CN116039189A - High-temperature-resistant halogen-free flame-retardant insulating multilayer composite material - Google Patents

High-temperature-resistant halogen-free flame-retardant insulating multilayer composite material Download PDF

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CN116039189A
CN116039189A CN202310052735.8A CN202310052735A CN116039189A CN 116039189 A CN116039189 A CN 116039189A CN 202310052735 A CN202310052735 A CN 202310052735A CN 116039189 A CN116039189 A CN 116039189A
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free flame
flame retardant
halogen
composite material
multilayer composite
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刘自清
梁利
江玉才
姚桂颖
才庆龙
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Liu'an Jianghuai Motor Co ltd
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Liu'an Jianghuai Motor Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B19/00—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica
    • B32B19/04—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica next to another layer of the same or of a different material
    • B32B19/045—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
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    • B32B19/00—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica
    • B32B19/06—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B17/00—Insulators or insulating bodies characterised by their form
    • H01B17/56—Insulating bodies
    • H01B17/60—Composite insulating bodies
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/04—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances mica
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/08—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances quartz; glass; glass wool; slag wool; vitreous enamels
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H—ELECTRICITY
    • H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
    • H02K—DYNAMO-ELECTRIC MACHINES
    • H02K3/00—Details of windings
    • H02K3/30—Windings characterised by the insulating material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
    • B32B2037/243—Coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/206—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
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    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

The invention discloses a high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material, which belongs to the technical field of composite materials, and is prepared by taking a mica tape as a dielectric material, taking a polyimide film and glass cloth as reinforcing materials, taking a modified organosilicon pressure-sensitive adhesive as an adhesive and matching with a halogen-free flame retardant; the high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material prepared by using 3 kinds of base materials has good comprehensive performance and can be widely applied to wrapping insulation, liner insulation and filling insulation of motor equipment. The flame-retardant system has small smoke amount during combustion, and does not generate corrosive and toxic gases. According to the test results, the multi-layer composite material has good insulating property, flame retardance, tensile strength and flexibility, and the temperature has less influence on the insulating property, and has higher insulating property at 200 ℃.

Description

High-temperature-resistant halogen-free flame-retardant insulating multilayer composite material
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material.
Background
The insulating structure is formed by combining one or more insulating materials through a specific process, and is mainly related to turn-to-turn insulation, ground insulation, outer-wrapping insulation and interphase insulation. Most of the prior large and medium-sized high-voltage motor insulation systems adopt an organosilicon glass cloth reinforced mica tape or an epoxy diphenyl ether glass cloth reinforced mica tape, so that the normal state and thermal state dielectric loss of a stator coil are seriously influenced, the electric heating aging life of coil insulation can be shortened, harmful and toxic gases are generated in the processes of stator insulation treatment and insulation curing (high-temperature drying), the harmful gases are harmful to operators and the environment, and the safety is poor in the fields of insulation products such as wrapping insulation, liner insulation and filling insulation.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material, which aims to solve the problems that the high-temperature resistance of the composite material in the processing or application process is poor and the safety is influenced in the field of insulating products such as wrapping insulation, liner insulation and filling insulation in the background technology.
The aim of the invention can be achieved by the following technical scheme:
the high temperature resistant halogen-free flame retardant insulating multilayer composite material comprises a polyimide film, a mica tape and glass cloth from top to bottom in sequence; the multilayer composite material is prepared by taking a mica tape as a dielectric material, taking a polyimide film and glass cloth as reinforcing materials, taking a modified organic silicon pressure-sensitive adhesive as an adhesive and matching with a halogen-free flame retardant; the polyimide film, the mica tape and the glass cloth are coated with halogen-free flame retardant on both sides, and the polyimide film, the mica tape and the glass cloth coated with the halogen-free flame retardant are bonded through modified organic silicon pressure sensitive adhesive; the halogen-free flame retardant comprises the following raw materials in percentage by weight: 55-65% of triazine compounds, 25-35% of epoxy anhydride resin, 0.8-1.5% of flatting agents, 0.8-1.5% of antioxidants and 8-20% of flame retardant auxiliary agents; compared with inorganic flame-retardant powder coating, the flame-retardant auxiliary agent used in the invention has less dosage, is an organic flame retardant, does not affect the mechanical property of the powder coating, is subjected to special surface treatment, and is added with 15-30% of halogen-free flame retardant, so that the flame-retardant auxiliary agent is easy to disperse in an insulating material, does not precipitate, and has good flame-retardant effect. The triazine compound is a triazinetrione compound and a triazinetriamine compound, and the mass ratio of the triazinetrione compound to the triazinetriamine compound is 3:7, mixing.
