the thermal conductive component of the epoxy adhesive, and the epoxy adhesive provided by this application are as follows:

[0017] (1) The thermal conductive filler in the thermal conductive composition is a surface-modified compound product, which can make the thermal conductivity of the thermal conductive composition all above 2.5 Wm -1 K -1 ; At the same time, the compounding of the fillers also helps to reduce the viscosity, the dispensing is smooth, and it is convenient for construction. And under the synergistic effect of different components in the formula, the thermal conductive composition has good flame retardant performance with a small amount of flame retardant used, and can all reach the V0 grade.

[0018] (2) The high thermal conductive and flame retardant two-component epoxy adhesive uses spherical alumina with different particle sizes in compound, and the thermal conductivity of the two-component epoxy adhesive is all above 2.5 Wm -1 K -1 ; At the same time, the compounding of the fillers also helps to reduce the viscosity, the dispensing is smooth, and it is convenient for construction.

[0019] (3) Different surface treatment agents are used for component A and component B of the high thermal conductive and flame retardant two-component epoxy adhesive. At the same time, the thermal conductive fillers and flame retardants of the two components are treated with different surface treatment agents, which helps to improve the dispersibility and filling amount of the thermal conductive fillers and flame retardants, making the two-component epoxy adhesive have excellent storage stability and high thermal conductivity.

[0020] (4) Under the synergistic effect of different components in the formula, the high thermal conductive and flame retardant two-component epoxy adhesive has good flame retardant performance with a small amount of flame retardant used, and can all reach the V0 grade.

[0021] (5) The high thermal conductivity and flame retardant two-component epoxy adhesive used contains surface modified products of alumina and inorganic flame retardants with different particle sizes. Due to the synergistic effect between the flame retardant and alumina, this two-component epoxy adhesive has high thermal conductivity, high flame retardancy, and smooth gluing. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the accompanying drawings required for the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, other accompanying drawings can be obtained based on these drawings without creative efforts.

[0023] Figure 1 It is a schematic flowchart of the first step of modifying the thermal conductive filler and the flame retardant provided by the present application;

[0024] Figure 2 It is a schematic flowchart of an embodiment of the preparation method of the epoxy adhesive provided by the present application;

[0025] Figure 3 It is a schematic flowchart of the first step of modifying the first thermal conductive filler and the first flame retardant provided by the present application;

[0026] Figure 4 It is a schematic flowchart of the first step of modifying the second thermal conductive filler and the second flame retardant provided by the present application. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0027] The present application will be further described in detail below with reference to the accompanying drawings and embodiments. It should be specifically noted that the following embodiments are only used to illustrate the present application, but do not limit the scope of the present application. Similarly, the following embodiments are only partial embodiments of the present application rather than all embodiments. All other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present application.

[0028] In the description of this application, the meaning of "a plurality of" is at least two, such as two, three, etc., unless otherwise specifically defined. The terms "first", "second", and "third" in the embodiments of this application are only for descriptive purposes and cannot be construed as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, features defined with "first", "second", and "third" may explicitly or implicitly include at least one such feature. All directional indications (such as up, down, left, right, front, back...) in the embodiments of this application are only used to explain the relative positional relationship and movement conditions between components in a specific posture (as shown in the drawings). If the specific posture changes, the directional indications will also change accordingly. The terms "include" and "have" and any variations thereof in the embodiments of this application are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that includes a series of steps or units is not limited to the listed steps or units, but may optionally further include unlisted steps or units, or may optionally further include other steps or components inherent to these processes, methods, products, or devices.

[0029] Referring to "embodiments" herein means that a particular feature, structure, or characteristic described in connection with the embodiments can be included in at least one embodiment of this application. The phrase appears in various places in the specification and does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment mutually exclusive with other embodiments. Those skilled in the art will explicitly and implicitly understand that the embodiments described herein can be combined with other embodiments.

[0030] With the development of science and technology, the global electronics industry has penetrated into various fields, and the demand and requirements for electronic products are getting higher and higher. Electronic products are constantly developing towards high performance and miniaturization. The number of components that need to be carried by electronic integrated circuits is increasing, resulting in a sharp rise in the heat dissipation of electronic components during operation and reducing the service life of electronic components. Therefore, in order to ensure the life and reliability of components, the generated heat must be dissipated in a timely manner. Traditional packaging materials include ceramic packaging materials, technical packaging materials, and metal-based packaging materials, which have high thermal conductivity and high mechanical strength and meet the performance requirements of general electronic products. However, they have disadvantages such as complex processing, poor adhesiveness, and poor corrosion resistance, which limit their development in some precision electronic component fields.

[0031] Polymer thermal conductive adhesives are widely used in the field of electronic packaging due to their excellent electrical insulation, fatigue resistance, chemical stability, and easy processability, etc. Polymer thermal conductive adhesives are usually studied with resin adhesives as the base. Commonly used resins include epoxy resins, silicone resins, and polyurethane resins, etc. The research of thermal conductive adhesives can be divided into intrinsic thermal conductive adhesives and filled thermal conductive adhesives according to their research methods.

[0032] Epoxy resin refers to the general term for a class of polymers containing more than two epoxy groups in the molecule. Due to the active chemical properties of the epoxy group, it can be ring-opened with a variety of compounds containing active hydrogen and cured and cross-linked into a network structure. Epoxy adhesives are prepared based on epoxy resin, and they have a series of advantages such as strong adhesion, small curing shrinkage, good corrosion resistance, and good processability. However, the oxygen index of epoxy resin is relatively low, belonging to flammable materials, and epoxy resin is prone to dripping and continues to burn spontaneously after leaving the fire, which is likely to cause a fire.

[0033] Based on this, in this application, the thermal conductive filler of the thermal conductive composition is a surface-modified compound product; the flame retardant is a surface-modified product, so that under the synergistic effect of different components in the formula of the thermal conductive composition, adding a small amount of inorganic flame retardant to the thermal conductive composition can achieve a V0-level flame retardant effect, and at the same time it also has high thermal conductivity. For specific reference, see any of the following technical solutions.

