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CN110527427A - Silicon resin component and silicone coatings - Google Patents

Silicon resin component and silicone coatings Download PDF

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CN110527427A
CN110527427A CN201810714853.XA CN201810714853A CN110527427A CN 110527427 A CN110527427 A CN 110527427A CN 201810714853 A CN201810714853 A CN 201810714853A CN 110527427 A CN110527427 A CN 110527427A
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CN110527427B (en
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陈志源
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Thinking Electronic Industrial Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04Polysiloxanes
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres

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Abstract

本发明涉及硅树脂组成物及硅树脂涂层。本发明的硅树脂组成物包括5重量份至20重量份的硅树脂、75重量份至92重量份的填料、1重量份至10重量份的有机溶剂,以及以该硅树脂、该填料和该有机溶剂的总重为100重量份,还包括0.25重量份至2重量份的催化剂,其中,该填料包括一绝缘纤维填料,该绝缘纤维填料选自玻璃纤维(例如,石英玻璃纤维)、金属氧化物纤维(例如,陶瓷纤维)及其组合物。当该硅树脂组成物固化形成硅树脂涂层后,不仅可通过高温储存测试和蒸煮测试,同时也可耐受2500伏特至4000伏特的交流电,且长时间处于高温或在高温蒸煮后的电压变化率界于0.1%至1.5%之间。The invention relates to a silicone resin composition and a silicone resin coating. The silicone resin composition of the present invention includes 5 parts by weight to 20 parts by weight of silicone resin, 75 parts by weight to 92 parts by weight of filler, 1 part by weight to 10 parts by weight of organic solvent, and the silicone resin, the filler and the The total weight of the organic solvent is 100 parts by weight, and also includes 0.25 parts by weight to 2 parts by weight of a catalyst, wherein the filler includes an insulating fiber filler, and the insulating fiber filler is selected from glass fiber (for example, quartz glass fiber), metal oxide Fibers (e.g., ceramic fibers) and compositions thereof. When the silicone resin composition is cured to form a silicone resin coating, it can not only pass the high-temperature storage test and cooking test, but also withstand the alternating current of 2500 volts to 4000 volts, and the voltage change after long-term high temperature or high-temperature cooking The rate ranges from 0.1% to 1.5%.

Description

硅树脂组成物及硅树脂涂层Silicone resin composition and silicone resin coating

技术领域technical field

本发明涉及涂层材料领域,尤指涉及一种硅树脂组成物及硅树脂涂层,硅树脂组成物在固化后的硅树脂涂层具有高绝缘耐压特性、高耐温性能和耐候性能,可用于压敏电阻、热敏电阻或传感器的包封涂层。The invention relates to the field of coating materials, in particular to a silicone resin composition and a silicone resin coating. The silicone resin coating of the silicone resin composition after curing has high insulation and voltage resistance properties, high temperature resistance and weather resistance. Can be used as an encapsulation coating for varistors, thermistors or sensors.

背景技术Background technique

随着科技的进步,电子产品的应用领域快速拓展,对性能的需求也日益提高并逐渐多样化,连带提高了市场对电子零件的品质要求,一般而言,电子零件需具备良好的耐温、耐候以及耐电压特性,以符合一定的安全规范。With the advancement of science and technology, the application fields of electronic products are rapidly expanding, and the demand for performance is also increasing and gradually diversifying, which jointly improves the quality requirements of the market for electronic parts. Weather resistance and voltage resistance characteristics to meet certain safety regulations.

以压敏电阻或热敏电阻的涂层材料而言,目前市面上普遍使用的涂层材料大致可分为硅树脂和环氧树脂二种,其中,硅树脂因主链为硅-氧-硅的直链结构,相比于环氧树脂具有优选的耐温和耐候性能,故目前应用于125℃高温环境的压敏电阻和热敏电阻大多是以硅树脂作为包封涂层的材料;但在绝缘耐压性质方面,硅树脂的表现并不如耐温和耐候性能般优秀,因此,为了满足市场上绝缘耐压性能大于2500VAC的需求(即可承受2500伏特的交流电),仅能通过增加硅树脂涂层的厚度来符合绝缘耐压的特性需求。In terms of coating materials for varistors or thermistors, the coating materials commonly used in the market can be roughly divided into two types: silicone resin and epoxy resin. Among them, silicone resin has a silicon-oxygen-silicon main chain. Compared with epoxy resin, it has better temperature and weather resistance. Therefore, most of the varistors and thermistors currently used in 125°C high temperature environment use silicone resin as the encapsulation coating material; but in In terms of insulation and voltage resistance properties, the performance of silicone resin is not as good as its temperature and weather resistance. Therefore, in order to meet the market's demand for insulation and voltage resistance greater than 2500VAC (that is, it can withstand 2500 volts of alternating current), only by adding silicone resin coating The thickness of the layer meets the characteristic requirements of insulation withstand voltage.

