CN114496349A - Ultra-long high-temperature-resistant mica tape and preparation method thereof - Google Patents
Ultra-long high-temperature-resistant mica tape and preparation method thereof Download PDFInfo
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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Abstract
The application relates to the technical field of mica tape manufacturing, and particularly discloses an ultralong high-temperature-resistant mica tape and a preparation method thereof. A super-long high-temperature resistant mica tape comprises an alkali-free glass fiber cloth, a first adhesive layer, synthetic mica paper and a second adhesive layer which are compounded in sequence; the first adhesive layer is formed by spraying a first adhesive on the surface of the synthetic mica paper in a dot matrix manner. The preparation method comprises the following steps: s1, pretreating the synthetic mica paper; s2, semi-curing the first adhesive; s3, compounding alkali-free glass fiber cloth on the side, coated with the first adhesive, of the synthetic mica paper to obtain a composite layer A, turning the composite layer A by 180 degrees to enable the glass cloth in the composite layer A to be arranged below the synthetic mica paper, then uniformly spraying a second adhesive on the side, not coated with benzoyl peroxide, of the synthetic mica paper, and baking, cutting and rolling to obtain a product; in addition, the product prepared by the preparation method has the advantage of improving the insulating property of the mica tape after vacuum pressure impregnation treatment.
Description
Technical Field
The application relates to the technical field of mica tape manufacturing, in particular to an ultralong high-temperature-resistant mica tape and a preparation method thereof.
Background
The mica tape is a material which is widely applied to the fields of motor insulation, cables and the like and has an excellent insulation effect, and the mica tape is generally of a multilayer structure consisting of mica paper, a reinforcing material, a binder and the like.
With the continuous development of the electrical industry, people have higher requirements on electric machines and electric appliances, and equipment such as transformer equipment develops towards high voltage and high capacity, which puts higher requirements on the heat resistance and the insulation effect of the mica tape.
In view of the above-mentioned related technologies, the invention considers that in the vacuum pressure impregnation process, the mica tape with a multilayer structure is difficult to be completely impregnated and permeated by the impregnating resin, so that air gaps appear in the mica tape after vacuum pressure impregnation, and the overall insulation performance of the product is affected.
Disclosure of Invention
In order to improve the insulating property of the mica tape after vacuum pressure impregnation treatment, the application provides the ultralong high-temperature-resistant mica tape and the preparation method thereof.
In a first aspect, the application provides an ultralong high temperature resistant mica tape, which adopts the following technical scheme: an ultralong high-temperature resistant mica tape comprises an alkali-free glass fiber cloth, a first adhesive layer, synthetic mica paper and a second adhesive layer which are compounded in sequence; the first adhesive layer is formed by spraying a first adhesive on the surface of the synthetic mica paper in a dot matrix manner, and the second adhesive layer is formed by spraying a second adhesive on the surface of the synthetic mica paper in a dot matrix manner; the first adhesive is prepared from the following raw materials: biphenyl type epoxy resin and heat conduction filler, and the mass ratio of heat conduction filler to biphenyl type epoxy resin is 21: 15-17.
By adopting the technical scheme, the first adhesive layer and the second adhesive layer are respectively formed by spraying the first adhesive and the second adhesive on the surface of the synthetic mica paper, so that the alkali-free glass fiber is distributed between the synthetic mica paper to form a plurality of pore structures, the air permeability of the application is improved, impregnating resin is favorably soaked into a mica tape, and the insulating property of the mica tape after vacuum pressure impregnation treatment is further improved, the application limits the dosage ratio between the modified heat-conducting filler and the biphenyl epoxy resin, so that the whole structural stability and the heat resistance of the application are further improved, in addition, the biphenyl epoxy resin has a symmetrical structure and excellent electrical property, on one hand, the insulating effect of the first adhesive in the application can be improved, on the other hand, the free volume in the first adhesive can be reduced, and the filling amount of the heat-conducting filler is improved, thereby comprehensively improving the heat resistance and the insulating property of the application.
Preferably, the second adhesive is prepared from the following raw materials in parts by weight: 45-50 parts of epoxy resin, 15-20 parts of heat-conducting filler, 6-8 parts of 4,4' -diaminodiphenyl sulfone, 0.1-0.5 part of N, N-dimethylbenzylamine and 6-8 parts of p-phenylenediamine.
Through adopting above-mentioned technical scheme, 4 '-diamino diphenyl sulfone and p-phenylenediamine all play the effect of curing agent in this application, and in the epoxy resin reaction process, take place crosslinking reaction through amine group and bisphenol A epoxy resin with the curing agent after compounding 4,4' -diamino diphenyl sulfone and p-phenylenediamine, can improve the heat resistance of this application on the one hand, and on the other hand can inject heat conduction filler position for the thermal motion of heat conduction filler is obstructed under high temperature environment, thereby has improved the high temperature resistance of this application.
Preferably, the epoxy resin in the second adhesive is a composite epoxy resin, and the composite epoxy resin is prepared from the following raw materials: bisphenol S epoxy resin and bisphenol A epoxy resin, wherein the mass ratio of the bisphenol S epoxy resin to the bisphenol A epoxy resin is 12: 3-5.
Through adopting above-mentioned technical scheme, this application carries out the complex formulation with bisphenol A epoxy resin and the bisphenol S epoxy resin that has good high temperature resistance to synthesize the heat resistance who improves this application, and this application is through injecing the mass ratio between the two, thereby further improved the heat-resisting effect of this application.
