High-strength transparent thermosetting insulation paste
By combining EPDM rubber and photothermal dual-curing additives, and employing an ethylene gradient distribution structure and a two-stage curing process, the problems of light transmittance and tensile strength of thermosetting insulating adhesives were solved, achieving high strength and high light transmittance of transparent thermosetting insulating adhesives.
Patent Information
- Application Number
- CN202511541269.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-27
- Publication Date
- 2025-12-23
AI Technical Summary
Existing thermosetting insulating adhesives have poor light transmission, which limits their application range, and their tensile strength is low, making them prone to breakage.
By using a combination of EPDM rubber, dynamic crosslinking agent, co-crosslinking agent, transparent tackifying resin, insulating and reinforcing filler, and photothermal dual-curing additive, and through solution mixing pre-dispersion and two-stage curing process, an ethylene gradient distribution structure is formed, which improves light transmittance and tensile strength.
This has improved the light transmittance of thermosetting insulating adhesives, expanded their application range, enhanced tensile strength, and improved safety and stability in use.
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Figure CN121182384A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of thermosetting insulating adhesives, specifically a high-strength transparent thermosetting insulating adhesive. Background Technology
[0002] Transparent thermosetting insulating adhesives are a type of special adhesive based on thermosetting resins that forms an insoluble and infusible insulating layer through heating and curing. Traditional insulating materials are difficult to meet the requirements of complex electrical structures due to their large weight and poor processability. Thermosetting resins, with their ability to achieve molecular cross-linking through heating and curing, have become an important direction for insulating materials. Transparent thermosetting insulating adhesives will evolve towards higher thermal conductivity, lower curing temperature, and better environmental adaptability. However, existing thermosetting insulating adhesives have poor light transmittance, which limits their application range, and their tensile strength is low, making them prone to breakage.
[0003] The existing thermosetting insulating adhesives have the following drawbacks:
[0004] 1. Patent document CN120118647A discloses a high thermal conductivity epoxy crystal-fixing insulating adhesive and its preparation method. "This invention involves adding epoxy resin, phosphorus-containing benzimidazole, diluent, curing accelerator, curing agent, defoamer, coupling agent, and thixotropic agent to a homogenizing tank, placing it in a homogenizer at 2000 rpm for 2-3 minutes for vacuum homogenization to obtain the epoxy crystal-fixing adhesive base material; baking the epoxy crystal-fixing adhesive base material at 140℃ for 1 hour to cure; adding thermally conductive filler to the epoxy crystal-fixing adhesive base material, placing it in a homogenizer at 2000 rpm for 2-4 minutes for vacuum homogenization to obtain a semi-finished epoxy crystal-fixing adhesive; and finally, obtaining a high thermal conductivity epoxy crystal-fixing insulating adhesive through a three-roll mill. The insulating adhesive of this invention has good thermal conductivity and flame retardant effects." However, existing thermosetting insulating adhesives have poor light transmittance, limiting their application range, and their tensile strength is low, making them prone to breakage. Summary of the Invention
[0005] The purpose of this invention is to provide a high-strength transparent thermosetting insulating adhesive to solve the technical problems mentioned in the background art, such as poor light transmission affecting the scope of application, and low tensile strength making the adhesive prone to breakage.
[0006] To achieve the above objectives, the present invention provides the following technical solution: a high-strength transparent thermosetting insulating adhesive, comprising the following components by weight: 100-120 parts of matrix, the matrix being EPDM rubber or epoxy resin; 15-30 parts of dynamic crosslinking agent; 2-6 parts of co-crosslinking agent; 20-40 parts of transparent tackifying resin; 5-15 parts of insulating reinforcing filler; and 0.5-3 parts of photothermal dual-curing agent. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene; 4.5-8.0% ethylene-methylborneol (DMPO) as the third monomer; and 1.5-3.5 parts of peroxide crosslinking agent, the peroxide crosslinking agent being selected from tert-butyl. The epoxy resin is selected from one or more of isopropyl peroxide, tert-butyl peroxide, and trimethylcyclohexane; the co-crosslinking agent is selected from at least one of trimethylolpropane trimethacrylate and triallyl isocyanurate; the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer; the insulating reinforcing filler is spherical nano-alumina with a surface modified by a silane coupling agent, and the particle size of the nano-alumina is 20-50 nm; the photothermal dual-curing aid is an organosiloxane containing epoxy and acrylate groups; and the epoxy resin is a compound of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin.
[0007] Preferably, the matrix is pre-dispersed using a solution mixing method, in which high-ethylene-content EPDM rubber is compounded with low-ethylene-content EPDM rubber at a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure, wherein the high-ethylene-content ethylene content is 58-60% by mass and the low-ethylene-content ethylene content is 45-50% by mass.
[0008] Preferably, the transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer, with a mass ratio of 2:1 to 1:1, and the softening point of the composite resin is 85 to 105°C.
[0009] Preferably, the silane coupling agent of the insulating reinforcing filler is methacryloyloxypropyltrimethoxysilane, and the grafting rate on the surface of the modified filler is 1.2~2.5% by mass.
[0010] Preferably, the photothermal dual-curing agent is selected from the condensation product of propylene oxide trimethoxysilane and hydroxyethyl methacrylate, and its epoxy value is 0.25~0.45 per 100g.