[0034] An embodiment of this application provides a thermal conductive composition, including: 800-1200 parts of thermal conductive filler, such as 800, 850, 900, 950, 1000, 1050, 1100, 1200 parts by weight or any value between them; 40-60 parts of flame retardant, such as 40, 45, 50, 55, 60 parts by weight or any value between them; 1-5 parts of thixotropic agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them; 1-5 parts of surface treatment agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them.

[0035] Among them, the thermal conductive filler is a surface-modified compound product; the flame retardant is a surface-modified product.

[0036] The thermal conductive filler is a surface-modified compound product, which can make the thermal conductivity of the thermal conductive composition all above 2.5Wm -1 K -1 above; at the same time, the compounding of the filler also helps to reduce the viscosity, make the dispensing smooth, and facilitate construction.

[0037] Furthermore, when a small amount of flame retardant is used in the thermal conductive composition, it has good flame retardant performance under the synergistic effect of different components in the formula and can all reach the V0 level.

[0038] In some embodiments, the thermal conductive filler may include thermal conductive fillers with different particle sizes. For example, the thermal conductive filler is alumina; the particle size of alumina includes at least three types of large, medium, and small particles, and their weight ratio is (6-9):(0.5-3):(0.5-3). Such as 6:2:2, 6:3:1, 6:1:3, 7:1:2, 7:2:1, 8:1:1, 9:0.5:0.5, etc. For example, the particle sizes of alumina can be 13μm, 5μm, and 2μm respectively. For example, the particle sizes of alumina can be 15μm, 6μm, and 3μm respectively. For example, the particle sizes of alumina can be 13μm, 6μm, and 1μm respectively. However, it is not limited to the listed values, and the combinations not listed within this range are also applicable.

[0039] In some embodiments, the flame retardant is selected from one or more combinations of silica powder, magnesium oxide, aluminum hydroxide, and magnesium hydroxide. In other embodiments, the first flame retardant and the second flame retardant can be aluminum hydroxide.

[0040] In some embodiments, the surface treatment agent includes one or more combinations of γ-glycidoxypropyltrimethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, vinyltri-tert-butylperoxysilane, 3-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltriethoxysilane. In other embodiments, the surface treatment agent is γ-glycidoxypropyltrimethoxysilane.

[0041] In some embodiments, the weight ratio of the thermal conductive filler to the flame retardant is (8-12):(0.4-0.6). Such as 8:0.4, 8:0.6, 9:0.4, 9:0.6, 10:0.4, 10:0.6, 11:0.4, 11:0.6, 12:0.4 or 12:0.6, etc. It can be understood that the above types are only for illustrative purposes, and the combinations not listed within this range are also applicable.

[0042] Refer to Figure 1 , the modification steps of the thermal conductive filler and the flame retardant are described as follows:

[0043] Step 11: Add the surface treatment agent to the ethanol aqueous solution with a pH value of 2-4 to completely hydrolyze the surface treatment agent.

[0044] In some embodiments, prepare an ethanol aqueous solution with a pH value of 2-4, add the surface treatment agent, and mechanically stir for more than 1 h to ensure complete hydrolysis of the surface treatment agent.

[0045] Step 12: Add thermal conductive fillers and flame retardants with different particle sizes and stir under preset conditions.

[0046] In some embodiments, the preset conditions can be stirring at 90°C - 100°C for 1 - 4 h.

[0047] Step 13: Dry the reacted mixture to obtain a mixture of surface-modified thermal conductive filler and flame retardant.

[0048] Wherein, the amount of the surface treatment agent added is 3-5% of the total amount of the thermal conductive filler and the flame retardant. Such as 3%, 3.5%, 4%, 4.5%, 5%, etc., but not limited to the listed values, and the combinations not listed within this range are also applicable.

[0049] Wherein, the thermal conductive composition of the embodiment of the present application can be added as an additive to epoxy glue and polypropylene colloid, which can effectively improve the thermal conductivity of the colloid.

[0050] The embodiment of the present application provides a thermal conductive component for epoxy glue, and the thermal conductive component for epoxy glue includes: 80-100 parts of epoxy resin, such as 80, 85, 90, 95, 100 parts by weight or any value between them; 5-15 parts of active diluent, such as 5, 8, 10, 13, 15 parts by weight or any value between them; 800-1200 parts of the first thermal conductive filler, such as 800, 850, 900, 950, 1000, 1050, 1100, 1200 parts by weight or any value between them; 40-60 parts of the first flame retardant, such as 40, 45, 50, 55, 60 parts by weight or any value between them; 1-5 parts of thixotropic agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them; 1-5 parts of the first surface treatment agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them.

[0051] The first thermal conductive filler is a surface-modified compound product; the first flame retardant is a surface-modified product.

[0052] In some embodiments, the first thermal conductive filler can use thermal conductive fillers with different particle sizes, and the first thermal conductive filler is a surface-modified compound product, which can make the thermal conductivity of the thermal conductive component of epoxy glue all above 2.5Wm -1 K -1 Above; at the same time, the filler compounding also helps to reduce the viscosity, enables smooth dispensing, and is convenient for construction.

[0053] Furthermore, when a small amount of flame retardant is used in the thermal conductive component of epoxy glue, it has good flame retardant performance under the synergistic effect of different components in the formula, and can all reach the V0 grade.

[0054] In some embodiments, the above-mentioned first surface treatment agent includes one or a combination of more of γ-glycidoxypropyltrimethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, vinyltri-tert-butylperoxysilane. In other embodiments, the first surface treatment agent is γ-glycidoxypropyltrimethoxysilane.

[0055] In some embodiments, the first thermal conductive filler may include thermal conductive fillers with different particle sizes. For example, the thermal conductive filler is alumina; the particle size of alumina includes at least three types of large, medium, and small particles, and their weight ratio is (6-9):(0.5-3):(0.5-3). Such as 6:2:2, 6:3:1, 6:1:3, 7:1:2, 7:2:1, 8:1:1, 9:0.5:0.5, etc. For example, the particle sizes of alumina can be 13μm, 5μm, and 2μm respectively. For example, the particle sizes of alumina can be 15μm, 6μm, and 3μm respectively. For example, the particle sizes of alumina can be 13μm, 6μm, and 1μm respectively. However, it is not limited to the listed values, and the combinations not listed within this range are also applicable.