Preferably, the second adhesive is prepared by the following steps:
s31, preparing composite epoxy resin;
s32, mixing the composite epoxy resin prepared in the S31 and the heat-conducting filler according to the mass ratio of 6: (1-3) and uniformly stirring to obtain a mixed material, uniformly mixing and stirring the 4,4' -diaminodiphenyl sulfone and the p-phenylenediamine at the temperature of 180-188 ℃, cooling to the temperature of 50-60 ℃, and uniformly mixing and stirring the mixed material and the N, N-dimethylbenzylamine in a toluene solution to obtain a second binder.
Through adopting above-mentioned technical scheme, this application is through injecing the mass ratio between compound epoxy and the modified heat conduction filler to the heat resistance of this application is improved comprehensively.
Preferably, the heat conducting fillers used in the first adhesive and the second adhesive are modified heat conducting fillers, and the modified heat conducting fillers are prepared from the following raw materials: methacryloxypropyl trimethoxy silane, hexagonal boron nitride micro powder, nano glass micro powder, nano alumina, zinc oxide whisker and nano boron nitride composite glass fiber.
By adopting the technical scheme, the methacryloxypropyl trimethoxysilane is adopted to modify the surfaces of the hexagonal boron nitride micro powder, the nano glass micro powder, the nano aluminum oxide, the zinc oxide whisker and the nano boron nitride composite glass fiber, so that the dispersion performance of the heat-conducting filler in a first adhesive and a second adhesive system is comprehensively improved, in addition, the nano aluminum oxide has a larger heat conductivity coefficient compared with common aluminum oxide, and a zero-dimensional structure of the nano aluminum oxide can be filled between the hexagonal boron nitride micro powder and the zinc oxide whisker, on one hand, the compactness among different heat-conducting particles can be improved, on the other hand, the heat-conducting effect of the mica paper can be further improved, in addition, as the mica paper has more pore structures, after the mica tape is subjected to vacuum pressure impregnation treatment, the resin for impregnation can be filled among the pores of the mica paper, but can have adverse effect to mica paper's heat conduction on the contrary, so this application is through adding the less and nano particle that has good electrically conductive effect of particle size for thereby the heat conduction effect of this application overall material is improved to the vacancy nature of nano particle filling in mica paper.
Preferably, the nano boron nitride composite glass fiber is prepared by the following steps:
s11, pretreating the fiber, and removing impurities from the surface of the glass fiber;
s12, carrying out dopamine surface treatment on fibers, mixing and stirring 45-55 parts of pretreated glass fibers in S11 and 4-6 parts of dopamine hydrochloride in a trihydroxymethyl aminomethane solution with the mass concentration of 1.0-1.5g/L uniformly at the temperature of 20-30 ℃ and under the condition that the pH value is 8-9, and filtering, washing with water, and carrying out freeze drying to prepare dopamine modified glass fibers;
and S13, mixing 10-15 parts of dopamine hydrochloride, 10-15 parts of nano boron nitride and 45-55 parts of dopamine modified glass fiber prepared in S12 in a trihydroxymethyl aminomethane solution with the mass concentration of 1.0-1.5g/L at the temperature of 20-30 ℃ and at the pH value of 8-9, stirring for 5-6h, washing with water, and drying to prepare the nano boron nitride composite glass fiber.
By adopting the technical scheme, the nano boron nitride is a high-insulation material, and the dopamine is precipitated on the surface of the glass fiber under the combined action of non-covalent bond self-service assembly and covalent bond polymerization under the alkaline condition, so that the nano boron nitride with excellent insulation effect is adsorbed on the surface of the dopamine surface treatment fiber under the intermolecular action, and the heat resistance and the insulation property of the nano boron nitride are improved; in addition, a polydopamine layer is deposited on the surface of the nano boron nitride under the alkaline condition in the step S14, so that hydrogen bonds can be formed between catechol groups on the surface of the dopamine modified glass fiber and catechol groups deposited on the surface of the boron nitride and epoxy resin, the connection stability between the nano boron nitride composite glass fiber and the epoxy resin is improved, and the mechanical property, the high temperature resistance and the insulating property of the composite glass fiber are comprehensively improved.
Preferably, the tris solution in the steps S12 and S13 is prepared by: mixing 11-13 parts of tris (hydroxymethyl) aminomethane in 9500-1000 parts of deionized water, stirring uniformly, adding 0.8-1.2mol/L hydrochloric acid solution to adjust the pH value to 8-9, and obtaining tris (hydroxymethyl) aminomethane solution.
By adopting the technical scheme, the pH value of the trihydroxymethyl aminomethane solution is limited by preparing the trihydroxymethyl aminomethane solution, so that the accuracy of regulating the pH value of dopamine deposited on the surfaces of glass fibers and nano boron nitride is improved, the dopamine deposition effect is improved, the nano boron nitride is more uniformly dispersed on the surfaces of the glass fibers, and the preparation convenience, the mechanical property, the high temperature resistance and the insulating property of the product are improved.
