WO2021109730A1 - 一种双组份有机硅灌封胶及其应用方法 - Google Patents

一种双组份有机硅灌封胶及其应用方法 Download PDF

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WO2021109730A1
WO2021109730A1 PCT/CN2020/121846 CN2020121846W WO2021109730A1 WO 2021109730 A1 WO2021109730 A1 WO 2021109730A1 CN 2020121846 W CN2020121846 W CN 2020121846W WO 2021109730 A1 WO2021109730 A1 WO 2021109730A1
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component
siloxane
conductive material
silicone
resin
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PCT/CN2020/121846
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English (en)
French (fr)
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井丰喜
吴斌
潘德忠
顾健峰
徐庆华
张春琪
夏智峰
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苏州太湖电工新材料股份有限公司
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Publication of WO2021109730A1 publication Critical patent/WO2021109730A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • the invention belongs to the technical field of insulating materials, and specifically relates to a two-component silicone potting glue and an application method thereof. It is mainly used for potting the ends of the stator channel steel of a wind generator, and is also suitable for high-power electronic components, Potting protection for module power supplies and circuit boards that require high heat dissipation and temperature resistance.
  • Potting can impart integrity to motors and electronic devices, so that internal components and circuits have good resistance to external shocks and vibrations, avoid direct exposure of internal components and circuits, and improve the waterproof, moisture-proof and insulating properties of electronic devices.
  • epoxy encapsulant After curing, epoxy encapsulant is brittle and has poor heat resistance. Compared with epoxy resin, silicone encapsulant is soft after curing, has good toughness and resistance to high and low temperatures, and can more effectively eliminate internal stress.
  • the electronic device In a relatively wide temperature range, the electronic device exhibits good resistance to external shocks and vibrations; at the same time, due to its excellent heat resistance, it is not easy to yellow during long-term use; but currently commonly used
  • the thermal conductivity of the silicone potting compound is poor, and it cannot dissipate the heat generated by the electronic device in time. It is easy to cause the internal temperature of the electronic device to be too high and cause damage or even danger.
  • the current method to improve the thermal conductivity of silicone encapsulants is mainly to add thermally conductive materials to the silicone encapsulants, but the dispersibility of the thermally conductive materials in the resin is poor, although the prior art uses the surface modification of the thermally conductive materials It is then filled into the silicone encapsulant, but there is still a great probability of uneven dispersion in actual use, and particle sedimentation occurs during use or storage, which affects the thermal conductivity, mechanical and electrical properties of the product.
  • a large amount of thermal conductive material is added, and the thermal conductive material is usually nano-sized.
  • the fluidity of the silicone encapsulant is poor regardless of whether it is at room temperature or under heating conditions, resulting in penetration
  • the performance is not good, which is not conducive to the formation of an overall insulating structure without air gaps, and there is a phenomenon of partial discharge in the later stage; on the other hand, even if the surface of the nanoparticles is modified, there is still a great probability during the storage or use of the silicone potting
  • the agglomeration phenomenon occurs, which not only increases the cost of buying nano-sized thermal conductive materials in the early stage, but also fails to obtain nano-sized high thermal conductivity in the later stage.
  • the purpose of the present invention is to overcome the shortcomings of the prior art and provide a new type of two-component silicone encapsulant, which can not only ensure that the silicone encapsulant has high thermal conductivity and long-lasting insulation, but also avoids use or storage Particle sedimentation occurs during the process, so that the quality of the potting glue between batches remains uniform and stable, and it also has high and low temperature resistance (high temperature resistance up to 250°C, low temperature resistance up to -60°C) and excellent mechanical mechanics Performance, etc.
