CN114496349B - 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 ultra-long high-temperature-resistant mica tape and a preparation method thereof. The ultra-long high temperature resistant mica tape comprises alkali-free glass fiber cloth, a first adhesive layer, synthetic mica paper and a second adhesive layer which are sequentially compounded; the first adhesive layer is formed by dot matrix spraying of a first adhesive on the surface of the synthetic mica paper. The preparation method comprises the following steps: s1, preprocessing synthetic mica paper; s2, semi-curing of the first adhesive; s3, compounding alkali-free glass fiber cloth on one side of the synthetic mica paper coated with a first adhesive to obtain a composite layer A, turning the composite layer A by 180 degrees to enable glass in the composite layer A to be arranged below the synthetic mica paper, uniformly spraying a second adhesive on one side of the synthetic mica paper which is not coated with benzoyl peroxide, and baking, cutting and rolling to obtain a product; in addition, the product obtained by the preparation method has the advantage of improving the insulation performance 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 ultra-long 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 excellent insulation effect, and is a multilayer structure which is generally composed of mica paper, reinforcing materials, binders and the like.
With the continuous development of the electrical industry, people have higher requirements on electric appliances of motors, equipment of voltage transformation and the like develop towards high voltage and high capacity, and therefore, higher requirements are put on heat resistance and insulation effect of the mica tape, so that in order to improve the insulation effect of the mica tape, people often adopt a vacuum pressure impregnation method to integrally impregnate the mica tape into impregnating resin, and accordingly, the insulation performance of the mica tape is improved.
In view of the above-mentioned related art, the application considers that in the vacuum pressure impregnation process, the mica tape having a multilayer structure is hardly impregnated and permeated by the impregnating resin completely, so that an air gap is formed inside the mica tape after vacuum pressure impregnation, and the insulation performance of the whole product is affected.
Disclosure of Invention
In order to improve the insulation performance of the mica tape after vacuum pressure impregnation treatment, the application provides an ultra-long high temperature resistant mica tape and a preparation method thereof.
In a first aspect, the application provides an ultra-long high temperature resistant mica tape, which adopts the following technical scheme: an ultra-long high temperature resistant mica tape comprises alkali-free glass fiber cloth, a first adhesive layer, synthetic mica paper and a second adhesive layer which are sequentially compounded; the first adhesive layer is formed by dot-matrix spraying of a first adhesive on the surface of the synthetic mica paper, and the second adhesive layer is formed by dot-matrix spraying of a second adhesive on the surface of the synthetic mica paper; the first adhesive is prepared from the following raw materials: biphenyl epoxy resin and heat conducting filler, and the mass ratio of the heat conducting filler to the biphenyl 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 a plurality of pore structures are formed among the synthetic mica paper by the alkali-free glass fiber cloth, the air permeability of the application is improved, the impregnating resin is facilitated to soak the mica tape, the insulating property of the mica tape after vacuum pressure impregnation treatment is further improved, the application further improves the overall structural stability and heat resistance by limiting the dosage ratio between the modified heat conducting filler and the biphenyl type epoxy resin, and in addition, the biphenyl type epoxy resin has a symmetrical structure and excellent electrical performance, so that on one hand, the insulation effect of the first adhesive can be improved, on the other hand, the free volume in the first adhesive can be reduced, the filling quantity of the heat conducting filler can be increased, and the heat resistance and the insulation performance of the application can be comprehensively improved.
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.
By adopting the technical scheme, the 4,4 '-diaminodiphenyl sulfone and the p-phenylenediamine play a role of the curing agent, and the curing agent compounded by the 4,4' -diaminodiphenyl sulfone and the p-phenylenediamine is subjected to a crosslinking reaction with bisphenol A epoxy resin through amine groups in the reaction process of the epoxy resin, so that the heat resistance of the heat-conducting filler can be improved on one hand, and the positions of the heat-conducting filler can be limited on the other hand, so that the heat movement of the heat-conducting filler is blocked in a high-temperature environment, and the high-temperature resistance of the heat-conducting filler is improved.
Preferably, the epoxy resin in the second adhesive is a composite epoxy resin, and the composite resin is prepared from the following raw materials: bisphenol S epoxy resin and bisphenol A epoxy resin, and the mass ratio of the bisphenol S epoxy resin to the bisphenol A epoxy resin is 12:3-5.
By adopting the technical proposal, the application compounds bisphenol A epoxy resin with bisphenol S epoxy resin with excellent high temperature resistance, therefore, the heat resistance of the heat-resistant material is comprehensively improved, and the heat-resistant effect of the heat-resistant material is further improved by limiting the mass ratio of the heat-resistant material to the heat-resistant material.