Preferably, the modified heat-conducting filler is prepared by the following steps:
s21, mixing and stirring 2-4 parts of methacryloxypropyltrimethoxysilane and 300-500 parts of 95% ethanol solution uniformly to obtain a mixed solution A;
s22, mixing and stirring 51-55 parts of hexagonal boron nitride micro powder and 28-32 parts of nano glass micro powder uniformly to obtain a mixed solid A, and mixing and stirring 28-32 parts of nano alumina and 63-68 parts of zinc oxide whisker uniformly to obtain a mixed solid B;
s23, ultrasonically dispersing the mixed solution A and the mixed solid A at 55-65 ℃ for 1.5-2h, adding the mixed solid B, ultrasonically dispersing for 1.2-1.8h, dripping 90-110 parts of deionized water at the speed of 0.2-0.8 part/min, heating to 79-82 ℃ for vacuum reflux to remove ethanol, and vacuum drying at 55-65 ℃ to obtain a mixture D;
s24, mixing and stirring uniformly 35-45 parts of nano boron nitride composite glass fiber and the mixture C to obtain the modified heat-conducting filler.
Through adopting above-mentioned technical scheme, this application is through the quantity of injecing different heat conduction filler, and mixes the heat conduction filler of different crystal forms and size respectively to reduced the possibility that nanometer glass miropowder and nanometer aluminium oxide take place the reunion, in addition, this application divides batch to carry out ultrasonic dispersion with mixture A and mixed solid B, thereby further improved the possibility that takes place the reunion between the different fillers, thereby synthesized the heat resistance effect of this application.
In a second aspect, the application provides a preparation method of an ultralong high-temperature resistant mica tape, which adopts the following technical scheme:
a preparation method of an ultralong high-temperature-resistant mica tape comprises the following steps:
s1, pretreating the synthetic mica paper, and uniformly coating a layer of benzoyl peroxide on the upper surface of the synthetic mica paper;
s2, semi-curing the first adhesive, uniformly spraying the first adhesive on the side, coated with benzoyl peroxide, of the synthetic mica paper, and shaping for 2-5min at 75-85 ℃;
s3, removing impurities from the surface of the alkali-free glass fiber cloth, compounding the alkali-free glass fiber cloth on the side, coated with the first adhesive, of the synthetic mica paper to obtain a composite layer A, turning the composite layer A180 degrees, enabling the glass cloth in the composite layer A to be arranged below the synthetic mica paper, then uniformly spraying the second adhesive on the side, not coated with benzoyl peroxide, of the synthetic mica paper, baking at the temperature of 145-155 ℃ for 5-10min, cutting and rolling to obtain the product.
By adopting the technical scheme, the first adhesive and the second adhesive are compounded on the surface of the synthetic mica paper in a spraying mode, so that on one hand, the dosage of the adhesive can be reduced, on the other hand, gaps can be formed on the surfaces of the glass cloth and the mica paper, thereby improving the air permeability of the application, being beneficial to soaking the impregnating resin in the subsequent vacuum pressure impregnation process, in the application, the first adhesive coated on the surface of the synthetic mica paper is semi-cured, so that a gap structure formed between the glass cloth and the mica paper is more stable, and the air permeability of the product is further improved, in addition, after the upper surface and the lower surface of the synthetic mica paper are both coated with a layer of benzoyl peroxide, the connection strength between the first adhesive and the synthetic mica paper and the second adhesive and the synthetic mica paper are improved, so that the stability of the whole structure of the paper is comprehensively improved.
In summary, the present application has the following beneficial effects:
1. in addition, the biphenyl epoxy resin has excellent electrical performance and heat resistance, the free volume in the first adhesive can be reduced, the filling amount of the heat-conducting filler is increased, and the heat resistance and the insulating performance of the heat-conducting filler are improved comprehensively;
2. according to the method, the first adhesive and the second adhesive are compounded on the surface of the synthetic mica paper in a spraying mode, so that the using amount of the adhesives can be reduced, and gaps can be formed between the glass cloth and the surface of the mica paper, so that the air permeability of the method is improved, and impregnation resin can be soaked in the subsequent vacuum pressure impregnation process.
Detailed Description
The present application is described in further detail below with reference to preparation examples and examples.
Raw materials
Table 1 source table of raw materials used in the present application
Preparation example
Preparation example 1
The nano boron nitride composite glass fiber is prepared by the following steps:
s11, preparing a tris (hydroxymethyl) aminomethane solution, mixing and stirring 12.1g of tris (hydroxymethyl) aminomethane in 9.5L of deionized water at the rotating speed of 150rpm for 15min to obtain a solution A with uniform texture, and adjusting the pH value of the solution A to 8.5 by 1mol/L hydrochloric acid solution to obtain the tris (hydroxymethyl) aminomethane solution;
s12, pretreating fibers, namely, putting 50g of glass fibers into an oven at 25 ℃, heating to 600 ℃ at a speed of 10 ℃/min, carrying out heat preservation treatment for 1h, cleaning the fibers for 3 times by using deionized water, carrying out ultrasonic dispersion (28KHz and 1000W) in an ultrasonic oscillator for 20min, and drying at 65 ℃ for 20min to obtain pretreated glass fibers;
s13, treating the surface of dopamine, sequentially adding 5L of a trihydroxymethylaminomethane solution prepared in S11, 50g of a pretreated glass fiber prepared in S12 and 5.35g of dopamine hydrochloride into a reaction kettle, mixing and stirring at 25 ℃ and 100rpm for 25 hours, filtering the glass fiber, washing the glass fiber for 3 times by using deionized water, and freeze-drying the glass fiber for 10 minutes by using a freeze-drying machine (SCIENTZ-25T freeze-drying machine sold by Ningbo New Ganoderma Freeze-drying Equipment GmbH) to prepare the dopamine modified glass fiber;
s14, mixing and stirring 4.5L of the tris solution prepared in S11, 12g of dopamine hydrochloride, 0.5L of absolute ethyl alcohol, 12g of nano boron nitride and 50g of dopamine modified glass fiber prepared in S13 in a magnetic stirrer (DF-101T 15L heat collection type magnetic stirrer sold by Shanghai Lingke industry development Co., Ltd.) at room temperature and 300rpm for 5.5h, filtering the fiber, washing the fiber with deionized water for 3 times, and baking the fiber in an oven at 60 ℃ for 20min to prepare the nano boron nitride composite glass fiber.