  • the invention also provides an application method of the above-mentioned two-component silicone potting glue.
  • the present invention adopts the following technical solutions:
  • a two-component silicone potting adhesive comprising component A and component B, said component A including hyperbranched silicone resin with terminal siloxane groups, vinyl MQ resin and first thermal conductive material,
  • the B component includes hydrogen-containing silicone oil, a silane coupling agent and a second thermal conductive material; wherein, the hyperbranched silicone resin with terminal siloxane groups is composed of methyl ethyl vinyl siloxane and dimethyl siloxane.
  • the molar ratio of the methyl ethyl vinyl siloxane to the dimethyl allyl siloxane is 0.5-2:1.
  • the molar ratio of the methyl ethyl vinyl siloxane to the dimethyl allyl siloxane is 1-2:1.
  • the methyl ethyl vinyl silicone Alkanes account for 50-70%, and the dimethylallylsiloxane accounts for 30-50%.
  • the temperature of the reaction is controlled to be 70-80°C.
  • the reaction in the reaction of the methyl ethyl vinyl siloxane and the dimethyl allyl siloxane, the reaction is controlled to proceed in the presence of a protective gas and under a catalyst .
  • the catalyst includes but is not limited to chloroplatinic acid.
  • the protective gas may be nitrogen, argon, or the like.
  • each molecule of the hyperbranched silicone resin with terminal siloxane groups contains 6-12 terminal siloxane groups, so that the hyperbranched silicone resin has a viscosity suitable for the system. , So that the entire system can maintain a high viscosity at room temperature, to ensure that the thermally conductive materials dispersed in the system remain stable, and reduce the sedimentation of the thermally conductive materials during storage; at the same time, it can have excellent fluidity after a little warming. It is conducive to the penetration of the potting compound, making it fully filled, and ensuring that the potting compound has excellent thermal conductivity and electrical insulation properties.
  • the feeding quality of the hyperbranched silicone resin with terminal siloxane groups, the vinyl MQ resin and the first thermally conductive material The ratio is 7-14:1:5.5-12.
  • the mass ratio of the hydrogen-containing silicone oil, the silane coupling agent and the second thermal conductive material is 13-25:1:3- 10.
  • the first thermally conductive material and the second thermally conductive material are respectively composed of aluminum oxide and boron nitride.
  • the aluminum oxide accounts for 70-80%
  • the boron nitride accounts for 20-80%. 30%.
  • the average particle size of the alumina is 2-50 ⁇ m, preferably 3-20 ⁇ m, more preferably 5-15 ⁇ m.
  • the alumina is spherical alumina, and in the first heat-conducting material and/or the second heat-conducting material, the mass percentage of the alumina is relative to its own average particle size. Is directly proportional to the size.
  • the first heat-conducting material and the second heat-conducting material are respectively composed of alumina and boron nitride with a feed mass ratio of 7:3; wherein the alumina is spherical alumina with an average The particle size is 6 ⁇ 1 ⁇ m.
  • the first heat-conducting material and the second heat-conducting material are respectively composed of alumina and boron nitride with a feed mass ratio of 8:2; wherein the alumina is spherical alumina, The average particle size is 14 ⁇ 1 ⁇ m.
  • the use of the above-mentioned combination of thermally conductive materials can further reduce the problem of thermally conductive material settling during the casting process of the silicone encapsulant, thereby ensuring that the prepared silicone encapsulant has better properties.
  • the thermal conductivity does not affect other properties and even has a boosting effect.
  • the feed mass ratio of the A component to the B component is 8-12:1.
  • the A component in terms of parts by mass, 500-700 parts of the hyperbranched silicone resin with terminal siloxane groups, and 50-70 parts of the vinyl MQ resin 400-600 parts of the first thermal conductive material, and optionally 1-1.5 parts of the catalyst.
  • the B component in terms of parts by mass, in the B component, 200-250 parts of the hydrogen-containing silicone oil, 10-15 parts of the silane coupling agent and 50-100 parts of the second thermal conductive material .