The halogen-free flame retardant is prepared by the following steps:
putting the raw materials with the component amounts into a mixing cylinder together, premixing for 15min, extruding and tabletting on an extruder, wherein the extruding temperature is 110 ℃ in a first area and 130 ℃ in a second area, crushing the tablets, and sieving coarse powder with a 300-mesh sieve to obtain fine powder which is the final powder coating, namely the halogen-free flame retardant.
The structural formula of the triazinetrione compound is shown as follows:
Figure BDA0004058986360000021
the structural formula of the triazine triamine compound is shown as follows:
Figure BDA0004058986360000022
further, the flame retardant auxiliary comprises the following components in percentage by weight: 50wt% of polyphenylene sulfide resin GF00, 25wt% of plasticizer and 25wt% of coupling agent SG-Si171;
dissolving a coupling agent in water to prepare a 10-30% solution, adding other components, stirring for 3-5h in a homogenizer, uniformly mixing, drying for 4-6h at 105 ℃ and minus 0.09MPa in a vacuum drying oven, and crushing to obtain the flame retardant auxiliary agent.
Further, the plasticizer is one of glyceryl triacetate, tri-n-butyl citrate and acetyl tri-n-butyl citrate.
Further, the modified organosilicon pressure-sensitive adhesive is prepared by the following steps:
step one, adding nano powder and a silane coupling agent A151 into a mixed solution of absolute ethyl alcohol and toluene, performing ultrasonic treatment for 30-40min at the temperature of 45 ℃, and filtering and drying to obtain pretreated nano powder;
and step two, stirring and mixing the pretreated nano powder and the organic silicon pressure-sensitive adhesive, and adding dibenzoyl peroxide to obtain the modified organic silicon pressure-sensitive adhesive. The dosage ratio of the mixed solution of the nano powder, the silane coupling agent A151, the absolute ethyl alcohol and the toluene is 1g:1g:20mL; the volume ratio of the absolute ethyl alcohol to the toluene in the mixed solution of the absolute ethyl alcohol and the toluene is 6.5:3.5; the mass ratio of the pretreated nano powder to the organosilicon pressure-sensitive adhesive is 3:5, a step of; the addition amount of dibenzoyl peroxide is 8% of the mass sum of the pretreated nano powder and the organosilicon pressure-sensitive adhesive, and the organosilicon pressure-sensitive adhesive is polydimethylsiloxane; the addition of the nano powder can better maintain stronger electrical strength.
Further, the nano powder is nano S iC and nano Al 2 O 3 According to the mass ratio of 1.5:1, mixing; the average grain diameter of the nano SiC is 30nm; nano Al 2 O 3 The average particle diameter of (2) is 30nm.
Further, the multilayer composite is prepared by the steps of:
the preparation method comprises the steps of respectively coating the two sides of a polyimide film, a mica tape and glass cloth with halogen-free flame retardant, coating the two sides of the mica tape coated with the halogen-free flame retardant with modified organosilicon pressure-sensitive adhesive, coating the one sides of the glass cloth coated with the halogen-free flame retardant with modified organosilicon pressure-sensitive adhesive, then placing the polyimide film, the mica tape and the glass cloth in sequence from top to bottom for mechanical compounding, and after compounding, obtaining the high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material after heat treatment.
Further, the thickness of the polyimide film is 0.025mm, the thickness of the mica tape is 0.060mm, and the thickness of the glass cloth is 0.030mm; coating weight of halogen-free flame retardant: 60-100mg/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Coating weight of modified silicone pressure sensitive adhesive: 20-35mg/m 2 。
Further, the pressure of mechanical compounding was 10kN, and the work cycle was 12 times/min.
Further, the temperature of the heat treatment was 80.+ -. 5 ℃.