[0011] Preferably, in the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5 to 1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1 to 5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation, and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 0-120 milliwatts per square centimeter, and the UV irradiation time is 30-60s to initiate acrylate crosslinking. The heat curing temperature is 150-170℃, and the heat curing time is 5-10 minutes to complete the peroxide crosslinking.
[0012] Preferably, the preparation method of the thermosetting insulating adhesive includes the following steps;
[0013] Step S1: Plasticize the matrix in an internal mixer to a temperature of 80~90℃;
[0014] Step S2: Add transparent tackifying resin and insulating reinforcing filler, and mix at 100~110℃ for 15~25 minutes to form material A;
[0015] Step S3: Cool material A to below 70°C, add dynamic crosslinking agent and photothermal dual curing agent, and mix for 10-15 minutes to form material B;
[0016] Step S4: Material B is extruded through a twin-screw extruder at an extrusion temperature of 95~105℃ to obtain transparent thermosetting insulating granules.
[0017] Preferably, in step S3, 0.1 to 0.5 parts by weight of an anti-yellowing agent is added, wherein the anti-yellowing agent is a disebacate.
[0018] Preferably, in step S2, the rotor speed of the internal mixer is 40~60 rpm, and the mixing process is divided into two stages. In the first stage, the mixture is mixed at 100~105℃ for 10 minutes with high shear force applied. In the second stage, the temperature is lowered to 95~100℃, the mixture is mixed for 5 minutes, and then the temperature is switched to low shear force.
[0019] Preferably, in step S4, the screw assembly of the twin-screw extruder includes three sets of kneading blocks with included angles of 30°, 60°, and 90°, respectively, and the 90° kneading block is located in front of the melt pump, and the screw length-to-diameter ratio is 40:1 to 44:1.
[0020] Compared with the prior art, the beneficial effects of the present invention are:
[0021] 1. This invention utilizes a ternary ethylene propylene diene monomer (EPDM) rubber comprising the following components by mass percentage: 45-60% ethylene, 4.5-8.0% ethylene-based third monomer (ethylidene norbornene), 1.5-3.5 parts of a dynamic crosslinking agent (a peroxide crosslinking agent selected from one or more of tert-butyl peroxyisopropyl, tert-butyl peroxide, and trimethylcyclohexane), at least one of a co-crosslinking agent selected from trimethylolpropane trimethacrylate and triallyl isocyanurate, at least one of a transparent tackifying resin selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer, an insulating reinforcing filler with spherical nano-alumina modified with a silane coupling agent and a nano-alumina particle size of 20-50 nm, a photothermal dual-curing agent containing an organosiloxane with epoxy and acrylate groups, and an epoxy resin composed of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin. This invention achieves the function of improving the light transmittance of thermosetting insulating adhesives and expanding their application range.
[0022] 2. This invention utilizes a solution mixing method to pre-disperse a matrix, blending high-ethylene-content EPDM rubber with low-ethylene-content EPDM rubber at a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure. The high-ethylene content ethylene accounts for 58-60% by mass, while the low-ethylene content ethylene accounts for 45-50% by mass. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer at a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85-105℃. The silane coupling agent for the insulating reinforcing filler is methacryloxypropyltrimethoxysilane. This invention achieves the functions of improving the tensile strength of thermosetting insulating adhesives and enhancing their safety in use.
[0023] 3. This invention utilizes a modified filler with a grafting rate of 1.2-2.5% by mass. The photothermal dual-curing agent is selected from the condensation of glycidoxypropyltrimethoxysilane and hydroxyethyl methacrylate, with an epoxy value of 0.25-0.45 per 100g. In the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5-1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1-5:1. The insulating adhesive is cured in two stages: a first stage of UV irradiation and a second stage of thermal curing. The UV irradiation wavelength is 365nm, the UV irradiation intensity is 0-120 mW / cm², and the UV irradiation time is 30-60s to initiate acrylate crosslinking. The thermal curing temperature is 150-170℃, and the thermal curing time is 5-10 minutes, completing the peroxide crosslinking. This achieves the function of improving the peel strength and enhancing the stability of thermosetting insulating adhesives. Attached Figure Description
[0024] Figure 1This is a schematic representation of the experimental data of the present invention. Detailed Implementation
[0025] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0026] In the description of this invention, it should be noted that the terms "upper," "lower," "inner," "outer," "front end," "rear end," "both ends," "one end," and "the other end," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.
[0027] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installed," "equipped with," "connected," etc., should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be a connection within two components. Those skilled in the art can understand this according to the specific circumstances.
[0028] Example 1: Please refer to Figure 1A high-strength transparent thermosetting insulating adhesive comprises the following components by weight: 100 parts matrix, which is EPDM rubber or epoxy resin; 15 parts dynamic crosslinking agent; 2 parts co-crosslinking agent; 20 parts transparent tackifying resin; 5 parts insulating reinforcing filler; and 0.5 parts photothermal dual-curing additive. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene; 4.5-8.0% ethylene-based third monomer; 1.5-3.5 parts dynamic crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butyl peroxide, tert-butyl peroxide, and trimethylcyclohexane); and the co-crosslinking agent selected from trimethylolpropane. The product contains at least one of propyltrimethacrylate and triallyl isocyanurate; the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer; the insulating reinforcing filler is spherical nano-alumina modified with a silane coupling agent, with a particle size of 20-50 nm; the photothermal dual-curing agent is an organosiloxane containing epoxy and acrylate groups; the epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin; the matrix is pre-dispersed using a solution mixing method; and the high-ethylene-content EPDM rubber is compared with the low-ethylene-content EPDM rubber... The rubber is compounded in a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure, with 58% ethylene by mass for high ethylene content and 45% ethylene by mass for low ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer in a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85 to 105°C. The silane coupling agent for the insulating reinforcing filler is methacryloyloxypropyltrimethoxysilane, and the grafting rate on the surface of the modified filler is 1.2 to 2.5% by mass. The photothermal dual-curing aid is selected from the condensation of epoxypropyloxypropyltrimethoxysilane and hydroxyethyl methacrylate. The value is 0.25~0.45 per 100g. In the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulation adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 20 milliwatts per square centimeter, and the UV irradiation time is 30s to initiate acrylate crosslinking. The heat curing temperature is 150℃ and the heat curing time is 5 minutes to complete the peroxide crosslinking.