[0056] Among them, the thermal conductive component of the epoxy adhesive in the embodiments of the present application can be used as the A component in the AB adhesive and mixed with the curing agent (B component) to achieve curing and form a highly thermal conductive epoxy adhesive layer.

[0057] The embodiments of the present application provide a thermal conductive component of an epoxy adhesive, and the thermal conductive component of the epoxy adhesive includes: 80-110 parts of a curing agent, such as 80, 85, 90, 95, 100 parts by weight or any value between them; 3-8 parts of an accelerator, such as 3, 4, 5, 6, 7, 8 parts by weight or any value between them; 800-1200 parts of a second thermal conductive filler, such as 800, 850, 900, 950, 1000, 1050, 1100, 1200 parts by weight or any value between them; 40-60 parts of a second flame retardant, such as 40, 45, 50, 55, 60 parts by weight or any value between them; 1-5 parts of a thixotropic agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them; 1-5 parts of a second surface treatment agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them.

[0058] The second thermal conductive filler is a surface-modified compound product; the second flame retardant is a surface-modified product.

[0059] In some embodiments, the second thermal conductive filler can use thermal conductive fillers with different particle sizes, and the second thermal conductive filler is a surface-modified compound product, which can make the thermal conductivity of the thermal conductive component of the epoxy adhesive all above 2.5Wm -1 K -1 above; at the same time, the filler compounding also helps to reduce the viscosity, the dispensing is smooth, and it is convenient for construction.

[0060] Furthermore, when a small amount of flame retardant is used in the thermal conductive component of the epoxy adhesive, it has good flame retardant performance under the synergistic effect of different components in the formula, and can all reach the V0 grade.

[0061] In some embodiments, the above-mentioned second surface treatment agent includes one or a combination of more than one of 3-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltriethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, vinyltri-tert-butylperoxysilane. In other embodiments, the second surface treatment agent is γ-aminopropyltriethoxysilane.

[0062] In some embodiments, the second heat-conducting filler may include heat-conducting fillers with different particle sizes. For example, the heat-conducting filler is alumina; the particle size of alumina includes at least three types of large, medium, and small particles, and their weight ratio is (6-9):(0.5-3):(0.5-3). Such as 6:2:2, 6:3:1, 6:1:3, 7:1:2, 7:2:1, 8:1:1, 9:0.5:0.5, etc. For example, the particle sizes of alumina can be 13μm, 5μm, 2μm respectively. For example, the particle sizes of alumina can be 15μm, 6μm, 3μm respectively. For example, the particle sizes of alumina can be 13μm, 6μm, 1μm respectively. However, it is not limited to the listed values, and the combinations not listed within this range are also applicable.

[0063] Among them, the epoxy adhesive heat-conducting group of the embodiments of the present application can be used as the curing agent (component B) in the AB adhesive, and is mixed with the A component of other epoxy adhesives to achieve curing and form a high-heat-conducting epoxy adhesive layer.

[0064] The embodiments of the present application provide an epoxy adhesive, which includes component A and component B.

[0065] Component A includes: 80-100 parts of epoxy resin, such as 80, 85, 90, 95, 100 parts by weight or any value between them; 5-15 parts of active diluent, such as 5, 8, 10, 13, 15 parts by weight or any value between them; 800-1200 parts of the first heat-conducting filler, such as 800, 850, 900, 950, 1000, 1050, 1100, 1200 parts by weight or any value between them; 40-60 parts of the first flame retardant, such as 40, 45, 50, 55, 60 parts by weight or any value between them; 1-5 parts of thixotropic agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them; 1-5 parts of the first surface treatment agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them.

[0066] Component B includes: 80 - 110 parts of curing agent, such as 80, 85, 90, 95, 100 parts by weight or any value between them; 3 - 8 parts of accelerator, such as 3, 4, 5, 6, 7, 8 parts by weight or any value between them; 800 - 1200 parts of second heat-conducting filler, such as 800, 850, 900, 950, 1000, 1050, 1100, 1200 parts by weight or any value between them; 40 - 60 parts of second flame retardant, such as 40, 45, 50, 55, 60 parts by weight or any value between them; 1 - 5 parts of thixotropic agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them; 1 - 5 parts of second surface treatment agent, such as 1, 2, 3, 4, 5 parts by weight or any value between them.

[0067] Among them, the first heat-conducting filler and the second heat-conducting filler are surface-modified compound products; the first flame retardant and the second flame retardant are surface-modified products, and the components of the first surface treatment agent and the second surface treatment agent are different.

[0068] In some embodiments, the first heat-conducting filler and / or the second heat-conducting filler are heat-conducting fillers with different particle sizes, and the first heat-conducting filler and the second heat-conducting filler are surface-modified compound products, which can make the thermal conductivity of the epoxy adhesive all above 2.5Wm -1 K -1 above; at the same time, the compounding of the fillers also helps to reduce the viscosity, make the dispensing smooth, and facilitate construction.

[0069] Furthermore, different surface treatment agents are used for Component A and Component B of the epoxy adhesive. At the same time, the heat-conducting fillers and flame retardants of Component A and Component B are treated with different surface treatment agents, which helps to improve the dispersibility and filling amount of the heat-conducting fillers and flame retardants, and makes the two-component epoxy adhesive have excellent storage stability and high thermal conductivity.

[0070] Furthermore, when a small amount of flame retardant is used in the epoxy adhesive, it has good flame retardant performance under the synergistic effect between different components of the formula, and can all reach the V0 grade.

[0071] Furthermore, due to the epoxy adhesive containing heat-conducting fillers with different particle sizes and surface-modified products of flame retardants, due to the synergistic effect between the flame retardant and the preferably matched alumina, the two-component epoxy adhesive has high thermal conductivity and high flame retardant performance, and the dispensing is smooth.

