Insulating flame retardant adhesive and preparation method thereof

By using specific components and photoinitiators in the adhesive to form a multiple interpenetrating network structure, the problem that existing adhesives are difficult to meet the excellent insulation and flame retardant properties at the same time is solved, and a high-performance insulating flame retardant adhesive is achieved.

CN117089310BActive Publication Date: 2025-03-25SUZHOU MAIGE TAPE TECH CO LTD
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Patent Information

Application Number
CN202311079165.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-25
Publication Date
2025-03-25
Estimated Expiration
2043-08-25

AI Technical Summary

Technical Problem

Existing adhesives are difficult to meet the excellent insulation and flame retardancy at the same time, and their performance stability and mechanical properties are insufficient, and the flame retardant efficiency and insulation effect need to be improved.

Method used

Allylated hyperbranched polyphenylene ether, amino-modified hexaphenoxycyclotriphosphazene, 2,4,6-trivinylboroxane, benzyl-methylbenzoate, 4-acryloyl hydroxybenzoate, rosin-based acrylamide monomer and cage-type silsesquioxane containing vinyl and epoxy groups are used to induce ultraviolet curing reactions through photoinitiators, and form multiple interpenetrating network structures to enhance the insulation and flame retardancy of the adhesive.

Benefits of technology

It has achieved insulating flame retardant adhesive with good insulation and flame retardant, strong bonding performance, stable performance and environmental protection, and has a long service life and is suitable for a variety of electronic and electrical fields.

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Abstract

The invention discloses an insulating flame-retardant adhesive and a preparation method thereof, and relates to the technical field of adhesives. The adhesive comprises the following components by weight: 40 parts of allylated hyperbranched polyphenylene ether, 8-12 parts of amino-modified hexaphenoxy cyclotriphosphazene, 2-4 parts of 2,4,6-trivinyl cycloboroxine, 1-3 parts of benzoguanamine, 3-5 parts of 4-acryloylhydroxybenzoic acid benzophenone, 1-3 parts of 2,4-diphenyl-4-methyl-1-pentene, 3-5 parts of rosin-based acrylamide monomer, 3-6 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 1-3 parts of photoinitiator, 0.6-0.8 parts of defoamer, and 30-40 parts of solvent. The adhesive has good insulation and flame retardancy, strong bonding performance, good performance stability and environmental protection.
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Description

Technical Field

[0001] The invention relates to the technical field of adhesives, and in particular to an insulating flame-retardant adhesive and a preparation method thereof. Background Art

[0002] Adhesives are natural or synthetic, organic or inorganic substances that connect two or more parts or materials together through interfacial adhesion and cohesion. Due to its good bonding performance, excellent functionality, relatively low price and simple bonding process, it has been widely used in the fields of home appliances, automobiles, water conservancy and transportation, electronic appliances and aerospace industries in recent decades. And as its application scope is further broadened, its performance requirements are getting higher and higher.

[0003] Flame retardancy and insulation are two important indicators for measuring the quality of adhesives, which directly affect the application of adhesives. However, it is rare for existing adhesives to meet both insulation and flame retardancy. In order to improve the above-mentioned properties of adhesives, the conventional practice in this field is to add various functional additives to ordinary adhesives. However, the addition of a large amount of functional additives often affects the mechanical properties of the adhesive. And due to the compatibility problems between functional additives and other components, the adhesive often suffers from the defect of insufficient performance stability during long-term use. In addition, the flame retardant efficiency and insulation effect of insulating flame retardant adhesives on the market need to be further improved.

[0004] For example, the Chinese invention patent with the authorization announcement number CN102533161B discloses a flame retardant pressure-sensitive adhesive and its preparation method. The flame retardant pressure-sensitive adhesive of the invention is composed of the following components in weight percentage: 50-60% styrene-butadiene rubber, 30-40% terpene resin, 5-14% antimony trioxide flame retardant masterbatch, 3-5% antioxidant D, 1-2% rosin resin, and 2-5% glycerol. The flame retardant pressure-sensitive adhesive of the invention has the highest level of flame retardancy, good insulation performance, long service life, and low cost, and is particularly suitable for the fields of electrical engineering and packaging printed circuits. However, its performance stability and mechanical properties need to be further improved.