[0029] The preparation method of this thermosetting insulating adhesive includes the following steps;
[0030] Step S1: Plasticize the matrix in an internal mixer to a temperature of 80~90℃;
[0031] Step S2: Add transparent tackifying resin and insulating reinforcing filler, and mix at 100~110℃ for 15~25 minutes to form material A;
[0032] Step S3: Cool material A to below 70°C, add dynamic crosslinking agent and photothermal dual curing agent, and mix for 10-15 minutes to form material B;
[0033] Step S4: Material B is extruded through a twin-screw extruder at an extrusion temperature of 95~105℃ to obtain transparent thermosetting insulating granules.
[0034] In step S3, 0.1 to 0.5 parts by weight of anti-yellowing agent is added. The yellowing agent is disebacate. In step S2, the rotor speed of the internal mixer is 40 to 60 rpm. The mixing process is divided into two stages. In the first stage, the mixture is mixed at 100 to 105°C for 10 minutes with high shear force applied. In the second stage, the temperature is lowered to 95 to 100°C and the mixture is mixed for 5 minutes. Then, the temperature is switched to low shear force. In step S4, the screw assembly of the twin-screw extruder includes three sets of kneading blocks with included angles of 30°, 60° and 90°. The 90° kneading block is located in front of the melt pump. The screw length-to-diameter ratio is 40:1 to 44:1.
[0035] Example 2: Please refer to Figure 1A high-strength transparent thermosetting insulating adhesive comprises the following components by weight: 120 parts matrix, which is EPDM rubber or epoxy resin; 30 parts dynamic crosslinking agent; 6 parts co-crosslinking agent; 40 parts transparent tackifying resin; 15 parts insulating reinforcing filler; and 3 parts photothermal dual-curing additive. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene; 4.5-8.0% ethylene-based third monomer; 1.5-3.5 parts dynamic crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butyl peroxide, tert-butyl peroxide, and trimethylcyclohexane); and the co-crosslinking agent selected from trimethylolpropane. The product contains at least one of propane trimethacrylate and triallyl isocyanurate; the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer; the insulating reinforcing filler is spherical nano-alumina modified with a silane coupling agent, with a particle size of 20-50 nm; the photothermal dual-curing agent is an organosiloxane containing epoxy and acrylate groups; the epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin; the matrix is pre-dispersed using a solution mixing method; and the high-ethylene-content EPDM rubber is compared with the low-ethylene-content EPDM rubber. The resin is compounded in a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure, with 60% ethylene by mass for high ethylene content and 50% by mass for low ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer in a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85 to 105°C. The silane coupling agent for the insulating reinforcing filler is methacryloyloxypropyltrimethoxysilane, and the grafting rate on the surface of the modified filler is 1.2 to 2.5% by mass. The photothermal dual-curing aid is selected from the condensation product of epoxypropyloxypropyltrimethoxysilane and hydroxyethyl methacrylate, and its epoxy value is... 0.25~0.45g per 100g of dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 120 milliwatts per square centimeter, and the UV irradiation time is 60s to initiate acrylate crosslinking. The heat curing temperature is 170℃ and the heat curing time is 10 minutes to complete peroxide crosslinking.
[0036] The preparation method of this thermosetting insulating adhesive includes the following steps;
[0037] Step S1: Plasticize the matrix in an internal mixer to a temperature of 80~90℃;
[0038] Step S2: Add transparent tackifying resin and insulating reinforcing filler, and mix at 100~110℃ for 15~25 minutes to form material A;
[0039] Step S3: Cool material A to below 70°C, add dynamic crosslinking agent and photothermal dual curing agent, and mix for 10-15 minutes to form material B;
[0040] Step S4: Material B is extruded through a twin-screw extruder at an extrusion temperature of 95~105℃ to obtain transparent thermosetting insulating granules.
[0041] In step S3, 0.1 to 0.5 parts by weight of anti-yellowing agent is added. The yellowing agent is disebacate. In step S2, the rotor speed of the internal mixer is 40 to 60 rpm. The mixing process is divided into two stages. In the first stage, the mixture is mixed at 100 to 105°C for 10 minutes with high shear force applied. In the second stage, the temperature is lowered to 95 to 100°C and the mixture is mixed for 5 minutes. Then, the temperature is switched to low shear force. In step S4, the screw assembly of the twin-screw extruder includes three sets of kneading blocks with included angles of 30°, 60° and 90°. The 90° kneading block is located in front of the melt pump. The screw length-to-diameter ratio is 40:1 to 44:1.