[0072] In some embodiments, the first heat-conducting filler and / or the second heat-conducting filler is alumina; the particle sizes of the alumina are 13μm, 5μm, 2μm respectively, and their weight ratio is (6 - 9):(0.5 - 3):(0.5 - 3). Such as 6:2:2, 6:3:1, 6:1:3, 7:1:2, 7:2:1, 8:1:1, 9:0.5:0.5, etc., but not limited to the listed values, and the combinations not listed within this range are also applicable.

[0073] In some embodiments, the first flame retardant and the second flame retardant are respectively selected from one or more combinations of silica powder, magnesium oxide, aluminum hydroxide, and magnesium hydroxide. In other embodiments, the first flame retardant and the second flame retardant can be aluminum hydroxide.

[0074] In some embodiments, the first surface treatment agent includes one or more combinations of γ-glycidoxypropyltrimethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, and vinyltri-tert-butylperoxysilane. In other embodiments, the first surface treatment agent is γ-glycidoxypropyltrimethoxysilane.

[0075] In some embodiments, the second surface treatment agent includes one or more combinations of 3-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltriethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, and vinyltri-tert-butylperoxysilane. In other embodiments, the second surface treatment agent is γ-aminopropyltriethoxysilane.

[0076] In some embodiments, the weight ratio of the first thermal conductive filler to the first flame retardant or the second thermal conductive filler to the second flame retardant is (8 - 12):(0.4 - 0.6). Such as 8:0.4, 8:0.6, 9:0.4, 9:0.6, 10:0.4, 10:0.6, 11:0.4, 11:0.6, 12:0.4, or 12:0.6, etc. It can be understood that the above types are only used for illustration, and the combinations not listed within this range are equally applicable.

[0077] In some embodiments, the above-mentioned epoxy resin may include one or more combinations of bisphenol A epoxy resin, bisphenol F epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, and alicyclic epoxy resin.

[0078] In some embodiments, the above-mentioned reactive diluent includes one or more combinations of 1,4-butanediol diglycidyl ether, polypropylene glycol diglycidyl ether, C10 - C14 alkyl glycidyl ether, o-tolyl glycidyl ether, benzyl glycidyl ether, 1,4-cyclohexanedimethanol diglycidyl ether, castor oil triglycidyl ether, and pentaerythritol tetraglycidyl ether. In other embodiments, the reactive diluent is 1,4-butanediol diglycidyl ether.

[0079] In some embodiments, the above-mentioned thixotropic agent includes one or more combinations of modified castor oil, organic bentonite, polyamide wax, and fumed silica. In other embodiments, the thixotropic agent is fumed silica.

[0080] In some embodiments, the above-mentioned curing agent includes one or a combination of more than one of fatty amines, modified fatty amines, modified alicyclic amines, modified aromatic amines, and phenolic amines. In other embodiments, the curing agent is a modified fatty amine.

[0081] In some embodiments, the above-mentioned accelerator includes one or a combination of more than one of 2,4,6-tris(dimethylaminomethyl)phenol, benzyldimethylamine, 2-methylimidazole, 2-phenylimidazole, and 2-ethyl-4-methylimidazole.

[0082] In other embodiments, Component A further includes 1 to 5 parts of defoamer and 0.5 to 2 parts of pigment, and Component B further includes 1 to 5 parts of defoamer.

[0083] In some embodiments, the above-mentioned defoamer includes one or a combination of more than one of silicone defoamers, polyether defoamers, and mineral oil defoamers.

[0084] Refer to Figure 2 , Figure 2 which is a schematic flow chart of an embodiment of the preparation method of the epoxy adhesive provided by this application. The epoxy adhesive includes Component A and Component B, and the preparation method includes:

[0085] Step 21: Respectively add 80 to 100 parts of epoxy resin, 5 to 15 parts of reactive diluent, 800 to 1200 parts of first thermal conductive filler, 40 to 60 parts of first flame retardant, 1 to 5 parts of thixotropic agent, and 1 to 5 parts of first surface treatment agent into a stirring kettle, and stir until completely dispersed and uniform; place the stirred glue solution in a planetary homogenizer for mixing and defoaming, and after defoaming is completed, Component A is obtained.

[0086] Step 22: Respectively add 80 to 110 parts of curing agent, 3 to 8 parts of accelerator, 800 to 1200 parts of second thermal conductive filler, 40 to 60 parts of second flame retardant, 1 to 5 parts of thixotropic agent, and 1 to 5 parts of second surface treatment agent into a stirring kettle, and stir until completely dispersed and uniform; place the stirred glue solution in a planetary homogenizer for mixing and defoaming, and after defoaming is completed, Component B is obtained.

[0087] Among them, the first thermal conductive filler and the second thermal conductive filler are surface-modified compound products; the first flame retardant and the second flame retardant are surface-modified products, and the components of the first surface treatment agent and the second surface treatment agent are different.

[0088] The defoaming in the above Step 21 and Step 22 is divided into three stages.

[0089] The first stage: 600 rpm to 800 rpm / 60 s to 120 s, such as 600 rpm / 60 s, 600 rpm / 120 s, 700 rpm / 60 s, 700 rpm / 120 s, 800 rpm / 60 s, 800 rpm / 120 s, etc., but not limited to the listed values, and the combinations not listed within this range are equally applicable.

[0090] The second stage: 1000 rpm to 1200 rpm / 120 s to 240 s, such as 1000 rpm / 120 s, 1000 rpm / 240 s, 1100 rpm / 120 s, 1100 rpm / 240 s, 1200 rpm / 120 s, 1200 rpm / 240 s, etc., but not limited to the listed values, and the combinations not listed within this range are equally applicable.

[0091] The third stage: 600 rpm to 800 rpm / 60 s to 120 s, such as 600 rpm / 60 s, 600 rpm / 120 s, 700 rpm / 60 s, 700 rpm / 120 s, 800 rpm / 60 s, 800 rpm / 120 s, etc., but not limited to the listed values, and the combinations not listed within this range are equally applicable.