Preferably, the second adhesive is prepared by the steps of:
s31, preparing composite epoxy resin;
s32, mixing the composite epoxy resin prepared in the step S31 with a heat-conducting filler according to a mass ratio of 6: mixing and stirring uniformly the mixture in the proportion of (1-3) to obtain a mixed material, mixing and stirring uniformly 4,4' -diaminodiphenyl sulfone and p-phenylenediamine at 180-188 ℃, cooling to 50-60 ℃, and mixing and stirring uniformly the mixed material and N, N-dimethylbenzylamine in toluene solution to obtain the second binder.
By adopting the technical scheme, the heat resistance of the application is comprehensively improved by limiting the mass ratio of the composite epoxy resin to the modified heat conducting filler.
Preferably, the heat conducting filler used in the first adhesive and the second adhesive is modified heat conducting filler, and the modified heat conducting filler is prepared from the following raw materials: methacryloxypropyl trimethoxysilane, hexagonal boron nitride micro powder, nanometer glass micro powder, nanometer aluminum oxide, zinc oxide whisker and nanometer boron nitride composite glass fiber.
According to the technical scheme, the methacryloxypropyl trimethoxysilane is adopted to modify the surfaces of hexagonal boron nitride micro powder, nano glass micro powder, nano aluminum oxide, zinc oxide whisker and 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, nano aluminum oxide has a larger heat conductivity coefficient compared with common aluminum oxide, 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 mica paper has a more pore structures, if mica tapes are subjected to vacuum pressure impregnation treatment, the impregnated resin can be filled among the pores of the mica paper, and on the contrary, the heat conducting effect of the whole material is improved by adding the nano particles with smaller particle size and excellent electric conducting effect.
Preferably, the nano boron nitride composite glass fiber is prepared by the following steps:
s11, preprocessing the fiber, and removing impurities on the surface of the glass fiber;
s12, uniformly mixing 45-55 parts of glass fiber pretreated in S11 and 4-6 parts of dopamine hydrochloride in a tris (hydroxymethyl) aminomethane solution with the mass concentration of 1.0-1.5g/L at the pH value of 8-9 and the temperature of 20-30 ℃, filtering, washing with water, and freeze-drying to obtain 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 trimethylol aminomethane solution with the mass concentration of 1.0-1.5g/L for 5-6 hours at the pH=8-9 and the temperature of 20-30 ℃, and washing and drying to obtain 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 self-assembly and covalent polymerization under the alkaline condition, so that the nano boron nitride with excellent insulation effect is uniformly adsorbed on the surface of the dopamine surface treatment fiber under the intermolecular acting force, and the heat resistance and the insulation performance of the nano boron nitride are improved; in addition, a polydopamine layer is deposited on the surface of the nanometer boron nitride in the step S14 under the alkaline condition, so that catechol groups on the surface of the dopamine modified glass fiber and catechol groups deposited on the surface of the boron nitride can form hydrogen bonds with epoxy resin, and the stability of connection between the nanometer boron nitride composite glass fiber and the epoxy resin is improved, thereby comprehensively improving the mechanical property, the high temperature resistance and the insulating property of the application.
Preferably, the preparation of the tris (hydroxymethyl) aminomethane solution in the steps S12 and S13 specifically comprises: mixing and stirring 11-13 parts of tris (hydroxymethyl) aminomethane in 9500-1000 parts of deionized water uniformly, and then adding 0.8-1.2mol/L hydrochloric acid solution to adjust the pH to 8-9, wherein the tris (hydroxymethyl) aminomethane solution.
By adopting the technical scheme, the pH value of the tris (hydroxymethyl) aminomethane solution is limited by the preparation of the tris (hydroxymethyl) aminomethane solution, so that on one hand, the accuracy of regulating the pH value when dopamine is deposited on the surfaces of glass fibers and nano boron nitride is improved, the effect of dopamine deposition is improved, the nano boron nitride is more uniformly dispersed on the surfaces of the glass fibers, and the convenience of the preparation, 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 methacryloxypropyl trimethoxy silane with 300-500 parts of ethanol solution with the purity of 95% uniformly to obtain a mixed solution A;
s22, uniformly mixing and stirring 51-55 parts of hexagonal boron nitride micro powder and 28-32 parts of nanometer glass micro powder to obtain a mixed solid A, and uniformly mixing and stirring 28-32 parts of nanometer aluminum oxide and 63-68 parts of zinc oxide whiskers to obtain a mixed solid B;
s23, dispersing the mixed solution A and the mixed solid A at 55-65 ℃ for 1.5-2 hours by ultrasonic, adding the mixed solid B for 1.2-1.8 hours by ultrasonic dispersion, 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 35-45 parts of nano boron nitride composite glass fiber and the mixture C uniformly to obtain the modified heat conduction filler.