[0042] Example 3: Please refer to Figure 1A high-strength transparent thermosetting insulating adhesive comprises the following components by weight: 105 parts matrix, which is EPDM rubber or epoxy resin; 20 parts dynamic crosslinking agent; 3 parts co-crosslinking agent; 25 parts transparent tackifying resin; 8 parts insulating reinforcing filler; and 1 part photothermal dual-curing agent. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene; 4.5-8.0% ethylene-based third monomer; 1.5-3.5 parts dynamic crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butyl peroxide, tert-butyl peroxide, and trimethylcyclohexane); and the co-crosslinking agent selected from trimethylolpropane. The product contains at least one of propane trimethacrylate and triallyl isocyanurate; the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer; the insulating reinforcing filler is spherical nano-alumina modified with a silane coupling agent, with a particle size of 20-50 nm; the photothermal dual-curing agent is an organosiloxane containing epoxy and acrylate groups; the epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin; the matrix is pre-dispersed using a solution mixing method; and the high-ethylene-content EPDM rubber is compared with the low-ethylene-content EPDM rubber... The adhesive is compounded at a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure, with 59% ethylene by mass for high ethylene content and 47% ethylene by mass for low ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer at a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85 to 105°C. The silane coupling agent for the insulating reinforcing filler is methacryloyloxypropyltrimethoxysilane, and the grafting rate on the surface of the modified filler is 1.2 to 2.5% by mass. The photothermal dual-curing aid is selected from the condensation product of epoxypropyloxypropyltrimethoxysilane and hydroxyethyl methacrylate, and its epoxy value is... The concentration is 0.25~0.45 per 100g. In the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulation adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 50 milliwatts per square centimeter, and the UV irradiation time is 40s to initiate acrylate crosslinking. The heat curing temperature is 160℃ and the heat curing time is 6 minutes to complete the peroxide crosslinking.
[0043] The preparation method of this thermosetting insulating adhesive includes the following steps;
[0044] Step S1: Plasticize the matrix in an internal mixer to a temperature of 80~90℃;
[0045] Step S2: Add transparent tackifying resin and insulating reinforcing filler, and mix at 100~110℃ for 15~25 minutes to form material A;
[0046] Step S3: Cool material A to below 70°C, add dynamic crosslinking agent and photothermal dual curing agent, and mix for 10-15 minutes to form material B;
[0047] Step S4: Material B is extruded through a twin-screw extruder at an extrusion temperature of 95~105℃ to obtain transparent thermosetting insulating granules.
[0048] In step S3, 0.1 to 0.5 parts by weight of anti-yellowing agent is added. The yellowing agent is disebacate. In step S2, the rotor speed of the internal mixer is 40 to 60 rpm. The mixing process is divided into two stages. In the first stage, the mixture is mixed at 100 to 105°C for 10 minutes with high shear force applied. In the second stage, the temperature is lowered to 95 to 100°C and the mixture is mixed for 5 minutes. Then, the temperature is switched to low shear force. In step S4, the screw assembly of the twin-screw extruder includes three sets of kneading blocks with included angles of 30°, 60° and 90°. The 90° kneading block is located in front of the melt pump. The screw length-to-diameter ratio is 40:1 to 44:1.
[0049] Example 4: Please refer to Figure 1A high-strength transparent thermosetting insulating adhesive comprises the following components by weight: 110 parts matrix, which is EPDM rubber or epoxy resin; 25 parts dynamic crosslinking agent; 5 parts co-crosslinking agent; 30 parts transparent tackifying resin; 12 parts insulating reinforcing filler; and 2 parts photothermal dual-curing additive. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene; 4.5-8.0% ethylene-based third monomer; 1.5-3.5 parts dynamic crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butyl peroxide, tert-butyl peroxide, and trimethylcyclohexane); and the co-crosslinking agent selected from trimethylolpropane. The product contains at least one of propane trimethacrylate and triallyl isocyanurate; the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer; the insulating reinforcing filler is spherical nano-alumina modified with a silane coupling agent, with a particle size of 20-50 nm; the photothermal dual-curing agent is an organosiloxane containing epoxy and acrylate groups; the epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin; the matrix is pre-dispersed using a solution mixing method; and the high-ethylene-content EPDM rubber is compared with the low-ethylene-content EPDM rubber... The adhesive is compounded at a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure, with 60% ethylene by mass for high ethylene content and 48% ethylene by mass for low ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer at a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85 to 105°C. The silane coupling agent for the insulating reinforcing filler is methacryloyloxypropyltrimethoxysilane, and the grafting rate on the surface of the modified filler is 1.2 to 2.5% by mass. The photothermal dual-curing aid is selected from the condensation product of epoxypropyloxypropyltrimethoxysilane and hydroxyethyl methacrylate, and its epoxy value is... The concentration is 0.25~0.45 per 100g. In the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulation adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 80 milliwatts per square centimeter, and the UV irradiation time is 50s to initiate acrylate crosslinking. The heat curing temperature is 165℃ and the heat curing time is 8 minutes to complete the peroxide crosslinking.
[0050] The preparation method of this thermosetting insulating adhesive includes the following steps;
[0051] Step S1: Plasticize the matrix in an internal mixer to a temperature of 80~90℃;
[0052] Step S2: Add transparent tackifying resin and insulating reinforcing filler, and mix at 100~110℃ for 15~25 minutes to form material A;
[0053] Step S3: Cool material A to below 70°C, add dynamic crosslinking agent and photothermal dual curing agent, and mix for 10-15 minutes to form material B;
[0054] Step S4: Material B is extruded through a twin-screw extruder at an extrusion temperature of 95~105℃ to obtain transparent thermosetting insulating granules.