[0092] Vacuum degree: 5 kPa to 10 kPa, such as 5 kPa, 6 kPa, 7 kPa, 8 kPa, 9 kPa, 10 kPa, etc., but not limited to the listed values, and the combinations not listed within this range are equally applicable.

[0093] Refer to Figure 3 , the modification steps of the first thermal conductive filler and the first flame retardant include:

[0094] Step 31: Add the first surface treatment agent to the ethanol aqueous solution with a pH value of 2 to 4 to completely hydrolyze the first surface treatment agent.

[0095] In some embodiments, prepare an ethanol aqueous solution with a pH value of 2 to 4, add the first surface treatment agent, and mechanically stir for more than 1 h to ensure complete hydrolysis of the first surface treatment agent.

[0096] Among them, the amount of the first surface treatment agent added is 3% to 5% of the total amount of the first thermal conductive filler and the first flame retardant. Such as 3%, 3.5%, 4%, 4.5%, 5%, etc., but not limited to the listed values, and the combinations not listed within this range are equally applicable.

[0097] Step 32: Add the first thermal conductive filler and the first flame retardant with different particle sizes and stir under preset conditions.

[0098] In some embodiments, the preset conditions can be stirring at 90 °C to 100 °C for 1 to 4 h.

[0099] Step 33: Dry the reacted mixture to obtain a mixture of the surface-modified first thermal conductive filler and the first flame retardant.

[0100] Refer to Figure 4 , and the modification steps of the second thermal conductive filler and the second flame retardant include:

[0101] Step 41: Add a second surface treatment agent to an ethanol aqueous solution with a pH value of 2-4 to completely hydrolyze the second surface treatment agent.

[0102] In some embodiments, prepare an ethanol aqueous solution with a pH value of 2-4, add the second surface treatment agent, and mechanically stir for more than 1 h to ensure complete hydrolysis of the second surface treatment agent.

[0103] In some embodiments, the amount of the second surface treatment agent added during the treatment of the second thermal conductive filler and the second flame retardant is also 3-5% of the total amount of the second thermal conductive filler and the second flame retardant, such as 3%, 3.5%, 4%, 4.5%, 5%, etc., but not limited to the listed values, and the combinations not listed within this range are equally applicable.

[0104] Step 42: Add second thermal conductive fillers and second flame retardants with different particle sizes and stir under preset conditions.

[0105] Step 43: Dry the reacted mixture to obtain a mixture of the surface-modified second thermal conductive filler and the second flame retardant.

[0106] The amount of the second surface treatment agent added during the treatment of the second thermal conductive filler and the second flame retardant is also 3-5% of the total amount of the second thermal conductive filler and the second flame retardant.

[0107] In some embodiments, the embodiments of the present application further provide a sealant, and the sealant includes the epoxy adhesive provided in any embodiment of the present application or the epoxy adhesive prepared by using the preparation method provided in any of the above embodiments.

[0108] In some embodiments, the embodiments of the present application further provide an adhesive, and the adhesive includes the epoxy adhesive provided in any embodiment of the present application or the epoxy adhesive prepared by using the preparation method provided in any of the above embodiments.

[0109] The raw materials and their sources used in the following examples and comparative examples are as follows:

[0110] Epoxy resin: Bisphenol A epoxy resin, grade jER-828, sourced from Mitsubishi Chemical; diluent, 1,4-butanediol diglycidyl ether, grade DENACOL EX-214, sourced from Nagase of Japan; thermal conductive filler, spherical alumina, sourced from Admatechs of Japan; flame retardant, aluminum hydroxide, from Guangdong Kinggo; thixotropic agent, fumed silica, grade TS-610, sourced from Cabot; surface treatment agent, γ-glycidoxypropyltrimethoxysilane, grade KH-560 and γ-aminopropyltriethoxysilane, grade KH-550, sourced from Nanjing Shuguang Chemical Industry; defoamer, grade BYK-141, sourced from BYK-Chemie; pigment, carbon black, sourced from Kayin Chemical; curing agent, modified aliphatic amine, grade and sourced from Huntsman; accelerator, grade DMP-30, sourced from Changzhou Shanfeng.

[0111] Examples 1-13

[0112] (1) Prepare raw materials according to the components and weight parts in Table 1 and Table 2 respectively.

[0113] (2) Modification of the first thermal conductive filler and the first flame retardant:

[0114] Add γ-glycidoxypropyltrimethoxysilane to an ethanol aqueous solution with a pH value of 2-4, and mechanically stir for 3 h; then, add 100 parts of 13 μm spherical alumina, 5 μm spherical alumina, 2 μm spherical alumina and aluminum hydroxide, and stir at 80 °C for 1 h; finally, dry the reaction product to obtain the modified mixture of the first thermal conductive filler and the first flame retardant.

[0115] (3) Modification steps of the second thermal conductive filler and the second flame retardant:

[0116] Add γ-aminopropyltriethoxysilane to an ethanol aqueous solution with a pH value of 2-4, and mechanically stir for 3 h; then, add 13 μm spherical alumina, 5 μm spherical alumina, 2 μm spherical alumina and aluminum hydroxide, and stir at 80 °C for 1 h; finally, dry the reaction product to obtain the modified mixture of the second thermal conductive filler and the second flame retardant.

[0117] (4) Preparation of high thermal conductivity and flame retardant two-component epoxy adhesive:

[0118] Add epoxy resin, diluent, the above-mentioned modified and dried first thermal conductive filler and first flame retardant modified mixture, thixotropic agent, surface treatment agent, defoaming agent and pigment into a stirring kettle, stir at 800 rpm until completely dispersed and uniform; place the stirred glue solution in a planetary homogenizer for mixing and defoaming. The defoaming process is divided into three stages: the first stage is 600 rpm / 60 s, the second stage is 1200 rpm / 120 s, the third stage is 600 rpm / 60 s, and the vacuum degree is 5 kPa; after defoaming is completed, component A can be obtained.