Preparation example 2
This production example is different from production example 1 in that the step of S12 was not performed in this production example.
Preparation example 3
This production example is different from production example 1 in that the step S13 was not performed in this production example, and the pretreated glass fiber obtained in step S12 was used as it is in step S14.
Preparation example 4
The present preparation example is different from preparation example 1 in that it replaces dopamine hydrochloride with an equal mass of deionized water in step S13.
Preparation example 5
The modified heat-conducting filler is prepared by the following steps:
s21, mixing and stirring 4g of methacryloxypropyltrimethoxysilane and 500mL of ethanol solution with the purity of 95% uniformly in a reaction kettle at the rotating speed of 1000rpm to obtain a mixed solution A;
s22, mixing and stirring 54g of hexagonal boron nitride micro powder and 30g of nano glass micro powder in a reaction kettle at the rotating speed of 500rpm for 20min to obtain a mixed solid A, and mixing and stirring 30g of nano alumina and 66g of zinc oxide whisker in the reaction kettle at the rotating speed of 500rpm for 20min to obtain a mixed solid B;
s23, ultrasonically dispersing the mixed liquid A prepared in S21 and the mixed solid A prepared in S22 in an ultrasonic oscillator (an ultrasonic stirring tank sold by Hangzhou vibration source ultrasonic equipment Co., Ltd. and having a model number of ZYCS) for 1.8h at 60 ℃, continuously adding the mixed solid B into the ultrasonic oscillator for ultrasonically dispersing (28KHz, 1000W) for 1.5h to obtain a mixture C, transferring the mixture C into a reaction kettle, mixing and stirring at the rotating speed of 200rpm for 50min, adding 100mL of deionized water into the reaction kettle at the speed of 0.5mL/min during the continuous stirring of the mixture C, heating to 80 ℃ (79-82 ℃), removing ethanol and other small molecular substances by vacuum reflux, and finally vacuumizing and drying at 60 ℃ for 20min to obtain a mixture D;
s24, mixing and stirring 40g of the nano boron nitride composite glass fiber prepared in the preparation example 1 and the mixture D prepared in the step S23 at the rotating speed of 200rpm for 20min to obtain the modified heat-conducting filler.
Preparation example 6
This production example is different from production example 5 in that it replaces methacryloxypropyltrimethoxysilane with an equal mass of gamma-glycidoxypropyltrimethoxysilane in step S21.
Preparation example 7
The present production example differs from production example 5 in that the present production example does not use the nano glass fine powder in step S22.
Preparation example 8
The present production example differs from production example 5 in that the hexagonal boron nitride fine powder is not used in step S22.
Preparation example 9
The present production example is different from production example 5 in that nano alumina is not used in step S22.
Preparation example 10
This production example is different from production example 5 in that zinc oxide whiskers were not used in step S22.
Preparation example 11
The difference between the preparation example and the preparation example 5 is that the step S23 of the preparation example is specifically as follows: ultrasonically dispersing (28KHz, 1000W) the mixed solid A and the mixed solid B prepared in the mixed solution A, S22 prepared in S21 in an ultrasonic oscillator (an ultrasonic stirring tank sold by Hangzhou vibration source ultrasonic equipment Co., Ltd. and having a model of ZYCS) for 3.3h at 60 ℃ to obtain a mixture C, transferring the mixture C into a reaction kettle, mixing and stirring at the rotating speed of 200rpm for 50min, adding 100mL of deionized water into the reaction kettle at the speed of 0.5mL/min during the continuous stirring process of the mixture C, heating to 80 ℃ (79-82 ℃), removing ethanol and other small molecular substances by vacuum reflux, and finally vacuumizing and drying at 60 ℃ for 20min to obtain a mixture D.
Preparation example 12
The modified heat-conducting filler in the preparation example is prepared by the following steps:
s21, mixing and stirring 4g of methacryloxypropyltrimethoxysilane and 500mL of ethanol solution with the purity of 95% uniformly in a reaction kettle at the rotating speed of 1000rpm to obtain a mixed solution A;
s22, mixing and stirring 54g of hexagonal boron nitride micro powder, 30g of nano glass micro powder, 30g of nano alumina and 66g of zinc oxide whisker in a reaction kettle at the rotating speed of 500rpm for 40min to obtain a mixed solid a;
s23, ultrasonically dispersing the mixed solution A prepared in the S21 and the mixed solid a prepared in the S22 in an ultrasonic oscillator (an ultrasonic stirring tank sold by Hangzhou vibration source ultrasonic equipment Co., Ltd. and having a model of ZYCS) at 60 ℃ for 3.3 hours to obtain a mixture b, transferring the mixture b into a reaction kettle, mixing and stirring at the rotating speed of 200rpm for 50 minutes, adding 100mL of deionized water into the reaction kettle at the speed of 0.5mL/min during the continuous stirring process of the mixture b, heating to 80 ℃ (79-82 ℃), removing ethanol and other small molecular substances by vacuum reflux, and finally, vacuumizing and drying at 60 ℃ for 20 minutes to obtain a mixture d;
s24, mixing and stirring 40g of the nano boron nitride composite glass fiber prepared in the preparation example 1 and the mixture d prepared in the step S23 at the rotating speed of 200rpm for 20min to obtain the modified heat-conducting filler.