故,就目前的技术发展而言,尚未有一可满足市场需求兼具良好耐温性、耐候性和绝缘耐压性的涂层材料。Therefore, as far as the current technological development is concerned, there is no coating material that can meet the market demand and has good temperature resistance, weather resistance and insulation voltage resistance.

发明内容Contents of the invention

有鉴于上述问题,本发明的目的为提供一种硅树脂组成物,其兼具良好的耐温性、耐候性和绝缘耐压性,而可应用于电子零件的包封涂层。In view of the above problems, the purpose of the present invention is to provide a silicone resin composition, which has good temperature resistance, weather resistance and insulation voltage resistance, and can be applied to the encapsulation coating of electronic components.

为达上述目的,本发明的硅树脂组成物包括一5重量份至20重量份的硅树脂、一75重量份至92重量份的填料、一1重量份至10重量份的有机溶剂;以及以该硅树脂、该填料和该有机溶剂的总重为100重量份,还包括0.25重量份至2重量份的催化剂;该填料包括一绝缘纤维填料,该绝缘纤维填料选自玻璃纤维(例如,石英玻璃纤维)、金属氧化物纤维(例如,陶瓷纤维,可选用的陶瓷纤维例如氧化铝纤维)及其组合物。In order to achieve the above object, the silicone resin composition of the present invention comprises a silicone resin of 5 to 20 parts by weight, a filler of 75 to 92 parts by weight, an organic solvent of 1 to 10 parts by weight; and The total weight of the silicone resin, the filler and the organic solvent is 100 parts by weight, and also includes a catalyst of 0.25 parts by weight to 2 parts by weight; the filler includes an insulating fiber filler, and the insulating fiber filler is selected from glass fibers (for example, quartz glass fibers), metal oxide fibers (eg, ceramic fibers, optionally ceramic fibers such as alumina fibers), and combinations thereof.

根据上述技术手段,本发明的硅树脂组成物固化后的涂层具有高绝缘耐压性以及良好的耐温性和耐候性;当涂层厚度为0.7毫米至0.9毫米时可承受2500伏特伏特至4000伏特的交流电,具体来说可耐受3000伏特至4000伏特的交流电;且无论是长时间处于高温或是处于高温蒸煮的状态下,其电压的变化率皆小于10%,符合市面上的需求,实际测量的电压变化率界于0.10%和1.50%之间。According to the above-mentioned technical means, the cured coating of the silicone resin composition of the present invention has high insulation voltage resistance and good temperature resistance and weather resistance; when the coating thickness is 0.7 mm to 0.9 mm, it can withstand 2500 volts to 4000 volts of alternating current, specifically, it can withstand 3000 volts to 4000 volts of alternating current; and whether it is under high temperature for a long time or under high temperature cooking, the change rate of its voltage is less than 10%, which meets the needs of the market , the actual measured voltage change rate is between 0.10% and 1.50%.

优选的,该硅树脂选自甲基硅树脂、甲基苯基硅树脂、乙烯基硅树脂、甲基乙烯基硅树脂、氨基硅树脂、环氧改性硅树脂(又称环氧硅树脂)及其组合物。Preferably, the silicone resin is selected from methyl silicone resin, methylphenyl silicone resin, vinyl silicone resin, methyl vinyl silicone resin, amino silicone resin, epoxy modified silicone resin (also known as epoxy silicone resin) and its composition.

优选的,该绝缘纤维填料的直径为5微米至15微米、长度为100微米至500微米。Preferably, the insulating fiber filler has a diameter of 5 microns to 15 microns and a length of 100 microns to 500 microns.

优选的,该填料包括一改性填料,该改性填料选自滑石粉、石英粉、云母粉、碳酸钙、石墨及其组合物。Preferably, the filler includes a modified filler selected from talc powder, quartz powder, mica powder, calcium carbonate, graphite and combinations thereof.

该催化剂具有加速反应作用。具体来说,前述催化剂为有机金属盐或胺类,该有机金属盐可以包含有铅、锡、锌或铝。The catalyst has the effect of accelerating the reaction. Specifically, the aforementioned catalysts are organometallic salts or amines, and the organometallic salts may contain lead, tin, zinc or aluminum.