[0119] Add curing agent, accelerator, the above-mentioned modified and dried second thermal conductive filler and second flame retardant modified mixture, thixotropic agent, surface treatment agent, defoaming agent into a stirring kettle, stir at 800 rpm until completely dispersed and uniform; place the stirred glue solution in a planetary homogenizer for mixing and defoaming. The defoaming process is divided into three stages: the first stage is 600 rpm / 60 s, the second stage is 1200 rpm / 120 s, the third stage is 600 rpm / 60 s, and the vacuum degree is 5 kPa; after defoaming is completed, component B can be obtained.

[0120] Compared with Example 1, the difference in Comparative Example 1 is only that the treatment of the thermal conductive filler and the flame retardant in steps (2) and (3) is not carried out.

[0121] Compared with Example 1, the difference in Comparative Examples 2-4 is only that only one kind of thermal conductive filler is added in steps (2) and (3).

[0122] Compared with Example 1, the difference in Comparative Examples 5-11 is that the parts by weight of the added components are different.

[0123] Table 1 Formulation table of high thermal conductivity and flame retardant two-component epoxy adhesive for component A in Examples 1-13 and Comparative Examples 1-11

[0124]

[0127] Table 2 Formulation table of high thermal conductivity and flame retardant two-component epoxy adhesive for component B in Examples 1-13 and Comparative Examples 1-11

[0128]

[0129] Table 2 Formulation table of high thermal conductivity and flame retardant two-component epoxy adhesive for component B in Examples 1-13 and Comparative Examples 1-11

[0130] Test Example

[0131] 1. Glue application amount:

[0132] The prepared Component A and Component B were separately filled into 50 mL two-component rubber tubes, which were placed vertically with the glue outlet facing down at room temperature for 7 days and then tested. During the test, the glue was extruded through a mixing tube, and the mass of the glue extruded within 10 s was weighed with a balance. The pushing force used during extrusion was fixed at about 200 N.

[0133] 2. Thermal conductivity:

[0134] (1) Preparation of the thermal conductivity test sample

[0135] Component A and Component B were mixed evenly at a mass ratio of 1:1, and then the evenly mixed glue was poured into a mold and cured at room temperature for 24 h to obtain the test sample. Sample requirements: diameter 30 mm, thickness ≤ 5 mm, and the surface was flat and smooth.

[0136] (2) Test process

[0137] A layer of thermal conductive silicone grease was coated on the surface of the prepared sample, and then it could be put into the equipment to start the test. The test process was carried out according to the standard ASTM D5470. The equipment used for the test was the Xiangtan Instrument DRL-V type thermal conductivity tester, with the cold pole temperature of 30 °C, the hot pole temperature of 70 °C, and the test pressure of 200 N.

[0138] 3. Flame retardancy:

[0139] (1) Preparation of the flame retardancy test sample

[0140] Component A and Component B were mixed evenly at a mass ratio of 1:1, and then the evenly mixed glue was poured into a mold and cured at room temperature for 24 h to obtain the test sample. Sample requirements: length 125 mm, width 13 mm, thickness 1.5 mm, and there were few bubbles on the surface of the sample.

[0141] (2) Test process

[0142] The prepared sample needed to be placed in an environment with a temperature of 23 ± 2 °C and a humidity of 50 ± 10% RH for 48 h before the test could be carried out. The entire test process was carried out according to the standard UL 94-2013.

[0143] Table 3 Performance test data of the preparation examples and the examples

[0144]

[0145]

[0146] By analyzing Comparative Example 1 and Example 1, it can be seen that the treatment of the thermal conductive filler before and after the preparation of the two-component epoxy adhesive has a great impact on the amount of glue applied. The thermal conductive filler added in the preparation of the two-component epoxy adhesive is not surface-modified and is prone to sedimentation, resulting in clogging of the pipe orifice at the bottom after being placed vertically for 7 days, and the amount of glue applied is 0 g. At the same time, affected by the sedimentation of the thermal conductive filler, the uniformity of the distribution of the thermal conductive filler becomes poor, resulting in a thermal conductivity of less than 2.5 Wm -1 K -1 and the flame retardant rating is only V1.

[0147] By analyzing Example 1 and Comparative Examples 2-4, it can be seen that when only a single particle size of thermal conductive filler is added in the preparation of the two-component epoxy adhesive, the thermal conductivity is significantly reduced, and the thermal conductivity does not reach 2.0 Wm -1 K -1 , the flame retardancy t 1 <5 s and t 2 <5 s, and the amount of glue applied is less than 10 g.

[0148] By analyzing Example 1 and Comparative Examples 5-6, it can be seen that when other components remain unchanged and the compounding ratio of the thermal conductive filler remains unchanged, when the amount of the thermal conductive filler is too small, the thermal conductivity decreases due to the decrease in the filler content, and the amount of glue applied and the flame retardancy also decrease slightly; while when the amount of the thermal conductive filler is too large, it is difficult to improve the thermal conductivity, and due to the large proportion of the filler content, the amount of glue applied does not exceed 10 g, and the flame retardancy t 1 <5 s and t 2 <5 s.

[0149] From Examples 2-7, it can be seen that when other components remain unchanged, the thermal conductivity of the treated thermal conductive filler can reach more than 2.5 Wm -1 K -1 and the amount of glue applied is more than 10 g, and at the same time the flame retardant performance also reaches the V0 level.

[0150] By analyzing Example 1 and Comparative Examples 10-11, it can be seen that when other components remain unchanged in the preparation of the two-component epoxy adhesive, when the compounding ratio of the thermal conductive filler exceeds the range, the thermal conductivity is significantly reduced, even lower than 2.0 Wm -1 K -1 , and the flame retardancy and the amount of glue applied decrease slightly.

[0151] From Examples 8-11, it can be seen that when the number of components is reasonably changed in the preparation of the two-component epoxy adhesive, the thermal conductivity is close to 3.0 Wm -1 K -1 , the amount of glue applied can also reach more than 12 g, and at the same time the flame retardant performance also reaches the V0 level.