[0055] In step S3, 0.1 to 0.5 parts by weight of anti-yellowing agent is added. The yellowing agent is disebacate. In step S2, the rotor speed of the internal mixer is 40 to 60 rpm. The mixing process is divided into two stages. In the first stage, the mixture is mixed at 100 to 105°C for 10 minutes with high shear force applied. In the second stage, the temperature is lowered to 95 to 100°C and the mixture is mixed for 5 minutes. Then, the temperature is switched to low shear force. In step S4, the screw assembly of the twin-screw extruder includes three sets of kneading blocks with included angles of 30°, 60° and 90°. The 90° kneading block is located in front of the melt pump. The screw length-to-diameter ratio is 40:1 to 44:1.
[0056] Example 5: Please refer to Figure 1A high-strength transparent thermosetting insulating adhesive comprises the following components by weight: 118 parts of matrix, which is EPDM rubber or epoxy resin; 28 parts of dynamic crosslinking agent; 5 parts of co-crosslinking agent; 38 parts of transparent tackifying resin; 14 parts of insulating reinforcing filler; and 2.8 parts of photothermal dual-curing additive. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene; 4.5-8.0% ethylene-based third monomer; 1.5-3.5 parts of peroxide crosslinking agent, selected from one or more of tert-butyl peroxide, tert-butyl peroxide, and trimethylcyclohexane; and the co-crosslinking agent selected from trihydroxy... The product contains at least one of methylpropane trimethacrylate and triallyl isocyanurate; the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer; the insulating reinforcing filler is spherical nano-alumina modified with a silane coupling agent, with a particle size of 20-50 nm; the photothermal dual-curing agent is an organosiloxane containing epoxy and acrylate groups; the epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin; the matrix is pre-dispersed using a solution mixing method; and the high-ethylene-content EPDM rubber is compared with the low-ethylene-content EPDM rubber... The rubber is compounded in a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure, with 60% ethylene by mass for high ethylene content and 48% ethylene by mass for low ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer in a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85 to 105°C. The silane coupling agent for the insulating reinforcing filler is methacryloyloxypropyltrimethoxysilane, and the grafting rate on the surface of the modified filler is 1.2 to 2.5% by mass. The photothermal dual-curing aid is selected from the condensation product of epoxypropyloxypropyltrimethoxysilane and hydroxyethyl methacrylate, and its epoxy value is... The concentration is 0.25~0.45 per 100g. In the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 110 milliwatts per square centimeter, and the UV irradiation time is 55s to initiate acrylate crosslinking. The heat curing temperature is 165℃ and the heat curing time is 8 minutes to complete the peroxide crosslinking.
[0057] The preparation method of this thermosetting insulating adhesive includes the following steps;
[0058] Step S1: Plasticize the matrix in an internal mixer to a temperature of 80~90℃;
[0059] Step S2: Add transparent tackifying resin and insulating reinforcing filler, and mix at 100~110℃ for 15~25 minutes to form material A;
[0060] Step S3: Cool material A to below 70°C, add dynamic crosslinking agent and photothermal dual curing agent, and mix for 10-15 minutes to form material B;
[0061] Step S4: Material B is extruded through a twin-screw extruder at an extrusion temperature of 95~105℃ to obtain transparent thermosetting insulating granules.
[0062] In step S3, 0.1 to 0.5 parts by weight of anti-yellowing agent is added. The yellowing agent is disebacate. In step S2, the rotor speed of the internal mixer is 40 to 60 rpm. The mixing process is divided into two stages. In the first stage, the mixture is mixed at 100 to 105°C for 10 minutes with high shear force applied. In the second stage, the temperature is lowered to 95 to 100°C and the mixture is mixed for 5 minutes. Then, the temperature is switched to low shear force. In step S4, the screw assembly of the twin-screw extruder includes three sets of kneading blocks with included angles of 30°, 60° and 90°. The 90° kneading block is located in front of the melt pump. The screw length-to-diameter ratio is 40:1 to 44:1.
[0063] Comparative experiment:
[0064] The difference between Comparative Example 1 and Example 1 is that;
[0065] The EPDM rubber comprises the following components by mass percentage: 100 parts matrix, 15 parts dynamic crosslinking agent, 2 parts co-crosslinking agent, 20 parts transparent tackifying resin, 5 parts insulating reinforcing filler, and 0.5 parts photothermal dual-curing agent. The EPDM rubber includes: 45-60% ethylene, 4.5-8.0% ethylene-methylborneol (DMPO), 1.5-3.5 parts dynamic crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butylperoxyisopropyl, tert-butylperoxy, and trimethylcyclohexane), and at least one co-crosslinking agent selected from at least one of trimethylolpropane trimethacrylate and triallyl isocyanurate. The transparent tackifying resin... The resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer. The insulating reinforcing filler is spherical nano-alumina with a surface modified by a silane coupling agent, and the particle size of the nano-alumina is 20-50 nm. The photothermal dual-curing aid is an organosiloxane containing epoxy and acrylate groups. The epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin. The matrix is pre-dispersed using a solution mixing method. High-ethylene-content EPDM rubber is blended with low-ethylene-content EPDM rubber at a mass ratio of 3:1 to 1:1 to form an ethylene ladder. The epoxy distribution structure shows that ethylene content is 58% by mass for high-ethylene content and 45% by mass for low-ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer, with a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85-105℃. The silane coupling agent for the insulating reinforcing filler is methacryloxypropyltrimethoxysilane, and the grafting rate on the modified filler surface is 1.2-2.5% by mass. The photothermal dual-curing aid is selected from the condensation of propylene oxide propyltrimethoxysilane and hydroxyethyl methacrylate, with an epoxy value of 0.25-0.45. In every 100g of dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 20 milliwatts per square centimeter, and the UV irradiation time is 30s to initiate acrylate crosslinking. The heat curing temperature is 150℃ and the heat curing time is 5 minutes to complete the peroxide crosslinking.