Preparation example 13
The present production example is different from production example 5 in that the nano boron nitride composite glass fiber prepared in production example 1 was replaced with the nano boron nitride composite glass fiber prepared in production example 2 of equal mass in S24.
Preparation example 14
The present production example is different from production example 5 in that the nano boron nitride composite glass fiber prepared in production example 1 was replaced with the nano boron nitride composite glass fiber prepared in production example 3 of equal mass in S24.
Preparation example 15
The present production example is different from production example 5 in that the nano boron nitride composite glass fiber produced in production example 1 was replaced with the nano boron nitride composite glass fiber produced in production example 4 of equal mass in S24.
Preparation example 16
The present production example is different from production example 5 in that the nano boron nitride composite glass fiber prepared in production example 1 was replaced with an equal mass of glass fiber in S24.
Preparation example 17
The first adhesive is prepared by the following steps: the modified heat-conducting filler prepared in preparation example 5 and biphenyl epoxy resin are mixed according to a mass ratio of 21: 16, mixing and stirring for 45min at the rotating speed of 250rpm, extruding and granulating by a double-screw extruder, and crushing and sieving in a crusher to obtain the first adhesive with the average particle size of less than 100 meshes, wherein the temperature of a feeding section of the double-screw extruder is 130 ℃, the temperature of a melting section of the double-screw extruder is 150 ℃, the temperature of a neck ring mold of the double-screw extruder is 150 ℃, and the rotating speed of screws of the extruder is 180 r/min.
Preparation example 18
The difference between the preparation example and the preparation example 17 is that the mass ratio of the modified heat-conducting filler to the biphenyl epoxy resin in the preparation example is 21: 15.
Preparation example 19
The difference between the preparation example and the preparation example 17 is that the mass ratio of the modified heat-conducting filler to the biphenyl epoxy resin in the preparation example is 21: 17.
Preparation example 20
The difference between the preparation example and the preparation example 17 is that the mass ratio of the modified heat-conducting filler to the biphenyl epoxy resin in the preparation example is 21: 12.
Preparation example 21
The difference between the preparation example and the preparation example 17 is that the mass ratio of the modified heat-conducting filler to the biphenyl epoxy resin in the preparation example is 21: 20.
Preparation example 22
This production example is different from production example 17 in that an equal mass of bisphenol a epoxy resin was used in place of the biphenyl type epoxy resin.
Preparation example 23
The present preparation example is different from preparation example 17 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 6 of equal mass.
Preparation example 24
The present preparation example is different from preparation example 17 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 7 of equal mass.
Preparation example 25
The preparation example is different from the preparation example 17 in that the modified heat conductive filler prepared in the preparation example 5 is replaced by the modified heat conductive filler prepared in the preparation example 8 with equal mass.
Preparation example 26
The preparation example is different from the preparation example 17 in that the modified heat conductive filler prepared in the preparation example 5 is replaced by the modified heat conductive filler prepared in the preparation example 9 with equal mass.
Preparation example 27
The preparation example is different from the preparation example 17 in that the modified heat conductive filler prepared in the preparation example 5 is replaced by the modified heat conductive filler prepared in the preparation example 10 with equal mass.
Preparation example 28
The present preparation example is different from preparation example 17 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 11 of equal mass.
Preparation example 29
The preparation example is different from the preparation example 17 in that the modified heat conductive filler prepared in the preparation example 5 is replaced by the modified heat conductive filler prepared in the preparation example 12 with equal mass.
Preparation example 30
The present preparation example is different from preparation example 17 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 13 of equal mass.
Preparation example 31
The preparation example is different from the preparation example 17 in that the modified heat conductive filler prepared in the preparation example 5 is replaced by the modified heat conductive filler prepared in the preparation example 14 with equal mass.
Preparation example 32
The preparation example is different from the preparation example 17 in that the modified heat-conducting filler prepared in the preparation example 5 is replaced by the modified heat-conducting filler prepared in the preparation example 15 with equal mass.
Preparation example 33
The preparation example is different from the preparation example 17 in that the modified heat conductive filler prepared in the preparation example 5 is replaced by the modified heat conductive filler prepared in the preparation example 16 with equal mass.
Preparation example 34
The second adhesive is prepared by the following steps:
s31, preparing composite epoxy resin, putting bisphenol S epoxy resin and bisphenol A epoxy resin into the reaction according to the mass ratio of 12:4, and mixing and stirring at the rotating speed of 200rpm for 40min to obtain the composite epoxy resin;
s32, mixing the composite epoxy resin prepared in the S31 and the modified heat-conducting filler prepared in the preparation example 5 in a mass ratio of 6: 2 in a reaction kettle at the rotating speed of 1000rpm and uniformly stirring to obtain a mixed material with the mass of 65g, mixing 6.5g of 4,4' -diaminodiphenyl sulfone and 6.5g of p-phenylenediamine at 185 ℃, uniformly stirring, cooling to 55 ℃, mixing with the mixed material, 0.3g of N, N-dimethylbenzylamine and 500ml of toluene solution at the rotating speed of 100rpm, and stirring for 1h to obtain a second binder.