The invention has the beneficial effects that:
the invention provides a high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material, which is formed by compounding a polyimide film, glass cloth and a mica tape through a modified organic pressure-sensitive adhesive and a halogen-free flame retardant. In the application of wrapping insulation, liner insulation and filling insulation of motor equipment, the polyimide film, glass cloth and mica tape in the composite material have better heat conductivity compared with the prior art after being compounded; compared with the prior art, the organosilicon glass cloth reinforced mica tape has excellent insulating property, and the organosilicon glass cloth in the prior art is reinforcedThe glass cloth in the mica tape belongs to inorganic materials, has lower electrical performance, and the polyimide film is added into the composite material prepared by the method as one of the reinforcing materials, and the volume resistivity of the prepared composite material at 200 ℃ is more than 1.2 multiplied by 10 12 Omega.m, and the resistivity at 200 ℃ is reduced by only one order of magnitude while maintaining a strong electrical strength; the high temperature resistance of the composite material is not affected.
According to the invention, the polyimide film, the glass cloth and the mica tape are compounded through the modified organic pressure-sensitive adhesive and the halogen-free flame retardant, so that the high temperature resistance is better, and the winding temperature rise can be reduced when the insulation thickness is the same; the motor size is reduced under the same temperature rising condition, and the motor weight is reduced; loss is reduced, and motor efficiency is improved. More prominently, from the test result, the tensile strength of the composite material can be better maintained by using three base materials, which means that the damage probability is greatly reduced under the same wrapping condition, the product quality is improved, the wrapping speed can be improved under the condition of equipment permission, the production efficiency is further improved, and the use requirements of insulated products such as wrapping insulation, liner insulation, filling insulation and the like are met.
The flame-retardant system has small smoke amount during combustion, and does not generate corrosive and toxic gases. According to test results, the multi-layer composite material has good insulating property, flame retardance, tensile strength and flexibility, has small influence on the insulating property by temperature, has higher insulating property at 200 ℃, is applied to the fields of insulating products such as wrapping insulation, liner insulation and filling insulation, and can better endow electrical equipment with good reliability and safety.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a halogen-free flame retardant, which is prepared through the following steps:
weighing the following raw materials in percentage by weight: 50wt% of polyphenylene sulfide resin GF00, 25wt% of plasticizer and 25wt% of coupling agent SG-Si171; dissolving a coupling agent in water to prepare a 10% solution, adding other components, stirring in a homogenizer for 3 hours, uniformly mixing, drying in a vacuum drying oven at 105 ℃ and minus 0.09MPa for 4 hours, and crushing to obtain the flame retardant auxiliary; the plasticizer is glyceryl triacetate.
Putting the raw materials in a mixing cylinder according to the weight percentage, wherein the raw materials comprise 65% of triazine compounds, 25% of epoxy anhydride resin (model: JF-9955 Kyoho material), 1% of flatting agents (PV 88 of Germany De Xinli chemistry), 1% of antioxidants (Basff antioxidants 1010 of Germany) and 8% of flame retardant additives; premixing for 15min, extruding on an extruder, tabletting at 110 ℃ in the first area and 130 ℃ in the second area, crushing the tablets, and crushing, wherein the fine powder obtained by sieving coarse powder with a 300-mesh sieve through a rotary sieve is the final powder coating, namely the halogen-free flame retardant. Wherein the particle size of the epoxy anhydride resin is less than or equal to 30 mu m.
Example 2
The embodiment provides a halogen-free flame retardant, which is prepared through the following steps:
weighing the following raw materials in percentage by weight: 50wt% of polyphenylene sulfide resin GF00, 25wt% of plasticizer and 25wt% of coupling agent SG-Si171; dissolving a coupling agent in water to prepare a 20% solution, adding other components, stirring in a homogenizer for 4 hours, uniformly mixing, drying in a vacuum drying oven at 105 ℃ and minus 0.09MPa for 5 hours, and crushing to obtain the flame retardant auxiliary; the plasticizer is tri-n-butyl citrate.
Adding the raw materials in weight percentage into a mixing cylinder, wherein the raw materials comprise 55% of triazine compounds, 35% of epoxy anhydride resin (model: JF-9955 Kyoho material), 1% of flatting agents (PV 88 of Germany De Xinli chemistry), 1% of antioxidants (Basff antioxidants 1010 of Germany) and 8% of flame retardant additives; premixing for 15min, extruding on an extruder, tabletting at 110 ℃ in the first area and 130 ℃ in the second area, crushing the tablets, and crushing, wherein the fine powder obtained by sieving coarse powder with a 300-mesh sieve through a rotary sieve is the final powder coating, namely the halogen-free flame retardant. Wherein the particle size of the epoxy anhydride resin is less than or equal to 30 mu m.