优选的,该有机溶剂为甲苯、二甲苯、异丙醇或其组合物。Preferably, the organic solvent is toluene, xylene, isopropanol or a combination thereof.

本发明的硅树脂涂层是由前述硅树脂组成物固化而成,固化方式可以是常温固化或加热固化,优选为加热固化。The silicone resin coating of the present invention is formed by curing the aforementioned silicone resin composition, and the curing method can be room temperature curing or heating curing, preferably heating curing.

具体而言,本发明的硅树脂涂层包括5重量份至20重量份的硅树脂和75重量份至92重量份的填料;原存在于硅树脂组成物的有机溶剂可在固化过程中逐渐挥发,致使所制得的硅树脂涂层中能实质上不含有机溶剂。Specifically, the silicone resin coating of the present invention includes 5 parts by weight to 20 parts by weight of silicone resin and 75 parts by weight to 92 parts by weight of filler; the organic solvent originally present in the silicone resin composition can gradually volatilize during the curing process , so that the obtained silicone resin coating can be substantially free of organic solvents.

优选的,厚度为0.7毫米至0.9毫米的硅树脂涂层具有可承受2500伏特至4000伏特的交流电的特性。Preferably, the silicone resin coating with a thickness of 0.7 mm to 0.9 mm has the property of withstanding 2500 volts to 4000 volts of alternating current.

具体实施方式Detailed ways

实施例1至6:硅树脂组成物Examples 1 to 6: Silicone resin compositions

实施例1至6的硅树脂组成物中包括了硅树脂、填料、有机溶剂和催化剂的重量份如表1所示。Table 1 shows the weight parts of silicone resin, filler, organic solvent and catalyst included in the silicone resin compositions of Examples 1 to 6.

填料的部分包括了绝缘纤维填料和改性填料,在操作时,先齐备绝缘纤维填料和改性填料,其中绝缘纤维填料选用相同重量比例的玻璃纤维(商品名:EMG13-70C)和石英玻璃纤维(商品名:QCF-03-A/C),绝缘纤维填料的直径为5微米至15微米、长度为100微米至500微米;改性填料选用石英粉、滑石粉和云母粉,改性填料的添加可用以使硅树脂组成物具备特定的性质,例如石英粉末可用以调控热膨胀系数,滑石粉可用以调控耐磨性,云母粉可用以调控冷热耐冲击性。The filler part includes insulating fiber filler and modified filler. During operation, the insulating fiber filler and modified filler are prepared first, and the insulating fiber filler is made of glass fiber (trade name: EMG13-70C) and quartz glass fiber in the same weight ratio. (trade name: QCF-03-A/C), the diameter of the insulating fiber filler is 5 microns to 15 microns, and the length is 100 microns to 500 microns; the modified filler is made of quartz powder, talc powder and mica powder, and the modified filler Addition can be used to make the silicone resin composition have specific properties. For example, quartz powder can be used to adjust the thermal expansion coefficient, talc powder can be used to adjust wear resistance, and mica powder can be used to adjust cold and heat impact resistance.

接着,依据表1中的重量比例将甲基硅树脂、乙烯基硅树脂或甲基乙烯基硅树脂的硅树脂添加于有机溶剂中,再将溶有硅树脂的有机溶剂与填料混合均匀,即为硅树脂组成物,并以硅树脂、填料和有机溶剂的总重为100重量份加入为0.25重量份至2重量份的含铝有机金属盐(商品名:朋诺K-7064)作为催化剂。Next, according to the weight ratio in Table 1, the silicone resin of methyl silicone resin, vinyl silicone resin or methyl vinyl silicone resin is added to the organic solvent, and then the organic solvent dissolved in silicone resin and the filler are mixed evenly, that is It is a silicone resin composition, and 0.25 to 2 parts by weight of an aluminum-containing organometallic salt (trade name: Pengnuo K-7064) is added as a catalyst with the total weight of the silicone resin, filler and organic solvent being 100 parts by weight.