Preparation example 35
This production example is different from production example 34 in that it replaces the bisphenol S epoxy resin with an equal mass of bisphenol a epoxy resin in step S31.
Preparation example 36
This production example is different from production example 34 in that this production example replaces 4,4' -diaminodiphenyl sulfone with p-phenylenediamine of equal mass in step S32.
Preparation example 37
The difference between the preparation example and the preparation example 34 is that in the step S32, the mass ratio of the composite epoxy resin to the modified heat conductive filler is 6: 1.
preparation example 38
The difference between the preparation example and the preparation example 34 is that in the step S32, the mass ratio of the composite epoxy resin to the modified heat conductive filler is 6: 3.
preparation example 39
The difference between the preparation example and the preparation example 34 is that in step S32, the mass ratio of the composite epoxy resin to the modified heat conductive filler is 8: 1.
preparation example 40
The difference between the preparation example and the preparation example 34 is that in the step S32, the mass ratio of the composite epoxy resin to the modified heat conductive filler is 6: 4.
preparation example 41
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 6 of equal mass.
Preparation example 42
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 7 of equal mass.
Preparation example 43
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 8 of equal mass.
Preparation example 44
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 9 of equal mass.
Preparation example 45
The preparation example is different from the preparation example 34 in that the modified heat conductive filler prepared in the preparation example 5 is replaced by the modified heat conductive filler prepared in the preparation example 10 with equal mass.
Preparation example 46
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 11 of equal mass.
Preparation example 47
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 12 of equal mass.
Preparation example 48
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 13 of equal mass.
Preparation example 49
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 14 of equal mass.
Preparation example 50
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 15 of equal mass.
Preparation example 51
The present preparation example is different from preparation example 34 in that the modified heat conductive filler obtained in preparation example 5 was replaced with the modified heat conductive filler obtained in preparation example 16 of equal mass.
Examples
Example 1
The ultralong high-temperature-resistant mica tape is prepared by the following steps:
s1, pretreating the synthetic mica paper, uniformly coating a layer of benzoyl peroxide on the upper surface of the synthetic mica paper through a coating machine, and standing for 5 min;
s2, semi-curing the first adhesive, uniformly spraying the first adhesive prepared in preparation example 17 in a powder state onto the side of the synthetic mica paper coated with benzoyl peroxide by a spraying device (five-axis numerical control automatic spraying machine sold by asahi robot automation equipment ltd, shenzhen city), and then placing the synthetic mica paper in an oven to bake for 3min at 80 ℃;
s3, uniformly wiping one side of the alkali-free glass fiber cloth once through absolute alcohol, after the alcohol naturally volatilizes, keeping the alkali-free glass fiber cloth in a horizontal state on a coating machine through a unreeling shaft, a compression roller and a reeling shaft, compounding the side, wiped by the absolute alcohol, of the alkali-free glass fiber cloth on the side, coated with the first adhesive, of the synthetic mica paper to obtain a composite layer A, turning the composite layer A by 180 degrees, enabling the glass cloth in the composite layer A to be arranged below the synthetic mica paper, then uniformly spraying the second adhesive prepared in the powder state in preparation example 34 to the side, not coated with the benzoyl peroxide, of the synthetic mica paper through a spraying device (a five-axis numerical control automatic spraying machine sold by Asahi robot automation equipment Limited in Shenzheke department) and then placing the synthetic mica paper in an oven to be baked for 7min at 150 ℃, and then cutting and rolling to obtain the product.
Example 2
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 18.
Example 3
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 19.
Example 4
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced with an equal mass of the first adhesive prepared in preparation example 23.
Example 5
The difference between the present example and example 1 is that the first adhesive prepared in preparation example 17 was replaced by the first adhesive prepared in preparation example 24 with equal mass.
Example 6
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced with an equal mass of the first adhesive prepared in preparation example 25.
Example 7
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced with an equal mass of the first adhesive prepared in preparation example 26.
Example 8
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced with an equal mass of the first adhesive prepared in preparation example 27.
Example 9
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 28.
Example 10
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 29.
Example 11
The difference between the present example and example 1 is that the first adhesive prepared in preparation example 17 was replaced by the first adhesive prepared in preparation example 30 with equal quality.
Example 12
The difference between the present example and example 1 is that the first adhesive prepared in preparation example 17 is replaced by the first adhesive prepared in preparation example 31 with equal quality.
Example 13
The difference between the present example and example 1 is that the first adhesive prepared in preparation example 17 was replaced by the first adhesive prepared in preparation example 32 with equal quality.
Example 14
This example differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 33.
Example 15
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 35 with equal quality.
Example 16
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 36 with equal quality.
Example 17
This example differs from example 1 in that the second adhesive prepared in preparation example 34 was replaced by an equal mass of the second adhesive prepared in preparation example 37.
Example 18
This example differs from example 1 in that the second adhesive prepared in preparation example 34 was replaced by an equal mass of the second adhesive prepared in preparation example 38.
Example 19
This example differs from example 1 in that the second adhesive prepared in preparation example 34 was replaced by an equal mass of the second adhesive prepared in preparation example 39.
Example 20
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 40 with equal quality.
Example 21
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 41 with equal quality.
Example 22
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 42 with equal quality.
Example 23
This example differs from example 1 in that the second adhesive prepared in preparation example 34 was replaced by an equal mass of the second adhesive prepared in preparation example 43.