[0005] Therefore, the development of an insulating flame-retardant adhesive with good insulation and flame retardancy, strong bonding performance, good performance stability and environmental protection and its preparation method meets market demand, has broad market value and application prospects, and is of great significance to promoting the further development of the adhesive field. Summary of the invention

[0006] The main purpose of the present invention is to provide an insulating flame retardant adhesive having good insulation and flame retardancy, strong bonding performance, good performance stability and environmental protection, and long service life, and a preparation method thereof.

[0007] To achieve the above purpose, the present invention provides an insulating flame-retardant adhesive, which comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 8-12 parts of amino-modified hexaphenoxy cyclotriphosphazene, 2-4 parts of 2,4,6-trivinyl cycloboroxine, 1-3 parts of benzoguanamine, 3-5 parts of 4-acryloylhydroxybenzoic acid benzophenone, 1-3 parts of 2,4-diphenyl-4-methyl-1-pentene, 3-5 parts of rosin-based acrylamide monomer, 3-6 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 1-3 parts of photoinitiator, 0.6-0.8 parts of defoamer, and 30-40 parts of solvent.

[0008] Preferably, the solvent is any one of cyclohexanone, methyl ethyl ketone, propylene glycol methyl ether and xylene.

[0009] Preferably, the defoamer is at least one of defoamer AT-99 and defoamer D6800; the manufacturer of the defoamer AT-99 is Datian Chemical Technology Co., Ltd.; the manufacturer of the defoamer D6800 is Deqian Chemical Co., Ltd.

[0010] Preferably, the photoinitiator is at least one of benzoin ethyl ether, benzoin isopropyl ether, diphenyl acetone, and 2,4-dihydroxybenzophenone.

[0011] Preferably, there is no special requirement for the source of the vinyl- and epoxy-containing cage-type silsesquioxane. In one embodiment of the present invention, the vinyl- and epoxy-containing cage-type silsesquioxane is a tetraepoxy cage-type silsesquioxane in an organic system, which is prepared according to the method in Example 1 of Chinese invention patent document CN101508698B.

[0012] Preferably, there is no special requirement for the source of the rosin-based acrylamide monomer. In one embodiment of the present invention, the rosin-based acrylamide monomer is prepared according to the method in Example 1 of Chinese invention patent document CN105348422B.

[0013] Preferably, the preparation method of the amino-modified hexaphenoxy cyclotriphosphazene comprises: adding hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide and water to a high boiling point solvent, stirring and reacting in a reactor equipped with a condensation reflux device at 175-190° C. for 12-16 hours, then rotary evaporating to remove the high boiling point solvent, washing with hot water at 80° C. for 3-5 times, and finally rotary evaporating to remove residual water to obtain the amino-modified hexaphenoxy cyclotriphosphazene.

[0014] Preferably, the mass ratio of the hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, water, and high boiling point solvent is (3-5):1:(0.1-0.3):0.3:1:(10-20).

[0015] Preferably, the high boiling point solvent is one or more of dimethyl sulfoxide, N-methylpyrrolidone, and N,N-dimethylformamide.

[0016] Preferably, there is no special requirement for the source of the allylated hyperbranched polyphenylene ether. In one embodiment of the present invention, the allylated hyperbranched polyphenylene ether is prepared according to the method of Example 3 in Chinese invention patent document CN101717503B.

[0017] Another object of the present invention is to provide a method for preparing the insulating flame-retardant adhesive, comprising the following steps: uniformly mixing the components by weight to obtain a finished insulating flame-retardant adhesive.

[0018] Due to the application of the above technical solution, the present invention has the following beneficial effects:

[0019] (1) The preparation method of the insulating flame-retardant adhesive disclosed in the present invention only requires uniform mixing of the components, is easy to operate and construct, does not require special equipment and production lines, has low dependence on equipment, has high preparation efficiency and finished product qualification rate, is suitable for continuous large-scale production, and has high promotion and application value.

[0020] (2) The insulating flame-retardant adhesive disclosed in the present invention comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 8-12 parts of amino-modified hexaphenoxy cyclotriphosphazene, 2-4 parts of 2,4,6-trivinyl cycloboroxine, 1-3 parts of benzoguanamine, 3-5 parts of 4-acryloylhydroxybenzoic acid benzophenone, 1-3 parts of 2,4-diphenyl-4-methyl-1-pentene, 3-5 parts of rosin-based acrylamide monomer, 3-6 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 1-3 parts of photoinitiator, 0.6-0.8 parts of defoamer, and 30-40 parts of solvent. Through the mutual cooperation between the components, the prepared adhesive product has good insulation and flame retardancy, strong bonding performance, good performance stability and environmental protection, and long service life.