Example 3
The embodiment provides a halogen-free flame retardant, which is prepared through the following steps:
weighing the following raw materials in percentage by weight: 50wt% of polyphenylene sulfide resin GF00, 25wt% of plasticizer and 25wt% of coupling agent SG-Si171; dissolving a coupling agent in water to prepare a 30% solution, adding other components, stirring for 5 hours in a homogenizer, uniformly mixing, drying for 6 hours in a vacuum drying oven at 105 ℃ and minus 0.09MPa, and crushing to obtain the flame retardant auxiliary; the plasticizer is acetyl tributyl citrate.
Adding the raw materials in weight percentage into a mixing cylinder, wherein the raw materials comprise 55% of triazine compounds, 25% of epoxy anhydride resin (model: JF-9955 Kyoho material), 1.5% of flatting agents (PV 88 of Desony chemical Germany), 1.5% of antioxidants (Basoff antioxidant 1010 of Germany) and 17% of flame retardant additives; premixing for 15min, extruding on an extruder, tabletting at 110 ℃ in the first area and 130 ℃ in the second area, crushing the tablets, and crushing, wherein the fine powder obtained by sieving coarse powder with a 300-mesh sieve through a rotary sieve is the final powder coating, namely the halogen-free flame retardant. Wherein the particle size of the epoxy anhydride resin is less than or equal to 30 mu m.
Example 4
The embodiment provides a modified organic silicon pressure-sensitive adhesive, which is prepared through the following steps:
step one, adding nano powder and a silane coupling agent A151 into a mixed solution of absolute ethyl alcohol and toluene, and performing ultrasonic treatment at 45 ℃ for 40min to obtain pretreated nano powder; the nanometer powder is nanometer SiC and nanometer Al 2 O 3 According to the mass ratio of 1.5:1, mixing; the average grain diameter of the nano SiC is 30nm; nano Al 2 O 3 The average particle diameter of (2) is 30nm; the dosage ratio of the mixed solution of the nano powder, the silane coupling agent A151, the absolute ethyl alcohol and the toluene is 1g:1g:20mL; the volume ratio of the absolute ethyl alcohol to the toluene in the mixed solution of the absolute ethyl alcohol and the toluene is 6.5:3.5;
secondly, stirring and mixing the pretreated nano powder and the organic silicon pressure-sensitive adhesive, and adding dibenzoyl peroxide to obtain a modified organic silicon pressure-sensitive adhesive; the mass ratio of the rice powder to the organic silicon pressure-sensitive adhesive is 3:5, a step of; the addition amount of dibenzoyl peroxide is 8% of the sum of the mass of the pretreated nano powder and the mass of the organosilicon pressure-sensitive adhesive. The organosilicon pressure sensitive adhesive is polydimethylsiloxane.
Comparative example 1
This example provides an organosilicon pressure sensitive adhesive, and compared with example 4, the comparative example does not add pretreated nano powder, and the rest raw materials and the preparation process remain the same as in example 4.