By adopting the technical scheme, the application limits the dosage of different heat conducting fillers, and respectively mixes the heat conducting fillers with different crystal forms and sizes, thereby reducing the possibility of agglomeration of nanometer glass micropowder and nanometer alumina.
In a second aspect, the application provides a preparation method of an ultra-long high temperature resistant mica tape, which adopts the following technical scheme:
a preparation method of an ultra-long high temperature resistant mica tape comprises the following steps:
s1, preprocessing 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 one side of the synthetic mica paper coated with benzoyl peroxide, and shaping for 2-5min at 75-85 ℃;
s3, carrying out impurity removal treatment on the surface of alkali-free glass fiber cloth, compositing the alkali-free glass fiber cloth on one side of the synthetic mica paper coated with the first adhesive to obtain a composite layer A, turning the composite layer A by 180 degrees to enable glass in the composite layer A to be arranged below the synthetic mica paper, uniformly spraying the second adhesive on one side of the synthetic mica paper which is not coated with benzoyl peroxide, baking at 145-155 ℃ for 5-10min, and cutting and rolling to obtain the product.
According to the technical scheme, the first adhesive and the second adhesive are compounded on the surface of the synthetic mica paper in a spraying manner, so that the use amount of the adhesive can be reduced, gaps can be formed between the glass cloth and the surface of the mica paper on the one hand, the air permeability of the synthetic mica paper is improved, the impregnation resin is facilitated to be impregnated in the subsequent vacuum pressure impregnation process, the first adhesive coated on the surface of the synthetic mica paper is subjected to semi-curing treatment, a gap structure is formed between the glass cloth and the mica paper, the air permeability of a product is further improved, and in addition, after the benzoyl peroxide is coated on the upper surface and the lower surface of the synthetic mica paper, the connection strength between the first adhesive and the second adhesive and the synthetic mica paper is improved, so that the overall structural stability of the synthetic mica paper is comprehensively improved.
In summary, the application has the following beneficial effects:
1. the application adopts the structure that 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 alkali-free glass fiber cloth forms a plurality of pore structures among the synthetic mica paper, the ventilation performance of the application is improved, the impregnating resin is facilitated to soak the mica tape, in addition, the biphenyl type epoxy resin has excellent electrical performance and heat resistance, the free volume in the first adhesive can be reduced, the filling quantity of the heat conducting filler is improved, and the heat resistance and the insulation performance of the application are comprehensively improved;
2. according to the method disclosed by the application, the first adhesive and the second adhesive are compounded on the surface of the synthetic mica paper in a spraying manner, so that the use amount of the adhesive can be reduced on one hand, and gaps can be formed on the surfaces of the glass cloth and the mica paper on the other hand, the air permeability of the synthetic mica paper is improved, and the impregnating resin is facilitated to be impregnated in the subsequent vacuum pressure impregnation process.
Detailed Description
The present application will be described in further detail with reference to examples and examples.
Raw materials
TABLE 1 Table of sources of raw materials used in the 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 a rotating speed of 150rpm for 15min to obtain a solution A with uniform texture, and adjusting the pH=8.5 of the solution A by 1mol/L of hydrochloric acid solution to obtain the tris (hydroxymethyl) aminomethane solution;
s12, preprocessing the fiber, namely heating 50g of glass fiber in a baking oven at 25 ℃, heating to 600 ℃ at a speed of 10 ℃/min, preserving heat for 1 hour, cleaning the fiber with deionized water for 3 times, performing ultrasonic dispersion (28 KHz, 1000W) in an ultrasonic oscillator for 20 minutes, and drying at 65 ℃ for 20 minutes to obtain preprocessed glass fiber;
s13, sequentially adding 5L of the tris (hydroxymethyl) aminomethane solution prepared in S11, 50g of the pretreated glass fiber prepared in S12 and 5.35g of dopamine hydrochloride into a reaction kettle, mixing and stirring at 25 ℃ for 25 hours at a rotating speed of 100rpm, filtering the glass fiber, washing the glass fiber with deionized water for 3 times, and freeze-drying the glass fiber by a freeze dryer (SCIENTZ-25T freeze dryer sold by Ningbo novel Zhi freeze dryer Co., ltd.) for 10 minutes to obtain the dopamine modified glass fiber;
s14, mixing and stirring 4.5L of the tris (hydroxymethyl) aminomethane 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-collecting magnetic stirrer sold by Shanghai Ling Ke Utility development Co., ltd.) at room temperature and a rotating speed of 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 preparation differs from preparation 1 in that the step S12 is not performed in this preparation.