[0066] Comparative experiment:
[0067] The difference between Comparative Example 1 and Example 2 is that;
[0068] The EPDM rubber comprises the following components by mass percentage: 120 parts matrix, 30 parts dynamic crosslinking agent, 6 parts co-crosslinking agent, 40 parts transparent tackifying resin, 15 parts insulating reinforcing filler, and 3 parts photothermal dual-curing additive. The EPDM rubber includes: 45-60 parts ethylene, 4.5-8.0 parts ethylene-methylnorbornene (third monomer), 1.5-3.5 parts peroxide crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butylperoxyisopropyl, tert-butylperoxy, and trimethylcyclohexane), and at least one of trimethylolpropane trimethacrylate and triallyl isocyanurate. The transparent tackifying resin... The resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer. The insulating and reinforcing filler is spherical nano-alumina with a surface modified by a silane coupling agent, and the particle size of the nano-alumina is 20-50 nm. The photothermal dual-curing agent is an organosiloxane containing epoxy and acrylate groups. The epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin. The matrix is pre-dispersed using a solution mixing method. High-ethylene-content EPDM rubber is blended with low-ethylene-content EPDM rubber at a mass ratio of 3:1 to 1:1 to form an ethylene gradient. The composition is as follows: 60% ethylene by mass for high ethylene content and 50% ethylene by mass for low ethylene content; the transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer in a mass ratio of 2:1 to 1:1; the softening point of the composite resin is 85-105℃; the silane coupling agent for the insulating reinforcing filler is methacryloxypropyltrimethoxysilane, and the grafting rate on the modified filler surface is 1.2-2.5% by mass; the photothermal dual-curing aid is selected from the condensation of propylene oxide propyltrimethoxysilane and hydroxyethyl methacrylate, with an epoxy value of 0.25-0.45 per... In 100g of dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 120 milliwatts per square centimeter, and the UV irradiation time is 60s to initiate acrylate crosslinking. The heat curing temperature is 170℃ and the heat curing time is 10 minutes to complete peroxide crosslinking.
[0069] Comparative experiment:
[0070] The difference between Comparative Example 1 and Example 3 is that;
[0071] The EPDM rubber comprises the following components by mass percentage: 105 parts matrix, 20 parts dynamic crosslinking agent, 3 parts co-crosslinking agent, 25 parts transparent tackifying resin, 8 parts insulating reinforcing filler, and 1 part photothermal dual-curing agent. The EPDM rubber includes: 45-60 parts ethylene, 4.5-8.0 parts ethylene-idene norbornene (third monomer), 1.5-3.5 parts peroxide crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butylperoxyisopropyl, tert-butylperoxy, and trimethylcyclohexane), and at least one of trimethylolpropane trimethacrylate and triallyl isocyanurate. The transparent tackifying resin... The resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer. The insulating and reinforcing filler is spherical nano-alumina with a surface modified by a silane coupling agent, and the particle size of the nano-alumina is 20-50 nm. The photothermal dual-curing agent is an organosiloxane containing epoxy and acrylate groups. The epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin. The matrix is pre-dispersed using a solution mixing method. High-ethylene-content EPDM rubber is blended with low-ethylene-content EPDM rubber at a mass ratio of 3:1 to 1:1 to form an ethylene gradient. The composition is as follows: ethylene content is 59% by mass for high-ethylene content and 47% by mass for low-ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer, with a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85-105℃. The silane coupling agent for the insulating reinforcing filler is methacryloxypropyltrimethoxysilane, and the grafting rate on the modified filler surface is 1.2-2.5% by mass. The photothermal dual-curing aid is selected from the condensation of propylene oxide propyltrimethoxysilane and hydroxyethyl methacrylate, with an epoxy value of 0.25-0.45. In every 100g of dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 50 milliwatts per square centimeter, and the UV irradiation time is 40s to initiate acrylate crosslinking. The heat curing temperature is 160℃ and the heat curing time is 6 minutes to complete peroxide crosslinking.