比较例1和2:硅树脂组成物Comparative Examples 1 and 2: Silicone resin compositions

比较例1和2的硅树脂组成物是以与实施例1至6的硅树脂组成物相似的方式混合制成,其中包括了硅树脂、填料、有机溶剂和催化剂,各成分的重量份请参照表1所示;比较例和实施例的差异在于:比较例1和2的硅树脂组成物中不包含绝缘纤维填料,填料的部分只包含改性填料,而不选用绝缘纤维填料。The silicone resin compositions of Comparative Examples 1 and 2 are prepared by mixing in a similar manner to the silicone resin compositions of Examples 1 to 6, which include silicone resin, fillers, organic solvents and catalysts. For the parts by weight of each component, please refer to As shown in Table 1; the difference between Comparative Examples and Examples is that the silicone resin compositions of Comparative Examples 1 and 2 do not contain insulating fiber fillers, and the filler part only includes modified fillers instead of insulating fiber fillers.

制备例:硅树脂涂层Preparation Example: Silicone Coating

分别将实施例1至6和比较例1和2的硅树脂组成物涂覆于相同规格的压敏电阻(厂牌:兴勤、型号:TVR20821)上,并以150℃加热1.5小时的固化条件固化形成厚度为0.7毫米至0.9毫米的硅树脂涂层,制得压敏电阻样品。Coat the silicone resin compositions of Examples 1 to 6 and Comparative Examples 1 and 2 on varistors of the same specification (brand: Xingqin, model: TVR20821), and heat at 150°C for 1.5 hours for curing Curing to form a silicone resin coating with a thickness of 0.7 mm to 0.9 mm to prepare a piezoresistor sample.

试验例1:绝缘耐压测试Test example 1: insulation withstand voltage test

为了测试实施例1至6与比较例1和2的硅树脂组成物制成的硅树脂涂层的绝缘耐压性能,将前述压敏电阻样品的正负极二端施以2500VAC的电压60秒,若压敏电阻样品未被击穿,则使施加的电压上调100伏特,即,在压敏电阻样品的正负极二端施以2600VAC的电压,并同样持续60秒,再观察压敏电阻样品是否有被击穿,若仍未被击穿,则重复上述步骤直至压敏电阻样品被击穿,并将被击穿时的施加电压记录于表2中,代表各实施例或比较例固化后的硅树脂涂层可承受交流电的电压。In order to test the insulation withstand voltage performance of the silicone resin coatings made of the silicone resin compositions of Examples 1 to 6 and Comparative Examples 1 and 2, a voltage of 2500 VAC was applied to the positive and negative terminals of the aforementioned varistor samples for 60 seconds , if the varistor sample is not broken down, increase the applied voltage by 100 volts, that is, apply a voltage of 2600VAC to the positive and negative terminals of the varistor sample, and continue for 60 seconds, then observe the varistor Whether the sample has been broken down, if it is still not broken down, repeat the above steps until the piezoresistor sample is broken down, and record the applied voltage when broken down in Table 2, which represents the solidification of each embodiment or comparative example The final silicone coating can withstand the voltage of alternating current.

试验例2:耐温测试Test example 2: temperature resistance test

为了测试实施例1至6与比较例1和2的硅树脂组成物制成的硅树脂涂层的耐温性能,分别将各压敏电阻样品长时间处于150℃的温度下储存1000小时,并以伏特计测量前后的电压差,将计算而得的电压变化率列于表2中。In order to test the temperature resistance of the silicone resin coatings made of the silicone resin compositions of Examples 1 to 6 and Comparative Examples 1 and 2, each varistor sample was stored at a temperature of 150°C for 1000 hours for a long time, and Measure the voltage difference before and after with a voltmeter, and list the calculated voltage change rate in Table 2.

试验例3:耐候测试Test Example 3: Weather Resistance Test

另为了测试实施例1至6与比较例1和2的硅树脂组成物制成的硅树脂涂层的耐候性能,分别将各压敏电阻样品长时间处于2大气压、121℃的温度下蒸煮12小时,并以伏特计测量前后的电压差,将计算而得的电压变化率列于表2中。In addition, in order to test the weather resistance of the silicone resin coatings made of the silicone resin compositions of Examples 1 to 6 and Comparative Examples 1 and 2, each varistor sample was boiled for 12 hours at 2 atmospheres and 121°C for a long time. Hours, and measure the voltage difference before and after with a voltmeter, and list the calculated voltage change rate in Table 2.

表2:实施例1至10(E1至E10)和比较例1和2(C1和C2)中硅树脂组成物固化形成的硅树脂涂层的特性测试。Table 2: Characteristic tests of the silicone resin coatings formed by curing the silicone resin compositions in Examples 1 to 10 (E1 to E10) and Comparative Examples 1 and 2 (C1 and C2).