[0021] (3) The insulating flame-retardant adhesive disclosed in the present invention contains unsaturated olefinic bond components, such as allylated hyperbranched polyphenylene ether, 2,4,6-trivinyl cycloboroxane, 4-acryloylhydroxybenzoic acid benzophenone, 2,4-diphenyl-4-methyl-1-pentene, rosin-based acrylamide monomer, and cage-type silsesquioxane containing vinyl and epoxy groups, which will undergo ultraviolet light curing reaction under the initiation of a photoinitiator; at the same time, the amino groups on the amino-modified hexaphenoxy cyclotriphosphazene and benzoguanamine can react with the cage-type silsesquioxane containing vinyl and epoxy groups. The epoxy group on the alkane undergoes an epoxy ring-opening reaction to form a multiple interpenetrating network structure; at the same time, hyperbranched polyphenylene ether, hexaphenoxy cyclotriphosphazene, cycloboroxane, benzoguanamine, hydroxybenzoic acid benzophenone, phenyl-4-methyl-1-pentene, and cage-type silsesquioxane structures are introduced into the molecular structure of the adhesive. Under the multiple effects of electronic effect, steric effect, and conjugated effect, these structures make the manufactured adhesive products have better insulation and flame retardancy, better performance stability, longer service life, stronger bonding performance, and better environmental protection performance. DETAILED DESCRIPTION

[0022] The following description is used to disclose the present invention so that those skilled in the art can implement the present invention. The preferred embodiments described below are only examples, and those skilled in the art may think of other obvious variations. Example 1

[0023] An insulating flame-retardant adhesive comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 8 parts of amino-modified hexaphenoxy cyclotriphosphazene, 2 parts of 2,4,6-trivinyl cycloboroxine, 1 part of benzoguanamine, 3 parts of 4-acryloylhydroxybenzoic acid benzophenone, 1 part of 2,4-diphenyl-4-methyl-1-pentene, 3 parts of rosin-based acrylamide monomer, 3 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 1 part of photoinitiator, 0.6 parts of defoamer and 30 parts of solvent.

[0024] The solvent is cyclohexanone; the defoamer is defoamer AT-99, and the manufacturer of the defoamer AT-99 is Datian Chemical Technology Co., Ltd.; the photoinitiator is benzoin ethyl ether; the cage-type silsesquioxane containing vinyl and epoxy groups is a tetraepoxy cage-type silsesquioxane in an organic system, which is prepared according to the method in Example 1 of Chinese invention patent document CN101508698B; the rosin-based acrylamide monomer is prepared according to the method in Example 1 of Chinese invention patent document CN105348422B.

[0025] The preparation method of amino-modified hexaphenoxy cyclotriphosphazene comprises: adding hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, and water to a high boiling point solvent, stirring and reacting in a reactor with a condensation reflux device at 175°C for 12 hours, then removing the high boiling point solvent by rotary evaporation, washing with 80°C hot water for 3 times, and finally removing the residual water by rotary evaporation to obtain amino-modified hexaphenoxy cyclotriphosphazene; the mass ratio of hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, water, and high boiling point solvent is 3:1:0.1:0.3:1:10; the high boiling point solvent is dimethyl sulfoxide. By elemental analysis of the product, the product contains sulfur element, which confirms the occurrence of the above reaction.

[0026] The allylated hyperbranched polyphenylene ether is prepared according to the method of Example 3 in Chinese invention patent document CN101717503B.

[0027] A method for preparing the insulating flame-retardant adhesive comprises the following steps: uniformly mixing the components by weight to obtain a finished insulating flame-retardant adhesive. Example 2

[0028] An insulating flame-retardant adhesive comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 9 parts of amino-modified hexaphenoxy cyclotriphosphazene, 2.5 parts of 2,4,6-trivinyl cycloboroxine, 1.5 parts of benzoguanamine, 3.5 parts of 4-acryloylhydroxybenzoic acid benzophenone, 1.5 parts of 2,4-diphenyl-4-methyl-1-pentene, 3.5 parts of rosin-based acrylamide monomer, 4 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 1.5 parts of photoinitiator, 0.65 parts of defoamer and 33 parts of solvent.