Preparation example 3
The present preparation example differs from preparation example 1 in that step S13 is not performed in the present preparation example, and the pretreated glass fiber obtained in step S12 is directly used in step S14.
Preparation example 4
The present preparation example differs from preparation example 1 in that the present preparation example replaces dopamine hydrochloride with deionized water of equal mass in step S13.
Preparation example 5
The modified heat-conducting filler is prepared by the following steps:
s21, mixing and stirring 4g of methacryloxypropyl trimethoxy silane and 500mL of ethanol solution with the purity of 95% in a reaction kettle at a rotating speed of 1000rpm uniformly 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 a rotating speed of 500rpm for 20min to obtain a mixed solid A, and mixing and stirring 30g of nano aluminum oxide and 66g of zinc oxide whisker in the reaction kettle at a rotating speed of 500rpm for 20min to obtain a mixed solid B;
s23, ultrasonically dispersing (28 KHz, 1000W) the mixed solid A prepared in the mixed liquid 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.) for 1.8 hours, continuously adding the mixed solid B into the ultrasonic oscillator for ultrasonic dispersion (28 KHz, 1000W) for 1.5 hours to obtain a mixture C, transferring the mixture C into a reaction kettle, mixing and stirring for 50 minutes at a rotating speed of 200rpm, adding 100mL of deionized water into the reaction kettle at a speed of 0.5mL/min in the continuous stirring process of the mixture C, heating to 80 ℃ (79-82 ℃), vacuum refluxing to remove ethanol and other small molecular substances, and finally vacuumizing and drying for 20 minutes at 60 ℃ 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 a rotation speed of 200rpm for 20min to obtain the modified heat-conducting filler.
Preparation example 6
This preparation differs from preparation 5 in that this preparation replaces methacryloxypropyl trimethoxysilane with an equal mass of gamma-glycidoxypropyl trimethoxysilane in step S21.
Preparation example 7
The present preparation example differs from preparation example 5 in that no nano-glass fine powder was used in step S22.
Preparation example 8
This preparation differs from preparation 5 in that hexagonal boron nitride fine powder is not used in step S22.
Preparation example 9
This preparation differs from preparation 5 in that the preparation does not employ nano alumina in step S22.
Preparation example 10
This preparation differs from preparation 5 in that no zinc oxide whisker was used in step S22.
PREPARATION EXAMPLE 11
The present preparation example differs from preparation example 5 in that step S23 of the present preparation example specifically includes: the mixed solid A and the mixed solid B prepared in the mixed liquid A, S prepared in the step S21 are ultrasonically dispersed (28 KHz, 1000W) for 3.3 hours in an ultrasonic oscillator (an ultrasonic stirring tank sold by Hangzhou vibration source ultrasonic equipment Co., ltd.) to obtain a mixture C, the mixture C is transferred into a reaction kettle to be mixed and stirred for 50 minutes at a rotating speed of 200rpm, 100mL of deionized water is added into the reaction kettle at a speed of 0.5mL/min in the continuous stirring process of the mixture C, the mixture C is heated to 80 ℃ (79-82 ℃), ethanol and other small molecular substances are removed by vacuum reflux, and finally the mixture D is obtained after the mixture C is vacuumized and dried for 20 minutes at 60 ℃.
Preparation example 12
The modified heat-conducting filler in the preparation example is prepared by the following steps:
s21, mixing and stirring 4g of methacryloxypropyl trimethoxy silane and 500mL of ethanol solution with the purity of 95% in a reaction kettle at a rotating speed of 1000rpm uniformly to obtain a mixed solution A;
s22, mixing 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 a rotating speed of 500rpm for 40min to obtain a mixed solid a;
s23, ultrasonically dispersing (28 KHz, 1000W) the mixed solid a prepared in the mixed liquid 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.) for 3.3 hours to obtain a mixture b, transferring the mixture b into a reaction kettle, mixing and stirring for 50 minutes at a rotating speed of 200rpm, adding 100mL of deionized water into the reaction kettle at a speed of 0.5mL/min in the continuous stirring process of the mixture b, heating to 80 ℃ (79-82 ℃), vacuum refluxing to remove ethanol and other small molecular substances, and finally vacuumizing and drying for 20 minutes at 60 ℃ 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 a rotation speed of 200rpm for 20min to obtain the modified heat-conducting filler.