[0152] It can be seen from Examples 12 to 13 that when the amount of flame retardant filler is changed between 40 and 60 parts during the preparation of the two-component epoxy adhesive, the thermal conductivity is greater than 2.5 Wm -1 K -1 , the amount of glue applied is greater than 10 g, and at the same time, the flame retardant performance also reaches V0 grade.

[0153] By comparative analysis of Example 1 and Comparative Examples 7 to 9, when no flame retardant is added or 20 parts of flame retardant are added, the flame retardant grade does not reach V0; when 80 parts of flame retardant are added, the flame retardancy can meet the requirements, but it will cause the poor uniformity of filler distribution and the thermal conductivity is less than 2.5 Wm -1 K -1 , and the amount of glue applied is less than 10 g.

[0154] Compared with Example 1, Example 14 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 800 parts.

[0155] Compared with Example 1, Example 15 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 900 parts.

[0156] Compared with Example 1, Example 16 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1100 parts.

[0157] Compared with Example 1, Example 17 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1200 parts.

[0158] Compared with Example 2, Example 18 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 800 parts.

[0159] Compared with Example 2, Example 19 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 900 parts.

[0160] Compared with Example 2, Example 20 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1100 parts.

[0161] Compared with Example 2, Example 21 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1200 parts.

[0162] Compared with Example 3, Example 22 is mostly the same, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 800 parts.

[0163] Example 23 is mostly the same as Example 3, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 900 parts.

[0164] Example 24 is mostly the same as Example 3, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1100 parts.

[0165] Example 25 is mostly the same as Example 3, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1200 parts.

[0166] Example 26 is mostly the same as Example 4, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 800 parts.

[0167] Example 27 is mostly the same as Example 4, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 900 parts.

[0168] Example 28 is mostly the same as Example 4, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1100 parts.

[0169] Example 29 is mostly the same as Example 4, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1200 parts.

[0170] Example 30 is mostly the same as Example 5, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 800 parts.

[0171] Example 31 is mostly the same as Example 5, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 900 parts.

[0172] Example 33 is mostly the same as Example 5, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1100 parts.

[0173] Example 34 is mostly the same as Example 5, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1200 parts.

[0174] Example 34 is mostly the same as Example 6, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 800 parts.

[0175] Example 35 is mostly the same as Example 6, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 900 parts.

[0176] Example 36 is mostly the same as Example 6, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1100 parts.

[0177] Example 37 is mostly the same as Example 6, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1200 parts.

[0178] Example 38 is mostly the same as Example 7, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 800 parts.

[0179] Example 39 is mostly the same as Example 7, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 900 parts.

[0180] Example 40 is mostly the same as Example 7, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1100 parts.

[0181] Example 41 is mostly the same as Example 7, except that in this example, the total amount of thermal conductive filler in Component A and Component B is adjusted to 1200 parts.

[0182] Example 42 is mostly the same as Example 2, except that in this example, the amount of flame retardant in Component A and Component B is adjusted to 40 parts.

[0183] Example 43 is mostly the same as Example 2, except that in this example, the amount of flame retardant in Component A and Component B is adjusted to 60 parts.

[0184] Example 44 is mostly the same as Example 3, except that in this example, the amount of flame retardant in Component A and Component B is adjusted to 40 parts.

[0185] Example 45 is mostly the same as Example 3, except that in this example, the amount of flame retardant in Component A and Component B is adjusted to 60 parts.

[0186] Example 46 is mostly the same as Example 4, except that in this example, the amount of flame retardant in Component A and Component B is adjusted to 40 parts.

[0187] Example 47 is mostly the same as Example 4, except that in this example, the amount of flame retardant in Component A and Component B is adjusted to 60 parts.

[0188] Example 48 is mostly the same as Example 5, except that in this example, the amount of flame retardant in Component A and Component B is adjusted to 40 parts.

[0189] Example 49 is mostly the same as Example 5, except that in this example, the amounts of flame retardants in Component A and Component B are adjusted to 60 parts.

[0190] Example 50 is mostly the same as Example 6, except that in this example, the amounts of flame retardants in Component A and Component B are adjusted to 40 parts.

[0191] Example 50 is mostly the same as Example 6, except that in this example, the amounts of flame retardants in Component A and Component B are adjusted to 60 parts.

[0192] Example 51 is mostly the same as Example 7, except that in this example, the amounts of flame retardants in Component A and Component B are adjusted to 60 parts.

[0193] Example 52 is mostly the same as Example 7, except that in this example, the amounts of flame retardants in Component A and Component B are adjusted to 60 parts.

[0194] Example 53 is mostly the same as Example 1, except that in this example, the first surface treatment agent of Component A is replaced with γ-(methacryloyloxy)propyltrimethoxysilane.

[0195] Example 54 is mostly the same as Example 1, except that in this example, the first surface treatment agent of Component A is replaced with vinyltri-tert-butylperoxysilane.

[0196] Example 55 is mostly the same as Example 1, except that in this example, the second surface treatment agent of Component B is replaced with 3-aminopropyltrimethoxysilane.

[0197] Example 56 is mostly the same as Example 1, except that in this example, the second surface treatment agent of Component B is replaced with γ-mercaptopropyltriethoxysilane.

[0198] Example 57 is mostly the same as Example 1, except that in this example, the second surface treatment agent of Component B is replaced with γ-(methacryloyloxy)propyltrimethoxysilane.

[0199] Example 58 is mostly the same as Example 1, except that in this example, the second surface treatment agent of Component B is replaced with vinyltri-tert-butylperoxysilane.

[0200] Example 59 is mostly the same as Example 1, except that in this example, the flame retardant coupling agent in Component A and Component B is replaced with silica powder.

[0201] Example 60 is mostly the same as Example 1, except that in this example, the flame retardant coupling agent in Component A and Component B is adjusted and replaced with magnesium oxide.

[0202] Example 61 is mostly the same as Example 1, except that in this example, the flame retardant coupling agent in Component A and Component B is adjusted and replaced with magnesium hydroxide.

[0203] Example 62 is mostly the same as Example 1, except that in this example, the stirring is carried out at 100 °C in the modification step of the first thermal conductive filler and the first flame retardant.