Example 24
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 44 with equal quality.
Example 25
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 45 with equal quality.
Example 26
This example differs from example 1 in that the second adhesive prepared in preparation example 34 was replaced by an equal mass of the second adhesive prepared in preparation example 46.
Example 27
This example differs from example 1 in that the second adhesive prepared in preparation example 34 was replaced by an equal mass of the second adhesive prepared in preparation example 47.
Example 28
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 48 with equal quality.
Example 29
This example differs from example 1 in that the second adhesive prepared in preparation example 34 was replaced by an equal mass of the second adhesive prepared in preparation example 49.
Example 30
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 50 with equal quality.
Example 31
The difference between the present example and example 1 is that the second adhesive prepared in preparation example 34 is replaced by the second adhesive prepared in preparation example 51 with equal quality.
Comparative example
Comparative example 1
The ultralong high-temperature-resistant mica tape is prepared by the following steps:
s1, pretreating the synthetic mica paper, uniformly coating a layer of benzoyl peroxide on the upper surface of the synthetic mica paper through a coating machine, and standing for 5 min;
s2, semi-curing the first adhesive, namely melting the first adhesive, coating the melted first adhesive on the side, coated with benzoyl peroxide, of the synthetic mica paper by using a coating machine, and then placing the synthetic mica paper in an oven to be baked for 3min at 80 ℃;
s3, uniformly wiping one side of the alkali-free glass fiber cloth once through absolute alcohol, after the alcohol naturally volatilizes, keeping the alkali-free glass fiber cloth in a horizontal state on a coating machine through an unwinding shaft, a compression roller and a winding shaft, compounding the side, wiped by the absolute alcohol, of the alkali-free glass fiber cloth on the side, coated with the first adhesive, of the synthetic mica paper to obtain a composite layer A, turning the composite layer A by 180 degrees, enabling the glass cloth in the composite layer A to be arranged below the synthetic mica paper, then melting the second adhesive in a powder state, uniformly coating the melted second adhesive on the side, not coated with the benzoyl peroxide, of the synthetic mica paper through the coating machine, then placing the synthetic mica paper in an oven, baking the synthetic mica paper for 7 minutes at 150 ℃, cutting and winding to obtain the product.
Comparative example 2
The ratio differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 20.
Comparative example 3
The ratio differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 21.
Comparative example 4
The ratio differs from example 1 in that the first adhesive prepared in preparation example 17 was replaced by an equal mass of the first adhesive prepared in preparation example 22.
Performance test
Detection method/test method
1. Air permeability (s/100 mL): reference is made to GB/T5019.12-2017 insulating Material based on mica, part 12: high air permeability glass cloth reinforced epoxy mica tapes with less glue were tested for air permeability on the mica tapes prepared in examples 1-32 and comparative examples 1-2.
Thermal state loss (%) at 2.180 ℃: the mica tapes prepared in examples 1-32 and comparative examples 1-2 were tested for thermal state loss at 180 ℃ with reference to the test method of IEC 60243-1.
3. Tensile strength (N/10 mm): reference is made to GB/T5019.12-2017 insulating Material based on mica, part 12: the tensile strength of the mica tapes prepared in the examples 1-32 and the comparative examples 1-2 is detected by a method of high-permeability glass cloth reinforced epoxy resin mica tape.
4. Electric strength (MV/m): reference is made to GB/T5019.12-2017 insulating Material based on mica, part 12: method of high air permeability glass cloth reinforced epoxy resin mica tape for electrical strength of air permeability for mica tapes prepared in examples 1-32 and comparative examples 1-2.
TABLE 2 summary of test results for examples 1-32 and comparative examples 1-2
As can be seen by combining examples 1 to 3, comparative examples 2 to 4, and table 2, the modified thermally conductive filler and the biphenyl type epoxy resin were mixed in a mass ratio of 21: 15-17 can comprehensively improve the air permeability, the thermal state loss at 155 ℃, the tensile strength and the electrical strength, and the mass ratio of the modified heat-conducting filler to the biphenyl epoxy resin is 21: at 16, the performance of the product is optimal.
By combining the examples 1, 4 to 10 and 21 to 27 and combining the table 2, it can be seen that the air permeability, the thermal loss at 155 ℃, the tensile strength and the electrical strength of the product can be comprehensively improved after the nano glass micro powder, the hexagonal boron nitride micro powder, the nano aluminum oxide, the zinc oxide whisker and the nano boron nitride composite glass fiber are compounded.
Combining example 1 and examples 15-20 with table 2, it can be seen that the heat resistance of the product can be improved comprehensively after the bisphenol a epoxy resin and the bisphenol S epoxy resin are compounded, and the electrical strength and the tensile strength of the product can also be improved by compounding p-phenylenediamine and 4,4' -diaminodiphenyl sulfone.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The ultralong high-temperature-resistant mica tape is characterized by comprising an alkali-free glass fiber cloth, a first adhesive layer, synthetic mica paper and a second adhesive layer which are compounded in sequence; the first adhesive layer is formed by spraying a first adhesive on the surface of the synthetic mica paper in a dot matrix manner, and the second adhesive layer is formed by spraying a second adhesive on the surface of the synthetic mica paper in a dot matrix manner; the first adhesive is prepared from the following raw materials: biphenyl type epoxy resin and heat conduction filler, and the mass ratio of the heat conduction filler to the biphenyl type epoxy resin is 21: 15-17.