Preparation example 13
The present preparation example is different from preparation example 5 in that the present preparation example replaces the nano boron nitride composite glass fiber prepared in preparation example 1 with the nano boron nitride composite glass fiber prepared in preparation example 2 of equal mass in S24.
PREPARATION EXAMPLE 14
The present preparation example is different from preparation example 5 in that the present preparation example replaces the nano boron nitride composite glass fiber prepared in preparation example 1 with the nano boron nitride composite glass fiber prepared in preparation example 3 of equal mass in S24.
Preparation example 15
The present preparation example is different from preparation example 5 in that the present preparation example replaces the nano boron nitride composite glass fiber prepared in preparation example 1 with the nano boron nitride composite glass fiber prepared in preparation example 4 of equal mass in S24.
PREPARATION EXAMPLE 16
The present preparation example is different from preparation example 5 in that the present preparation example replaces the nano boron nitride composite glass fiber prepared in preparation example 1 with glass fiber of equal mass in S24.
Preparation example 17
The preparation of the first adhesive specifically comprises the following steps: the modified heat-conducting filler and biphenyl type epoxy resin prepared in preparation example 5 are prepared according to the mass ratio of 21:16, mixing at a rotation speed of 250rpm, stirring for 45min, 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 smaller than 100 meshes, wherein the temperature of a feeding section of the double-screw extruder is 130 ℃, the temperature of a melting section is 150 ℃ and the temperature of a die is 150 ℃, and the screw rotation speed of the extruder is 180r/min.
PREPARATION EXAMPLE 18
The present preparation example differs from preparation example 17 in that the mass ratio of the modified heat conductive filler and the biphenyl epoxy resin in the present preparation example is 21:15.
Preparation example 19
The present preparation example differs from preparation example 17 in that the mass ratio of the modified heat conductive filler and the biphenyl epoxy resin in the present preparation example is 21:17.
Preparation example 20
The difference between this preparation example and preparation example 17 is that the mass ratio of the modified heat conductive filler and the biphenyl epoxy resin in this preparation example is 21:12.
Preparation example 21
The present preparation example differs from preparation example 17 in that the mass ratio of the modified heat conductive filler and the biphenyl epoxy resin in the present preparation example is 21:20.
PREPARATION EXAMPLE 22
This preparation differs from preparation 17 in that the biphenyl type epoxy resin is replaced with bisphenol A epoxy resin of equal mass in this preparation.
Preparation example 23
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 6 of equal mass.
PREPARATION EXAMPLE 24
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 7 of equal mass.
Preparation example 25
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 8 of equal mass.
PREPARATION EXAMPLE 26
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 9 of equal mass.
Preparation example 27
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 10 of equal mass.
PREPARATION EXAMPLE 28
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 11 of equal mass.
Preparation example 29
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 12 of equal mass.
Preparation example 30
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 13 of equal mass.
Preparation example 31
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 14 of equal mass.
PREPARATION EXAMPLE 32
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 15 of equal mass.
PREPARATION EXAMPLE 33
This preparation differs from preparation 17 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 16 of equal mass.
PREPARATION EXAMPLE 34
The second adhesive is prepared by the following steps:
s31, preparing composite epoxy resin, namely adding bisphenol S epoxy resin and bisphenol A epoxy resin into a reaction according to a mass ratio of 12:4, and mixing and stirring for 40 minutes at a rotating speed of 200rpm to obtain composite epoxy resin;
s32, mixing the composite epoxy resin prepared in the step S31 with the modified heat-conducting filler prepared in the preparation example 5 according to the mass ratio of 6:2 are mixed and stirred uniformly in a reaction kettle at a rotating speed of 1000rpm to obtain a mixed material with a mass of 65g, 6.5g of 4,4' -diaminodiphenyl sulfone and 6.5g of p-phenylenediamine are mixed and stirred uniformly at 185 ℃ and cooled to 55 ℃, and then the mixed material, 0.3g of N, N-dimethylbenzylamine and 500ml of toluene solution are mixed and stirred for 1h at a rotating speed of 100rpm to obtain a second binder.
Preparation example 35
This preparation differs from preparation 34 in that this preparation replaces bisphenol S epoxy resin with bisphenol A epoxy resin of equal mass in step S31.
Preparation example 36
This preparation differs from preparation 34 in that this preparation replaces 4,4' -diaminodiphenyl sulfone with an equal mass of p-phenylenediamine in step S32.