[0204] Example 63 is mostly the same as Example 1, except that in this example, the stirring is carried out at 100 °C in the modification step of the second thermal conductive filler and the second flame retardant.

[0205] Example 64 is mostly the same as Example 1, except that in this example, the stirring is carried out at 90 °C in the modification step of the first thermal conductive filler and the first flame retardant.

[0206] Example 65 is mostly the same as Example 1, except that in this example, the stirring is carried out at 90 °C in the modification step of the second thermal conductive filler and the second flame retardant.

[0207] In summary, the epoxy adhesive, its preparation method, sealant, and adhesive provided by this application use a high thermal conductivity and flame retardant two-component epoxy adhesive by compounding spherical alumina with different particle sizes. The thermal conductivity of this two-component epoxy adhesive is above 2.5 Wm -1 K -1 -1; at the same time, the compounding of fillers also helps to reduce the viscosity, enables smooth dispensing, and is convenient for construction.

[0208] Furthermore, different surface treatment agents are used for Component A and Component B of the high thermal conductivity and flame retardant two-component epoxy adhesive, and at the same time, the thermal conductive fillers and flame retardants of the two components are treated with different surface treatment agents, which helps to improve the dispersibility and filling amount of the thermal conductive fillers and flame retardants, and enables the two-component epoxy adhesive to have excellent storage stability and high thermal conductivity performance.

[0209] Furthermore, when a small amount of flame retardant is used in the high thermal conductivity and flame retardant two-component epoxy adhesive, it has good flame retardant performance under the synergistic effect between different components of the formula, and can all reach the V0 grade.

[0210] Furthermore, since the high thermal conductivity and flame retardant two-component epoxy adhesive contains surface modified products of alumina and inorganic flame retardants with different particle sizes, due to the synergistic effect between the flame retardant and alumina, this two-component epoxy adhesive has high thermal conductivity performance, high flame retardant performance, and smooth dispensing.

[0211] The above are only some embodiments of the present application, and thus do not limit the protection scope of the present application. Any equivalent device or equivalent process transformation made by using the content of the specification and drawings of the present application, or directly or indirectly applied in other related technical fields, shall similarly be included in the patent protection scope of the present application.

Claims

1. A thermally conductive composition, characterized in that: include: 800-1200 parts of thermal conductive filler, 40-60 parts of flame retardant, 1-5 parts of thixotropic agent, 1-5 parts of surface treatment agent; The thermal conductive filler is a surface-modified composite product; and the flame retardant is a surface-modified product.

2. The thermally conductive composition according to claim 1, characterized in that The thermal conductive filler is aluminum oxide; the particle size of the aluminum oxide includes at least three types of particles: large, medium and small, and the weight ratio thereof is (6-9): (0.5-3): (0.5-3).

3. The thermally conductive composition according to claim 1, characterized in that The flame retardant is selected from a combination of one or more of silicon powder, magnesium oxide, aluminum hydroxide, and magnesium hydroxide; the surface treatment agent includes a combination of one or more of γ-glycidyloxypropyltrimethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, vinyl tri-tert-butyl peroxide silane, 3-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, and γ-mercaptopropyltriethoxysilane.

4. The thermally conductive composition according to claim 1, characterized in that: The weight ratio of the thermal conductive filler to the flame retardant is (8-12): (0.4-0.6).

5. The thermally conductive composition according to claim 1, characterized in that: The step of modifying the thermally conductive filler and the flame retardant comprises: Adding the surface treatment agent to an ethanol aqueous solution with a pH value of 2 to 4 to completely hydrolyze the surface treatment agent; Adding the thermal conductive filler and the flame retardant of different particle sizes, and stirring under preset conditions; Drying the stirred reactants to obtain a surface-modified mixture of the thermally conductive filler and the flame retardant; The amount of the surface treatment agent added is 3-5% of the total amount of the thermal conductive filler and the flame retardant.

6. An epoxy adhesive thermal conductive component, characterized in that: The epoxy adhesive heat-conducting component includes: 80-100 parts of epoxy resin, 5-15 parts of active diluent, 800-1200 parts of first heat-conducting filler, 40-60 parts of first flame retardant, 1-5 parts of thixotropic agent, and 1-5 parts of first surface treatment agent; The first thermally conductive filler is a surface-modified composite product; the first flame retardant is a surface-modified product.

7. An epoxy adhesive thermal conductive component, characterized in that: The epoxy adhesive heat-conducting component includes: 80-110 parts of curing agent, 3-8 parts of accelerator, 800-1200 parts of second heat-conducting filler, 40-60 parts of second flame retardant, 1-5 parts of thixotropic agent, and 1-5 parts of second surface treatment agent; The second thermally conductive filler is a surface-modified compound product; and the second flame retardant is a surface-modified product.

8. The epoxy adhesive thermal conductive component according to claim 7, characterized in that: The second surface treatment agent includes one or more of 3-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltriethoxysilane, γ-(methacryloyloxy)propyltrimethoxysilane, and vinyltri-tert-butylperoxide silane.

9. An epoxy adhesive, characterized in that: The epoxy adhesive comprises component A and component B; The component A comprises: 80 to 100 parts of epoxy resin, 5 to 15 parts of active diluent, 800 to 1200 parts of first thermal conductive filler, 40 to 60 parts of first flame retardant, 1 to 5 parts of thixotropic agent, and 1 to 5 parts of first surface treatment agent; The B component includes: 80-110 parts of curing agent, 3-8 parts of accelerator, 800-1200 parts of second thermal conductive filler, 40-60 parts of second flame retardant, 1-5 parts of thixotropic agent, and 1-5 parts of second surface treatment agent; The first thermally conductive filler and the second thermally conductive filler are surface-modified composite products; the first flame retardant and the second flame retardant are surface-modified products, and the first surface treatment agent and the second surface treatment agent have different components.

10. The epoxy adhesive according to claim 9, characterized in that: The component A further comprises 1 to 5 parts of a defoamer and 0.5 to 2 parts of a pigment, and the component B further comprises 1 to 5 parts of a defoamer.

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