2. The ultra-long high temperature resistant mica tape according to claim 1, characterized in that: the second adhesive is prepared from the following raw materials in parts by weight: 45-50 parts of epoxy resin, 15-20 parts of heat-conducting filler, 6-8 parts of 4,4' -diaminodiphenyl sulfone, 0.1-0.5 part of N, N-dimethylbenzylamine and 6-8 parts of p-phenylenediamine.
3. The ultra-long high temperature resistant mica tape according to claim 2, characterized in that:
the epoxy resin in the second adhesive is composite epoxy resin, and the composite resin is prepared from the following raw materials: bisphenol S epoxy resin and bisphenol A epoxy resin, wherein the mass ratio of the bisphenol S epoxy resin to the bisphenol A epoxy resin is 12: 3-5.
4. The ultra-long high temperature resistant mica tape according to claim 3, wherein:
the second adhesive is prepared by the following steps:
s31, preparing composite epoxy resin;
s32, mixing the composite epoxy resin prepared in the S31 and the heat-conducting filler according to the mass ratio of 6: (1-3) and uniformly stirring to obtain a mixed material, uniformly mixing and stirring the 4,4' -diaminodiphenyl sulfone and the p-phenylenediamine at the temperature of 180-188 ℃, cooling to the temperature of 50-60 ℃, and uniformly mixing and stirring the mixed material and the N, N-dimethylbenzylamine in a toluene solution to obtain a second binder.
5. The ultra-long high temperature resistant mica tape according to claim 2, characterized in that:
the heat conducting fillers used in the first adhesive and the second adhesive are modified heat conducting fillers, and the modified heat conducting fillers are prepared from the following raw materials: methacryloxypropyl trimethoxy silane, hexagonal boron nitride micro powder, nano glass micro powder, nano alumina, zinc oxide whisker and nano boron nitride composite glass fiber.
6. The ultra-long high temperature resistant mica tape according to claim 5, wherein: the nano boron nitride composite glass fiber is prepared by the following steps:
s11, pretreating the fiber, and removing impurities from the surface of the glass fiber;
s12, treating the surface of dopamine, mixing and stirring 45-55 parts of pretreated glass fiber in S11 and 4-6 parts of dopamine hydrochloride in a trihydroxymethyl aminomethane solution with the mass concentration of 1.0-1.5g/L uniformly at the temperature of 20-30 ℃ and under the condition that the pH is =8-9, and filtering, washing with water and freeze-drying to prepare the dopamine modified glass fiber;
s13, mixing and stirring 10-15 parts of dopamine hydrochloride, 10-15 parts of nano boron nitride and 45-55 parts of dopamine modified glass fiber prepared in S12 in a trihydroxymethyl aminomethane solution with the mass concentration of 1.0-1.5g/L at the temperature of 20-30 ℃ and with the pH =8-9 for 5-6h, and washing and drying to obtain the nano boron nitride composite glass fiber.
7. The ultra-long high temperature resistant mica tape according to claim 6, wherein: the preparation of the tris solution in the steps S12 and S13 is specifically as follows: after 11-13 parts of tris (hydroxymethyl) aminomethane is mixed and stirred uniformly in 9500-1000 parts of deionized water, 0.8-1.2mol/L hydrochloric acid solution is added to adjust the pH to be 8-9, and tris (hydroxymethyl) aminomethane solution is added.
8. The ultra-long high temperature resistant mica tape according to claim 5, wherein: the modified heat-conducting filler is prepared by the following steps:
s21, mixing and stirring 2-4 parts of methacryloxypropyltrimethoxysilane and 300-500 parts of 95% ethanol solution uniformly to obtain a mixed solution A;
s22, mixing and stirring 51-55 parts of hexagonal boron nitride micro powder and 28-32 parts of nano glass micro powder uniformly to obtain a mixed solid A, and mixing and stirring 28-32 parts of nano alumina and 63-68 parts of zinc oxide whisker uniformly to obtain a mixed solid B;
s23, ultrasonically dispersing the mixed solution A and the mixed solid A at 55-65 ℃ for 1.5-2h, adding the mixed solid B, ultrasonically dispersing for 1.2-1.8h, dripping 90-110 parts of deionized water at the speed of 0.2-0.8 part/min, heating to 79-82 ℃ for vacuum reflux to remove ethanol, and vacuum drying at 55-65 ℃ to obtain a mixture D;
s24, mixing and stirring uniformly 35-45 parts of nano boron nitride composite glass fiber and the mixture C to obtain the modified heat-conducting filler.
9. The method for preparing the ultra-long high temperature resistant mica tape according to any one of claims 1 to 8, characterized by comprising the following steps:
s1, pretreating the synthetic mica paper, and uniformly coating a layer of benzoyl peroxide on the upper surface of the synthetic mica paper;
s2, semi-curing the first adhesive, uniformly spraying the first adhesive on the side, coated with benzoyl peroxide, of the synthetic mica paper, and shaping for 2-5min at 75-85 ℃;
s3, removing impurities from the surface of the alkali-free glass fiber cloth, compounding the alkali-free glass fiber cloth on the side, coated with the first adhesive, of the synthetic mica paper to obtain a composite layer A, overturning the composite layer A by 180 degrees, so that the glass cloth in the composite layer A is arranged below the synthetic mica paper, then uniformly spraying the second adhesive on the side, not coated with benzoyl peroxide, of the synthetic mica paper, baking at the temperature of 145-155 ℃ for 5-10min, cutting and rolling to obtain the product.
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