综合表1和表2的结果可得知,本发明的硅树脂组成物中包含有绝缘纤维填料,故形成的硅树脂涂层具有较高的绝缘耐压性质以及良好的耐温和耐候性。Based on the results of Table 1 and Table 2, it can be seen that the silicone resin composition of the present invention contains insulating fiber fillers, so the formed silicone resin coating has high insulation and voltage resistance properties and good temperature and weather resistance.

针对绝缘耐压的部分,本发明的硅树脂涂层不仅达到市面上对包封涂层的绝缘耐压需求(可承受2500伏特的交流电),其可耐受的交流电电压更可高达3000伏特至4000伏特,明显优于比较例1和2的绝缘耐压结果(仅可承受1500伏特的交流电)。For the insulation and withstand voltage part, the silicone resin coating of the present invention not only meets the insulation and withstand voltage requirements of the encapsulation coating on the market (can withstand 2500 volts of alternating current), but its withstandable alternating current voltage can be as high as 3000 volts to 4000 volts, significantly better than the insulation withstand voltage results of Comparative Examples 1 and 2 (only able to withstand 1500 volts of alternating current).

另外,针对耐温性和耐候性的测试,无论是长时间处于高温或于高温蒸煮状态下,本发明的硅树脂涂层的电压变化率符合业界的要求(电压变化率低于10%),实际测量的电压变化率为0.10%和1.50%之间,明显优于业界针对电压变化率的要求。In addition, for the test of temperature resistance and weather resistance, the voltage change rate of the silicone resin coating of the present invention meets the requirements of the industry (voltage change rate is less than 10%), no matter it is at high temperature for a long time or in a high-temperature cooking state. The actual measured voltage change rate is between 0.10% and 1.50%, which is obviously better than the industry's requirements for the voltage change rate.

因此,本发明的硅树脂组成物在添加了绝缘纤维填料之后,具有较高的绝缘耐压性质以及良好的耐温和耐候性;而硅树脂组成物固化形成硅树脂涂层后,其符合业界对绝缘耐压性和电压变化率的要求,且可耐受较高的交流电电压。此外,存在于硅树脂组成物的有机溶剂可在固化过程中逐渐挥发,故利用该硅树脂组成物所制得的硅树脂涂层中能实质上不含有机溶剂。Therefore, the silicone resin composition of the present invention has high insulation and voltage resistance properties and good temperature and weather resistance after adding insulating fiber filler; Insulation withstand voltage and voltage change rate requirements, and can withstand higher AC voltage. In addition, the organic solvent present in the silicone resin composition can gradually volatilize during the curing process, so the silicone resin coating prepared by using the silicone resin composition can substantially contain no organic solvent.

Claims (9)

1. a kind of silicon resin component comprising:
The silicone resin of 5 parts by weight to 20 parts by weight;
The filler of 75 parts by weight to 92 parts by weight comprising an insulating fibrous fillers, the insulating fibrous fillers be selected from glass fibre, Metal-oxide fiber and combinations thereof;
The organic solvent of 1 parts by weight to 10 parts by weight;And
With the gross weight of the silicone resin, the filler and the organic solvent for 100 parts by weight, which further includes 0.25 weight Measure the catalyst of part to 2 parts by weight.
2. silicon resin component according to claim 1, wherein the silicone resin is selected from methyl silicon resin, aminomethyl phenyl silicon tree Rouge, vinyl polysiloxane, methyl vinyl silicone, amino silicone, epoxy-modified silicone resin and combinations thereof.
3. silicon resin component according to claim 1, wherein the diameter of the insulating fibrous fillers is 5 microns to 15 micro- Rice, length are 100 microns to 500 microns.
4. silicon resin component according to claim 1, wherein the glass fibre is quartz glass fibre.
5. silicon resin component according to claim 1, wherein the metal-oxide fiber is ceramic fibre.
6. silicon resin component according to claim 1, wherein the filler includes modified filler, which is selected from Talcum powder, silica flour, mica powder, calcium carbonate, graphite and combinations thereof.
7. silicon resin component according to claim 1, wherein the catalyst is organic metal salt or aminated compounds;Its In the organic solvent be toluene, dimethylbenzene, isopropanol or combinations thereof object.
8. a kind of silicone coatings are that the silicon resin component as described in any one of claims 1 to 7 solidifies.
9. silicone coatings according to claim 8, wherein with a thickness of 0.7 millimeter to the 0.9 millimeter silicone coatings It can bear 2500 volts to 4000 volts of alternating current.
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