[0072] Comparative experiment:
[0073] The difference between Comparative Example 1 and Example 4 is that;
[0074] The EPDM rubber comprises the following components by mass percentage: 110 parts matrix, 25 parts dynamic crosslinking agent, 5 parts co-crosslinking agent, 30 parts transparent tackifying resin, 12 parts insulating reinforcing filler, and 2 parts photothermal dual-curing additive. The EPDM rubber includes: 45-60 parts ethylene, 4.5-8.0 parts ethylene-methylnorbornene (third monomer), 1.5-3.5 parts peroxide crosslinking agent (peroxide crosslinking agent selected from one or more of tert-butylperoxyisopropyl, tert-butylperoxy, and trimethylcyclohexane), and at least one of trimethylolpropane trimethacrylate and triallyl isocyanurate. The transparent tackifying resin... The resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer. The insulating reinforcing filler is spherical nano-alumina with a surface modified by a silane coupling agent, and the particle size of the nano-alumina is 20-50 nm. The photothermal dual-curing aid is an organosiloxane containing epoxy and acrylate groups. The epoxy resin is a blend of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin. The matrix is pre-dispersed using a solution mixing method. High-ethylene-content EPDM rubber is blended with low-ethylene-content EPDM rubber at a mass ratio of 3:1 to 1:1 to form an ethylene ladder. The resin exhibits a high ethylene content (60% by mass) and a low ethylene content (48% by mass). The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer in a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85–105°C. The silane coupling agent for the insulating reinforcing filler is methacryloxypropyltrimethoxysilane, with a modified filler surface grafting rate of 1.2–2.5% by mass. The photothermal dual-curing aid is selected from the condensation of propylene oxide propyltrimethoxysilane and hydroxyethyl methacrylate, with an epoxy value of 0.25–0.45. In every 100g of dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 80 milliwatts per square centimeter, and the UV irradiation time is 50s to initiate acrylate crosslinking. The heat curing temperature is 165℃ and the heat curing time is 8 minutes to complete the peroxide crosslinking.
[0075] Comparative experiment:
[0076] The difference between Comparative Example 1 and Example 5 is that;
[0077] A high-strength transparent thermosetting insulating adhesive comprises the following components by weight: 118 parts matrix, 28 parts dynamic crosslinking agent, 5 parts co-crosslinking agent, 38 parts transparent tackifying resin, 14 parts insulating reinforcing filler, and 2.8 parts photothermal dual-curing additive. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene, 4.5-8.0% ethylene-based third monomer, 1.5-3.5 parts peroxide crosslinking agent, selected from one or more of tert-butyl peroxide, tert-butyl peroxide, and trimethylcyclohexane; and the co-crosslinking agent is selected from trimethylolpropane trimethacrylate. At least one of triallyl isocyanurate, the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer, the insulating reinforcing filler is spherical nano-alumina with a surface modified by a silane coupling agent, the nano-alumina particle size is 20-50 nm, the photothermal dual-curing aid is an organosiloxane containing epoxy and acrylate groups, the epoxy resin is a compound of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin, the matrix is pre-dispersed by solution mixing, and high-ethylene content EPDM rubber is mixed with low-ethylene content EPDM rubber at a mass ratio of 3: A 1:1 to 1:1 compound is used to form an ethylene gradient distribution structure, with 60% ethylene by mass for high ethylene content and 48% by mass for low ethylene content. The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer, with a mass ratio of 2:1 to 1:1. The softening point of the composite resin is 85 to 105℃. The silane coupling agent for the insulating reinforcing filler is methacryloxypropyltrimethoxysilane, and the grafting rate on the modified filler surface is 1.2 to 2.5% by mass. The photothermal dual-curing aid is selected from the condensation product of propylene oxide propyltrimethoxysilane and hydroxyethyl methacrylate, with an epoxy value of 0.2. 5~0.45 per 100g, in the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5~1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1~5:1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 110 milliwatts per square centimeter, and the UV irradiation time is 55s to initiate acrylate crosslinking. The heat curing temperature is 165℃ and the heat curing time is 8 minutes to complete the peroxide crosslinking.
[0078] The thermosetting insulating adhesives of Examples 1, 2, 3, 4, and 5 of the present invention were compared with a conventional thermosetting insulating adhesive (Comparative Example 1) in light transmittance, tensile strength, and peel strength tests, and their values were calculated and statistically analyzed. The results are shown in the experimental data table.
[0079]
[0080] The data from the experimental data table show that the light transmittance of the thermosetting insulating adhesives used in Examples 1, 2, 3, 4, and 5 of this invention is 91%, 92%, 90%, 90%, and 92%, respectively, which is significantly higher than that of the thermosetting insulating adhesive in Comparative Example 1. Therefore, this indicates that the light transmittance of the thermosetting insulating adhesive of this invention is significantly improved, thus achieving the function of improving the light transmittance of the thermosetting insulating adhesive and expanding its application range.
[0081] The data from the experimental data table show that the tensile strengths of the thermosetting insulating adhesives used in Examples 1, 2, 3, 4, and 5 of this invention are 14, 13, 12, 13, and 13, respectively, which are significantly higher than the tensile strength of the thermosetting insulating adhesive in Comparative Example 1. This indicates that the tensile strength of the thermosetting insulating adhesive of this invention is significantly improved, thus achieving the function of enhancing the tensile strength of the thermosetting insulating adhesive and strengthening its safety in use.
[0082] The data from the experimental data table show that the peel strength of the thermosetting insulating adhesives used in Examples 1, 2, 3, 4, and 5 of this invention is 8, 7, 9, 8, and 9, respectively, which is significantly higher than that of the thermosetting insulating adhesive in Comparative Example 1. Therefore, this indicates that the peel strength of the thermosetting insulating adhesive of this invention is significantly improved, and the function of improving the peel strength of thermosetting insulating adhesive and enhancing the stability of thermosetting insulating adhesive in use is achieved.
[0083] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.