Example 5
The present example provides a multilayer composite material prepared by the steps of:
coating the halogen-free flame retardant prepared in the example 3 on the two sides of a polyimide film, a mica tape (model: 501) and glass cloth respectively, coating the modified organic silicon pressure-sensitive adhesive prepared in the example 4 on the two sides of the mica tape coated with the halogen-free flame retardant, coating the modified organic silicon pressure-sensitive adhesive on one side of the glass cloth coated with the halogen-free flame retardant, then placing the polyimide film, the mica tape and the glass cloth in sequence from top to bottom for mechanical compounding, wherein the mechanical compounding pressure is 10kN, the working beat is 12 times/min, and after compounding, the heat treatment temperature is 80+/-5 ℃, and obtaining the high-temperature-resistant halogen-free flame retardant insulating multilayer composite material after heat treatment; the thickness of the polyimide film is 0.025mm, the thickness of the mica tape is 0.060mm, and the thickness of the glass cloth is 0.030mm; coating weight of halogen-free flame retardant: 60mg/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Coating weight of modified silicone pressure sensitive adhesive: 35mg/m 2 。
Example 6
The present example provides a multilayer composite material prepared by the steps of:
the polyimide film, the mica tape (model: 501) and the glass cloth were coated with the halogen-free flame retardant prepared in example 2 on both sides, respectively, and then the modified silicone pressure-sensitive adhesive prepared in example 4 was coated on both sides of the mica tape coated with the halogen-free flame retardant, and the single side coating of the glass cloth coated with the halogen-free flame retardant was changedPlacing a polyimide film, a mica tape and glass cloth in sequence from top to bottom for mechanical compounding, wherein the pressure of the mechanical compounding is 10kN, the working beat is 12 times/min, the temperature of the heat treatment is 80+/-5 ℃ after the compounding, and the high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material is obtained after the heat treatment; the thickness of the polyimide film is 0.025mm, the thickness of the mica tape is 0.060mm, and the thickness of the glass cloth is 0.030mm; coating weight of halogen-free flame retardant: 80mg/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Coating weight of modified silicone pressure sensitive adhesive: 25mg/m 2 。
Example 7
The present example provides a multilayer composite material prepared by the steps of:
coating the halogen-free flame retardant prepared in the example 1 on the two sides of a polyimide film, a mica tape (model: 501) and glass cloth respectively, coating the modified organic silicon pressure-sensitive adhesive prepared in the example 4 on the two sides of the mica tape coated with the halogen-free flame retardant, coating the modified organic silicon pressure-sensitive adhesive on one side of the glass cloth coated with the halogen-free flame retardant, then placing the polyimide film, the mica tape and the glass cloth in sequence from top to bottom for mechanical compounding, wherein the mechanical compounding pressure is 10kN, the working beat is 12 times/min, and after compounding, the heat treatment temperature is 80+/-5 ℃, and obtaining the high-temperature-resistant halogen-free flame retardant insulating multilayer composite material after heat treatment; the thickness of the polyimide film is 0.025mm, the thickness of the mica tape is 0.060mm, and the thickness of the glass cloth is 0.030mm; coating weight of halogen-free flame retardant: 100mg/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Coating weight of modified silicone pressure sensitive adhesive: 20mg/m 2 。
Comparative example 2
In this comparative example, compared with example 7, the modified silicone pressure-sensitive adhesive was changed to the silicone pressure-sensitive adhesive prepared in comparative example 1, and the remaining raw materials and preparation process were the same as in example 7.
Comparative example 3
In this comparative example, compared with comparative example 2, the polyimide film was changed to glass cloth, and the remaining raw materials and the preparation process were kept the same as those of comparative example 2.
Performance tests were performed on examples 5-7 and comparative examples 2-3, and the results are shown in table 1:
TABLE 1
Figure BDA0004058986360000081
Figure BDA0004058986360000091
As can be seen from the test results in Table 1, the composite material prepared in the examples of the present invention has higher electrical strength than the products prepared in comparative examples 2 to 3, and the volume resistivity at 200℃is more than 1.0X10 12 Omega.m, has excellent insulating property, and the resistivity at 200 ℃ is reduced by only one order of magnitude, which shows that the influence of high temperature on volume resistivity is smaller, and further shows that the composite material can be used at 200 ℃ for resisting high temperature.