[0029] The solvent is methyl ethyl ketone; the defoamer is defoamer D6800, and the manufacturer of the defoamer D6800 is Deqian Chemical Co., Ltd.; the photoinitiator is benzoin isopropyl ether; the cage-type silsesquioxane containing vinyl and epoxy groups is a tetraepoxy cage-type silsesquioxane in an organic system, which is prepared according to the method in Example 1 of Chinese invention patent document CN101508698B; the rosin-based acrylamide monomer is prepared according to the method in Example 1 of Chinese invention patent document CN105348422B.

[0030] The preparation method of amino-modified hexaphenoxy cyclotriphosphazene comprises: adding hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide and water into a high boiling point solvent, stirring and reacting in a reactor equipped with a condensation reflux device at 180°C for 13 hours, then rotary evaporating to remove the high boiling point solvent, washing with hot water at 80°C for 4 times, and finally rotary evaporating to remove residual water to obtain amino-modified hexaphenoxy cyclotriphosphazene; the mass ratio of the hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, water and high boiling point solvent is 3.5:1:0.15:0.3:1:13; and the high boiling point solvent is N-methylpyrrolidone.

[0031] The allylated hyperbranched polyphenylene ether is prepared according to the method of Example 3 in Chinese invention patent document CN101717503B.

[0032] A method for preparing the insulating flame-retardant adhesive comprises the following steps: uniformly mixing the components by weight to obtain a finished insulating flame-retardant adhesive. Example 3

[0033] An insulating flame-retardant adhesive comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 10 parts of amino-modified hexaphenoxy cyclotriphosphazene, 3 parts of 2,4,6-trivinyl cycloboroxine, 2 parts of benzoguanamine, 4 parts of 4-acryloylhydroxybenzoic acid benzophenone, 2 parts of 2,4-diphenyl-4-methyl-1-pentene, 4 parts of rosin-based acrylamide monomer, 4.5 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 2 parts of photoinitiator, 0.7 parts of defoamer and 35 parts of solvent.

[0034] The solvent is propylene glycol methyl ether; the defoamer is defoamer AT-99, and the manufacturer of the defoamer AT-99 is Datian Chemical Technology Co., Ltd.; the photoinitiator is diphenyl acetophenone; the cage-type silsesquioxane containing vinyl and epoxy groups is a tetraepoxy cage-type silsesquioxane in an organic system, which is prepared according to the method in Example 1 of Chinese invention patent document CN101508698B; the rosin-based acrylamide monomer is prepared according to the method in Example 1 of Chinese invention patent document CN105348422B.

[0035] The preparation method of amino-modified hexaphenoxy cyclotriphosphazene comprises: adding hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide and water into a high boiling point solvent, stirring and reacting in a reactor equipped with a condensation reflux device at 183°C for 14 hours, then rotary evaporating to remove the high boiling point solvent, washing with hot water at 80°C for 4 times, and finally rotary evaporating to remove residual water to obtain amino-modified hexaphenoxy cyclotriphosphazene; the mass ratio of the hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, water and high boiling point solvent is 4:1:0.2:0.3:1:15; and the high boiling point solvent is N,N-dimethylformamide.

[0036] The allylated hyperbranched polyphenylene ether is prepared according to the method of Example 3 in Chinese invention patent document CN101717503B.

[0037] A method for preparing the insulating flame-retardant adhesive comprises the following steps: uniformly mixing the components by weight to obtain a finished insulating flame-retardant adhesive. Example 4

[0038] An insulating flame-retardant adhesive comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 11 parts of amino-modified hexaphenoxy cyclotriphosphazene, 3.5 parts of 2,4,6-trivinyl cycloboroxine, 2.5 parts of benzoguanamine, 4.5 parts of 4-acryloylhydroxybenzoic acid benzophenone, 2.5 parts of 2,4-diphenyl-4-methyl-1-pentene, 4.5 parts of rosin-based acrylamide monomer, 5.5 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 2.5 parts of photoinitiator, 0.75 parts of defoamer and 38 parts of solvent.

[0039] The solvent is xylene; the defoamer is a mixture of defoamer AT-99 and defoamer D6800 in a mass ratio of 3:5; the manufacturer of the defoamer AT-99 is Datian Chemical Technology Co., Ltd.; the manufacturer of the defoamer D6800 is Deqian Chemical Co., Ltd.; the photoinitiator is a mixture of benzoin ethyl ether, benzoin isopropyl ether, diphenyl acetone, and 2,4-dihydroxybenzophenone in a mass ratio of 1:2:1:3; the vinyl- and epoxy-containing cage-type silsesquioxane is a tetraepoxy cage-type silsesquioxane in an organic system, which is prepared according to the method in Example 1 of Chinese invention patent document CN101508698B; the rosin-based acrylamide monomer is prepared according to the method in Example 1 of Chinese invention patent document CN105348422B.