Claims
1. A high-strength transparent thermosetting insulating adhesive, characterized in that, The composition by weight is as follows: 100-120 parts matrix, which is EPDM rubber or epoxy resin; 15-30 parts dynamic crosslinking agent; 2-6 parts co-crosslinking agent; 20-40 parts transparent tackifying resin; 5-15 parts insulating and reinforcing filler; and 0.5-3 parts photothermal dual-curing agent. The EPDM rubber comprises the following components by weight percentage: 45-60% ethylene; 4.5-8.0% ethylene-methylnorbornene (third monomer); and 1.5-3.5 parts peroxide crosslinking agent, selected from tert-butyl peroxide isopropyl, tert-butyl peroxide, and trimethylolpropionate. The resin is selected from one or more of cyclohexane, the co-crosslinking agent is selected from at least one of trimethylolpropane trimethacrylate and triallyl isocyanurate, the transparent tackifying resin is selected from at least one of hydrogenated C9 petroleum resin, hydrogenated rosin glycerol ester, and styrene-indene copolymer, the insulating reinforcing filler is spherical nano-alumina with a surface modified by a silane coupling agent, the nano-alumina has a particle size of 20-50 nm, the photothermal dual-curing aid is an organosiloxane containing epoxy and acrylate groups, and the epoxy resin is a compound of 60-80 parts of bisphenol A type epoxy resin and 10-20 parts of hydrogenated bisphenol A epoxy resin.
2. The high-strength transparent thermosetting insulating adhesive according to claim 1, characterized in that: The matrix is pre-dispersed using a solution mixing method, in which high-ethylene-content EPDM rubber is compounded with low-ethylene-content EPDM rubber at a mass ratio of 3:1 to 1:1 to form an ethylene gradient distribution structure, with the high-ethylene-content ethylene accounting for 58 to 60% by mass and the low-ethylene-content ethylene accounting for 45 to 50% by mass.
3. The high-strength transparent thermosetting insulating adhesive according to claim 1, characterized in that: The transparent tackifying resin is a composite of hydrogenated C9 petroleum resin and styrene-indene copolymer, with a mass ratio of 2:1 to 1:1, and the softening point of the composite resin is 85 to 105°C.
4. The high-strength transparent thermosetting insulating adhesive according to claim 1, characterized in that: The silane coupling agent of the insulating reinforcing filler is methacryloyloxypropyltrimethoxysilane, and the grafting rate on the surface of the modified filler is 1.2~2.5% by mass.
5. The high-strength transparent thermosetting insulating adhesive according to claim 1, characterized in that: The photothermal dual-curing additive is selected from the condensation product of propylene oxide trimethoxysilane and hydroxyethyl methacrylate, and its epoxy value is 0.25~0.45 per 100g.
6. The high-strength transparent thermosetting insulating adhesive according to claim 1, characterized in that: In the dynamic crosslinking agent, the mass ratio of peroxide crosslinking agent to co-crosslinking agent is 1:1.5 to 1:2.5, and the co-crosslinking agent is composed of trimethylolpropane trimethacrylate and triallyl isocyanurate in a mass ratio of 3:1 to 5:
1. The insulating adhesive is cured in two stages: the first stage is UV irradiation and the second stage is heat curing. The wavelength of UV irradiation is 365nm, the intensity of UV irradiation is 0-120 milliwatts per square centimeter, and the UV irradiation time is 30-60s to initiate acrylate crosslinking. The heat curing temperature is 150-170℃, and the heat curing time is 5-10 minutes to complete the peroxide crosslinking.
7. A method for using a high-strength transparent thermosetting insulating adhesive, applicable to the high-strength transparent thermosetting insulating adhesive described in any one of claims 1 to 6, characterized in that, The preparation method of this thermosetting insulating adhesive includes the following steps; Step S1: Plasticize the matrix in an internal mixer to a temperature of 80~90℃; Step S2: Add transparent tackifying resin and insulating reinforcing filler, and mix at 100~110℃ for 15~25 minutes to form material A; Step S3: Cool material A to below 70°C, add dynamic crosslinking agent and photothermal dual curing agent, and mix for 10-15 minutes to form material B; Step S4: Material B is extruded through a twin-screw extruder at an extrusion temperature of 95~105℃ to obtain transparent thermosetting insulating granules.
8. The high-strength transparent thermosetting insulating adhesive according to claim 7, characterized in that: In step S3, 0.1 to 0.5 parts by weight of an anti-yellowing agent is added, wherein the anti-yellowing agent is a bis(decanedioate) ester.
9. The high-strength transparent thermosetting insulating adhesive according to claim 7, characterized in that: In step S2, the internal mixer rotor speed is 40~60 rpm. The mixing process is divided into two stages. In the first stage, the mixture is mixed at 100~105℃ for 10 minutes with high shear force applied. In the second stage, the temperature is lowered to 95~100℃, the mixture is mixed for 5 minutes, and then the temperature is switched to low shear force.
10. A high-strength transparent thermosetting insulating adhesive according to claim 7, characterized in that: In step S4, the screw assembly of the twin-screw extruder includes three sets of kneading blocks with included angles of 30°, 60°, and 90°, respectively. The 90° kneading block is located in front of the melt pump, and the screw length-to-diameter ratio is 40:1 to 44:1.
Citation Information
Patent Citations
High-thermal-conductivity epoxy die-bonding insulation paste and preparation method thereof
CN120118647A