Preparation example 37
The difference between the preparation example and the preparation example 34 is that the mass ratio of the composite epoxy resin to the modified heat conductive filler in the step S32 is 6:1.
preparation example 38
The difference between the preparation example and the preparation example 34 is that the mass ratio of the composite epoxy resin to the modified heat conductive filler in the step S32 is 6:3.
preparation example 39
The preparation example is different from the preparation example 34 in that the mass ratio of the composite epoxy resin to the modified heat conductive filler in the step S32 is 8:1.
preparation example 40
The difference between the preparation example and the preparation example 34 is that the mass ratio of the composite epoxy resin to the modified heat conductive filler in the step S32 is 6:4.
PREPARATION EXAMPLE 41
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 6 of equal mass.
PREPARATION EXAMPLE 42
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 7 of equal mass.
Preparation example 43
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 8 of equal mass.
PREPARATION EXAMPLE 44
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 9 of equal mass.
PREPARATION EXAMPLE 45
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 10 of equal mass.
Preparation example 46
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 11 of equal mass.
Preparation example 47
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 12 of equal mass.
Preparation example 48
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 13 of equal mass.
Preparation example 49
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 14 of equal mass.
PREPARATION EXAMPLE 50
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 15 of equal mass.
PREPARATION EXAMPLE 51
This preparation differs from preparation 34 in that the modified heat conductive filler prepared in preparation 5 is replaced with the modified heat conductive filler prepared in preparation 16 of equal mass.
Examples
Example 1
The ultra-long high temperature resistant mica tape is prepared by the following steps:
s1, preprocessing synthetic mica paper, uniformly coating a layer of benzoyl peroxide on the upper surface of the synthetic mica paper by a coating machine, and standing for 5min;
s2, semi-curing of a first adhesive, namely uniformly spraying the first adhesive prepared in the preparation example 17 in a powder state on one side of synthetic mica paper coated with benzoyl peroxide through a spraying device (a five-axis numerical control automatic spraying machine sold by Shenzhen Kazakhstan robot Automation Equipment Co., ltd.), 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 by absolute ethyl 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, compositing one side of the alkali-free glass fiber cloth, which is wiped by the absolute ethyl alcohol, on one side of the synthetic mica paper coated with a first adhesive to obtain a composite layer A, turning the composite layer A180 degrees, enabling glass in the composite layer A to be arranged below the synthetic mica paper, uniformly spraying a second adhesive prepared in a powder state on one side of the synthetic mica paper which is not coated with benzoyl peroxide through a spraying device (five-axis numerical control automatic spraying machine sold by Asahi robot equipment Co., ltd., shenzhi, and then placing the composite layer A in an oven to bake for 7min at 150 ℃, and cutting and reeling to obtain a product.
Example 2
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 18 of equal mass.
Example 3
This example differs from example 1 in that the first adhesive of preparation 17 is replaced by the first adhesive of preparation 19 of equal mass.
Example 4
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 23 of equal mass.
Example 5
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 24 of equal mass.
Example 6
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 25 of equal mass.
Example 7
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 26 of equal mass.
Example 8
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 27 of equal mass.
Example 9
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 28 of equal mass.
Example 10
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 29 of equal mass.
Example 11
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 30 of equal mass.
Example 12
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 31 of equal mass.
Example 13
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 32 of equal mass.
Example 14
This example differs from example 1 in that the first adhesive of preparation 17 is replaced with the first adhesive of preparation 33 of equal mass.
Example 15
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 35 of equal mass.
Example 16
This example differs from example 1 in that the second adhesive of preparation 34 was replaced with the second adhesive of preparation 36 of equal mass.
Example 17
This example differs from example 1 in that the second adhesive of preparation 34 was replaced with the second adhesive of preparation 37 of equal mass.
Example 18
This example differs from example 1 in that the second adhesive of preparation 34 is replaced with the second adhesive of preparation 38 of equal mass.
Example 19
This example differs from example 1 in that the second adhesive of preparation 34 is replaced with the second adhesive of preparation 39 of equal mass.
Example 20
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 40 of equal mass.
Example 21
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 41 of equal mass.
Example 22
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 42 of equal mass.
Example 23
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 43 of equal mass.
Example 24
This example differs from example 1 in that the second adhesive of preparation 34 is replaced with the second adhesive of preparation 44 of equal mass.
Example 25
This example differs from example 1 in that the second adhesive of preparation 34 is replaced with the second adhesive of preparation 45 of equal mass.
Example 26
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 46 of equal mass.