[0040] The preparation method of amino-modified hexaphenoxy cyclotriphosphazene comprises: adding hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide and water into a high boiling point solvent, stirring and reacting in a reactor equipped with a condensation reflux device at 187°C for 15 hours, then removing the high boiling point solvent by rotary evaporation, washing with hot water at 80°C for 5 times, and finally removing the residual water by rotary evaporation to obtain amino-modified hexaphenoxy cyclotriphosphazene; the mass ratio of the hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, water and the high boiling point solvent is 4.5:1:0.25:0.3:1:18; and the high boiling point solvent is a mixture formed by mixing dimethyl sulfoxide, N-methylpyrrolidone and N,N-dimethylformamide in a mass ratio of 1:2:4.

[0041] The allylated hyperbranched polyphenylene ether is prepared according to the method of Example 3 in Chinese invention patent document CN101717503B.

[0042] A method for preparing the insulating flame-retardant adhesive comprises the following steps: uniformly mixing the components by weight to obtain a finished insulating flame-retardant adhesive. Example 5

[0043] An insulating flame-retardant adhesive comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 12 parts of amino-modified hexaphenoxy cyclotriphosphazene, 4 parts of 2,4,6-trivinyl cycloboroxine, 3 parts of benzoguanamine, 5 parts of 4-acryloylhydroxybenzoic acid benzophenone, 3 parts of 2,4-diphenyl-4-methyl-1-pentene, 5 parts of rosin-based acrylamide monomer, 6 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 3 parts of photoinitiator, 0.8 parts of defoamer and 40 parts of solvent.

[0044] The solvent is cyclohexanone; the defoamer is defoamer AT-99, and the manufacturer of the defoamer AT-99 is Datian Chemical Technology Co., Ltd.; the photoinitiator is benzoin ethyl ether; the cage-type silsesquioxane containing vinyl and epoxy groups is a tetraepoxy cage-type silsesquioxane in an organic system, which is prepared according to the method in Example 1 of Chinese invention patent document CN101508698B; the rosin-based acrylamide monomer is prepared according to the method in Example 1 of Chinese invention patent document CN105348422B.

[0045] The preparation method of amino-modified hexaphenoxy cyclotriphosphazene comprises: adding hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide and water into a high boiling point solvent, stirring and reacting in a reactor equipped with a condensation reflux device at 190°C for 16 hours, then removing the high boiling point solvent by rotary evaporation, washing with hot water at 80°C for 5 times, and finally removing the residual water by rotary evaporation to obtain amino-modified hexaphenoxy cyclotriphosphazene; the mass ratio of the hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, water and high boiling point solvent is 5:1:0.3:0.3:1:20; and the high boiling point solvent is N,N-dimethylformamide.

[0046] The allylated hyperbranched polyphenylene ether is prepared according to the method of Example 3 in Chinese invention patent document CN101717503B.

[0047] A method for preparing the insulating flame-retardant adhesive comprises the following steps: uniformly mixing the components by weight to obtain a finished insulating flame-retardant adhesive.

[0048] Comparative Example 1

[0049] An insulating flame-retardant adhesive is substantially the same as that of Example 1, except that hexaphenoxy cyclotriphosphazene is used instead of amino-modified hexaphenoxy cyclotriphosphazene.

[0050] Comparative Example 2

[0051] An insulating flame-retardant adhesive is substantially the same as Example 1, except that cage-type silsesquioxane containing vinyl and epoxy groups and 2,4,6-trivinyl cycloboroxine are not added.

[0052] In order to further illustrate the beneficial technical effects of the insulating flame retardant adhesives prepared in various embodiments of the present invention, relevant performance tests were conducted on the insulating flame retardant adhesives prepared in Examples 1-5 and Comparative Examples 1-2. The test results are shown in Table 1. The test method is as follows:

[0053] (1) Volume resistivity: The volume resistivity of the cured insulating flame retardant adhesive in each case was measured using the solid material volume resistivity determination method specified in GB / T1410-2006. The curing was performed using an IGE XC210 (wavelength 365nm) ultraviolet lamp with a light intensity of 1000mw / cm 2 , time is 30 seconds; then dried at 80℃ for 2h.