The prepared composite material has a better halogen-free flame retardant effect, achieves the flame retardant grade V-O, can be automatically extinguished within a very short time after leaving flame, and has a good flame retardant effect on fire hazards possibly occurring in electrical equipment; in addition, the halogen-containing flame retardant is not added in the system of the composite material, toxic and pollutant substances are not contained, and gas which is harmful to human beings and the environment is not released after the combustion, so that the flame retardant performance is better.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material is characterized in that a polyimide film, a mica tape and glass cloth are sequentially arranged from top to bottom; the polyimide film, the mica tape and the glass cloth are coated with halogen-free flame retardant on both sides, and the polyimide film, the mica tape and the glass cloth coated with the halogen-free flame retardant are bonded through modified organic silicon pressure sensitive adhesive; the halogen-free flame retardant comprises the following raw materials in percentage by weight: 55-65% of triazine compounds, 25-35% of epoxy anhydride resin, 0.8-1.5% of flatting agents, 0.8-1.5% of antioxidants and 8-20% of flame retardant auxiliary agents; the triazine compound is a triazinetrione compound and a triazinetriamine compound, and the mass ratio of the triazinetrione compound to the triazinetriamine compound is 3:7, mixing; the halogen-free flame retardant is prepared through the following steps:
premixing the raw materials for 15min, extruding and tabletting on an extruder, wherein the extruding temperature is 110 ℃ in the first area, 130 ℃ in the second area, and crushing and sieving with a 300-mesh sieve to obtain the halogen-free flame retardant;
the structural formula of the triazinetrione compound is shown as follows:
Figure FDA0004058986350000011
the structural formula of the triazine triamine compound is shown as follows:
Figure FDA0004058986350000012
2. the high temperature resistant halogen-free flame retardant insulating multilayer composite material of claim 1, wherein the flame retardant auxiliary comprises the following components in percentage by weight: 50wt% of polyphenylene sulfide resin GF00, 25wt% of plasticizer and 25wt% of coupling agent SG-Si171; dissolving coupling agent SG-Si171 in water to prepare 10-30% solution, adding other components, stirring in a homogenizer for 3-5h, mixing uniformly, drying in a vacuum drying oven at 105 ℃ and minus 0.09MPa for 4-6h, and crushing to obtain the flame retardant auxiliary agent.
3. The high temperature resistant halogen-free flame retardant insulating multilayer composite material according to claim 2, wherein the plasticizer is one of glyceryl triacetate, tri-n-butyl citrate and acetyl tri-n-butyl citrate.
4. The high temperature resistant halogen-free flame retardant insulating multilayer composite material of claim 1, wherein the modified organosilicon pressure sensitive adhesive is prepared by the following steps:
step one, adding nano powder and a silane coupling agent A151 into a mixed solution of absolute ethyl alcohol and toluene, performing ultrasonic treatment for 30-40min at the temperature of 45 ℃, filtering, and drying to obtain pretreated nano powder; the dosage ratio of the mixed solution of the nano powder, the silane coupling agent A151, the absolute ethyl alcohol and the toluene is 1g:1g:20mL; the volume ratio of the absolute ethyl alcohol to the toluene in the mixed solution of the absolute ethyl alcohol and the toluene is 6.5:3.5;
secondly, stirring and mixing the pretreated nano powder and the organic silicon pressure-sensitive adhesive, and adding dibenzoyl peroxide to obtain a modified organic silicon pressure-sensitive adhesive; the mass ratio of the pretreated nano powder to the organosilicon pressure-sensitive adhesive is 3:5.
5. the high temperature resistant halogen-free flame retardant insulating multilayer composite material according to claim 4, wherein the nano powder is nano SiC and nano Al 2 O 3 According to the mass ratio of 1.5:1, mixing; the average grain diameter of the nano SiC is 30nm; nano Al 2 O 3 The average particle diameter of (2) is 30nm.
6. The high temperature resistant halogen-free flame retardant insulating multilayer composite of claim 1, wherein the multilayer composite is prepared by:
the preparation method comprises the steps of respectively coating the two sides of a polyimide film, a mica tape and glass cloth with halogen-free flame retardant, coating the two sides of the mica tape coated with the halogen-free flame retardant with modified organosilicon pressure-sensitive adhesive, coating the one sides of the glass cloth coated with the halogen-free flame retardant with modified organosilicon pressure-sensitive adhesive, then placing the polyimide film, the mica tape and the glass cloth in sequence from top to bottom for mechanical compounding, and after compounding, obtaining the high-temperature-resistant halogen-free flame-retardant insulating multilayer composite material after heat treatment.
7. The high temperature resistant halogen-free flame retardant insulating multilayer composite material according to claim 6, wherein the thickness of the polyimide film is 0.025mm, the thickness of the mica tape is 0.060mm, and the thickness of the glass cloth is 0.030mm; coating weight of halogen-free flame retardant: 60-100mg/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Coating weight of modified silicone pressure sensitive adhesive: 20-35mg/m 2 。
8. The high temperature resistant halogen-free flame retardant insulating multilayer composite material according to claim 6, wherein the pressure of mechanical compounding is 10kN and the working time is 12 times/min.
9. The high temperature resistant halogen-free flame retardant insulating multilayer composite of claim 6, wherein the temperature of the heat treatment is 80 ± 5 ℃.
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