Example 27
This example differs from example 1 in that the second adhesive of preparation 34 is replaced with the second adhesive of preparation 47 of equal mass.
Example 28
This example differs from example 1 in that the second adhesive of preparation 34 is replaced with the second adhesive of preparation 48 of equal mass.
Example 29
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 49 of equal mass.
Example 30
This example differs from example 1 in that the second adhesive of preparation 34 is replaced with the second adhesive of preparation 50 of equal mass.
Example 31
This example differs from example 1 in that the second adhesive of preparation example 34 was replaced with the second adhesive of preparation example 51 of equal mass.
Comparative example
Comparative example 1
The ultra-long high temperature resistant mica tape is prepared by the following steps:
s1, preprocessing synthetic mica paper, uniformly coating a layer of benzoyl peroxide on the upper surface of the synthetic mica paper by a coating machine, and standing for 5min;
s2, semi-curing the first adhesive, coating the first adhesive on one side of the synthetic mica paper coated with benzoyl peroxide through a coating machine after the first adhesive is melted, 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 by absolute ethyl alcohol, after the alcohol naturally volatilizes, keeping the alkali-free glass fiber cloth in a horizontal state on a coating machine by a unreeling shaft, a compression roller and a reeling shaft, compositing one side of the alkali-free glass fiber cloth, which is wiped by the absolute ethyl alcohol, on one side of the synthetic mica paper coated with a first adhesive to obtain a composite layer A, turning the composite layer A by 180 degrees, enabling glass in the composite layer A to be arranged below the synthetic mica paper, melting a powdery second adhesive, uniformly coating the melted glass on one side of the synthetic mica paper, which is not coated with benzoyl peroxide, by the coating machine, then placing the melted glass in an oven, baking at 150 ℃ for 7min, and cutting and reeling to obtain the product.
Comparative example 2
This ratio differs from example 1 in that the first adhesive from preparation 17 is replaced by the same mass of the first adhesive from preparation 20.
Comparative example 3
This ratio differs from example 1 in that the first adhesive from preparation 17 is replaced by the same mass of the first adhesive from preparation 21.
Comparative example 4
This ratio differs from example 1 in that the first adhesive from preparation 17 is replaced by the first adhesive from preparation 22 of equal mass.
Performance test
Detection method/test method
1. Air permeability (s/100 mL): reference is made to GB/T5019.12-2017 section 12 of mica-based insulation: the mica tapes prepared in examples 1-32 and comparative examples 1-2 were tested for air permeability in high air permeability glass cloth reinforced epoxy few-glue mica tape.
Thermal state loss (%) at 2.180 ℃: the mica tapes prepared in examples 1 to 32 and comparative examples 1 to 2 were examined for thermal losses at 180℃with reference to the detection method of IEC 60243-1.
3. Tensile strength (N/10 mm): reference is made to GB/T5019.12-2017 section 12 of mica-based insulation: the test of tensile strength was carried out on the mica tapes prepared in examples 1 to 32 and comparative examples 1 to 2 by the method of high air permeability glass cloth reinforced epoxy few-glue mica tape.
4. Electrical strength (MV/m): reference is made to GB/T5019.12-2017 section 12 of mica-based insulation: the method of high air permeability glass cloth reinforced epoxy little glue mica tape "carries out air permeability electrical strength on the mica tapes prepared in examples 1-32 and comparative examples 1-2.
TABLE 2 summary of the results of the measurements of examples 1-32 and comparative examples 1-2
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As can be seen from the combination of examples 1-3, comparative examples 2-4 and table 2, the modified heat conductive filler and the biphenyl type epoxy resin were in mass ratio of 21:15-17, the air permeability, the thermal state loss at 155 ℃ of the application, the tensile strength and the electrical strength can be comprehensively improved, and the mass ratio of the modified heat conducting filler to the biphenyl type epoxy resin is 21: at 16, the performance of the product is optimal.
It can be seen from the combination of examples 1, 4-10 and 21-27 and the combination of table 2 that the ventilation property, thermal loss at 155 ℃ and tensile strength and electrical strength of the product can be comprehensively improved after the nano glass micro powder, hexagonal boron nitride micro powder, nano aluminum oxide, zinc oxide whisker and nano boron nitride composite glass fiber are compounded.