[0054] (2) Tensile shear strength: Each adhesive was coated on the bonded test piece to form a uniform film layer with a thickness of 0.2 mm. After curing, the tensile shear strength at room temperature of 20°C was measured using GB / T 7124-2008. The curing was performed using an IGE XC210 (wavelength 365 nm) ultraviolet lamp with a light intensity of 1000 mw / cm 2 , time is 30 seconds; then dried at 80℃ for 2h.

[0055] (3) Flame retardancy: After curing, each adhesive was tested for limiting oxygen index according to GB / T 2406.2-2009. The curing was performed using an IGE XC210 (wavelength 365nm) ultraviolet lamp with a light intensity of 1000mw / cm 2 , time is 30 seconds; then dried at 80℃ for 2h.

[0056] (4) Moisture and heat resistance: The cured adhesive samples were placed in an environment of 85°C and 95% relative humidity for 100 hours. After cooling to room temperature, the tensile shear strength was tested again according to the method in (2), and the retention rate of the tensile shear strength was calculated. The larger the value, the better the moisture and heat resistance.

[0057] Table 1

[0058]

[0059] As can be seen from Table 1, the insulating flame-retardant adhesive disclosed in the embodiment of the present invention has better bonding performance, insulating performance, flame retardant performance and moisture and heat resistance than the comparative example product. The addition of amino-modified hexaphenoxy cyclotriphosphazene, cage-type silsesquioxane containing vinyl and epoxy groups, and 2,4,6-trivinyl cycloboroxine is beneficial to improving the above-mentioned properties.

[0060] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions only describe the principles of the present invention. The present invention may be subject to various changes and improvements without departing from the spirit and scope of the present invention. These changes and improvements fall within the scope of the present invention. The scope of protection claimed by the present invention is defined by the attached claims and their equivalents.

Claims

1. An insulating flame retardant adhesive, characterized in that: The invention comprises the following components in parts by weight: 40 parts of allylated hyperbranched polyphenylene ether, 8-12 parts of amino-modified hexaphenoxy cyclotriphosphazene, 2-4 parts of 2,4,6-trivinyl cycloboroxine, 1-3 parts of benzoguanamine, 3-5 parts of 4-acryloylhydroxybenzoic acid benzophenone, 1-3 parts of 2,4-diphenyl-4-methyl-1-pentene, 3-5 parts of rosin-based acrylamide monomer, 3-6 parts of cage-type silsesquioxane containing vinyl and epoxy groups, 1-3 parts of photoinitiator, 0.6-0.8 parts of defoamer and 30-40 parts of solvent; The preparation method of amino-modified hexaphenoxy cyclotriphosphazene comprises: adding hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide and water into a high boiling point solvent, stirring and reacting in a reactor equipped with a condensation reflux device at 175-190° C. for 12-16 hours, then removing the high boiling point solvent by rotary evaporation, washing with hot water at 80° C. for 3-5 times, and finally removing the residual water by rotary evaporation to obtain amino-modified hexaphenoxy cyclotriphosphazene; the mass ratio of the hexaphenoxy cyclotriphosphazene, 2,5-diaminobenzenesulfonic acid, polyphosphoric acid, phosphorus pentoxide, water and high boiling point solvent is (3-5):1:(0.1-0.3):0.3:1:(10-20); the high boiling point solvent is one or more of dimethyl sulfoxide, N-methylpyrrolidone and N,N-dimethylformamide.

2. The insulating flame-retardant adhesive according to claim 1, characterized in that: The solvent is any one of cyclohexanone, methyl ethyl ketone, propylene glycol methyl ether and xylene.

3. The insulating flame-retardant adhesive according to claim 1, characterized in that: The defoamer is at least one of defoamer AT-99 and defoamer D6800.

4. The insulating flame-retardant adhesive according to claim 1, characterized in that: The photoinitiator is at least one of benzoin ethyl ether, benzoin isopropyl ether, diphenyl acetone, and 2,4-dihydroxybenzophenone.

5. A method for preparing the insulating flame-retardant adhesive according to any one of claims 1 to 4, characterized in that: The method comprises the following steps: uniformly mixing the components according to weight to obtain a finished insulating flame-retardant adhesive.

Citation Information

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