It can be seen from the combination of examples 1 and 15-20 and the combination of Table 2 that the combination of bisphenol A epoxy resin and bisphenol S epoxy resin can comprehensively improve the heat resistance of the product, and the combination of p-phenylenediamine and 4,4' -diaminodiphenyl sulfone can also improve the electrical strength and tensile strength of the product.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (3)
1. The ultra-long high temperature resistant mica tape is characterized by comprising alkali-free glass fiber cloth, a first adhesive layer, synthetic mica paper and a second adhesive layer which are sequentially compounded; 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 epoxy resin and heat conducting filler, and the mass ratio of the heat conducting filler to the biphenyl epoxy resin is 21:15-17;
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;
the heat conducting filler used in the first adhesive and the second adhesive is modified heat conducting filler, and the modified heat conducting filler is prepared from the following raw materials: methacryloxypropyl trimethoxysilane, hexagonal boron nitride micro powder, nanometer glass micro powder, nanometer aluminum oxide, zinc oxide whisker and nanometer boron nitride composite glass fiber;
the epoxy resin in the second adhesive is composite epoxy resin, and the composite epoxy resin is prepared from the following raw materials: bisphenol S epoxy resin and bisphenol A epoxy resin, and the mass ratio of the bisphenol S epoxy resin to the bisphenol A epoxy resin is 12:3-5;
the second adhesive is prepared by the following steps:
s31, preparing composite epoxy resin;
s32, mixing the composite epoxy resin prepared in the step S31 with a heat-conducting filler according to a mass ratio of 6: mixing and stirring uniformly the mixture in the proportion of (1-3) to obtain a mixed material, mixing and stirring uniformly 4,4' -diaminodiphenyl sulfone and p-phenylenediamine at 180-188 ℃, cooling to 50-60 ℃, and mixing and stirring uniformly the mixed material and N, N-dimethylbenzylamine in a toluene solution to obtain a second binder;
the nano boron nitride composite glass fiber is prepared by the following steps:
s11, preprocessing the fiber, and removing impurities on the surface of the glass fiber;
s12, uniformly mixing 45-55 parts of glass fiber pretreated in S11 and 4-6 parts of dopamine hydrochloride in a tris (hydroxymethyl) aminomethane solution with the mass concentration of 1.0-1.5g/L at the pH value of 8-9 and the temperature of 20-30 ℃, filtering, washing with water, and freeze-drying to obtain 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 tris (hydroxymethyl) aminomethane solution with the mass concentration of 1.0-1.5g/L for 5-6 hours at the pH=8-9 and the temperature of 20-30 ℃, and washing and drying to obtain nano boron nitride composite glass fiber;
the modified heat-conducting filler is prepared by the following steps:
s21, mixing and stirring 2-4 parts of methacryloxypropyl trimethoxy silane with 300-500 parts of ethanol solution with the purity of 95% uniformly to obtain a mixed solution A;
s22, uniformly mixing and stirring 51-55 parts of hexagonal boron nitride micro powder and 28-32 parts of nanometer glass micro powder to obtain a mixed solid A, and uniformly mixing and stirring 28-32 parts of nanometer aluminum oxide and 63-68 parts of zinc oxide whiskers to obtain a mixed solid B;
s23, dispersing the mixed solution A and the mixed solid A at 55-65 ℃ for 1.5-2 hours by ultrasonic, adding the mixed solid B for 1.2-1.8 hours by ultrasonic dispersion, 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 35-45 parts of nano boron nitride composite glass fiber and the mixture D uniformly to obtain the modified heat conduction filler.
2. An ultralong high temperature resistant mica tape as recited in claim 1, wherein: the preparation of the tris (hydroxymethyl) aminomethane solution in the step S12 and the step S13 specifically comprises the following steps: mixing and stirring 11-13 parts of tris (hydroxymethyl) aminomethane in 9500-1000 parts of deionized water uniformly, and then adding 0.8-1.2mol/L hydrochloric acid solution to adjust the pH to 8-9, wherein the tris (hydroxymethyl) aminomethane solution.
3. The method for preparing the ultra-long high temperature resistant mica tape according to any one of claims 1 to 2, which is characterized by comprising the following steps:
s1, preprocessing 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 one side of the synthetic mica paper coated with benzoyl peroxide, and shaping for 2-5min at 75-85 ℃;
s3, carrying out impurity removal treatment on the surface of alkali-free glass fiber cloth, compositing the alkali-free glass fiber cloth on one side of the synthetic mica paper coated with the first adhesive to obtain a composite layer A, turning the composite layer A by 180 degrees to enable glass in the composite layer A to be arranged below the synthetic mica paper, uniformly spraying the second adhesive on one side of the synthetic mica paper which is not coated with benzoyl peroxide, baking at 145-155 ℃ for 5-10min, and cutting and rolling to obtain the product.
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