  • the content of vinyl in the vinyl MQ resin is 2.0-4.0%.
  • the hydrogen content of the hydrogen-containing silicone oil is 1.55-1.85%.
  • the silane coupling agent includes: vinyl triethoxy silane, vinyl trimethoxy silane, vinyl tris ( ⁇ -methoxyethoxy) silane) and the like.
  • an application method of the above-mentioned two-component silicone encapsulant includes the following steps: during application, weigh the A component and the formula according to the formula. The B component is mixed and stirred uniformly, and then poured on the device to be potted and protected, and cured by reaction.
  • the devices to be potted and protected include potting of the ends of the stator channel steel of the wind generator, high-power electronic components, module power supplies and circuit boards that require high heat dissipation and temperature resistance, and so on.
  • the present invention has the following advantages compared with the prior art:
  • the present invention innovatively uses components A and B with specific ingredients to form a two-component silicone potting sealant.
  • components A and B When stored, components A and B are separately packaged and stored, and when used, they can be directly mixed with groups A and B. It can be divided, poured, and reacted to cure.
  • the use of a specific hyperbranched silicone resin with terminal siloxane groups in the A component of the two-component silicone encapsulant gives the system a Proper viscosity can ensure that the thermal conductive material remains stable in the system, reduce the sedimentation of the thermal conductive material during storage, make the quality of the potting glue between batches stable, and have excellent fluidity after heating.
  • the product has high temperature resistance (up to 250 °C), low temperature resistance (can be as low as -60°C), good aging resistance, small shrinkage, excellent waterproof and moisture resistance, good adhesion, good rubber elasticity after curing, etc., thereby making the two-component of the present invention
  • the potting glue is especially suitable for the potting of the end of the stator channel steel of the wind generator, and it is also suitable for the potting protection of high-power electronic components, module power supplies and circuit boards that require high heat dissipation and temperature resistance.
  • the hyperbranched silicone resin with terminal siloxane groups has 6 terminal siloxane groups per molecule.
  • the hyperbranched silicone resin with terminal siloxane groups has 12 terminal siloxane groups per molecule.
  • the hyperbranched silicone resin with terminal siloxane groups has 8 terminal siloxane groups per molecule.
  • examples 4-7 respectively provide a two-component silicone potting compound, including A component and B component, the mass ratio of A component and B component is 10:1, and the specific components and dosage are shown in Table 1 below.
  • component A Preparation of component A: Weigh the ingredients in component A according to the formula, and then mix them for later use;
  • Preparation of component B Weigh the ingredients in component B according to the formula and mix them for later use.
  • Example 4 It is basically the same as in Example 4, except that the hyperbranched silicone resin with terminal siloxane group prepared according to Example 1 in the A component is replaced with a commonly used commercially available double-terminated vinyl group of the same mass. Silicone oil (viscosity is about 60Mpa.s, purchased from Jiande Poly New Material Co., Ltd.). After one year of storage at room temperature and dark, a large amount of filler deposits can be seen at the bottom of the barrel, serious agglomeration at the bottom, the upper layer is resin, and the lower layer is filler. The filler in the lower layer is heavily deposited and cannot be poured out.
  • Silicone oil viscosity is about 60Mpa.s, purchased from Jiande Poly New Material Co., Ltd.

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Abstract

本发明公开了一种双组份有机硅灌封胶及其应用方法，包括A、B组分，A组分包括具有端基硅氧烷基的超支化有机硅树脂、乙烯基MQ树脂和第一导热材料，B组分包括含氢硅油、硅烷偶联剂和第二导热材料；具有端基硅氧烷基的超支化有机硅树脂由投料摩尔比为0.5-2∶1的甲基乙基乙烯基硅氧烷和二甲基烯丙基硅氧烷反应制成；应用方法：在应用时，按配方量称取A、B组分，混合搅拌均匀后浇注在待灌封保护的器件上，反应固化即可；本发明的双组份有机硅灌封胶，其不仅能够确保有机硅灌封胶具有高导热性能、绝缘性持久，而且避免了使用或存放过程中出现粒子沉降现象，使得批次间的灌封胶质量保持均一稳定，同时还兼具耐高低温性能及优异的机械力学性能等。

Description

一种双组份有机硅灌封胶及其应用方法
本申请要求申请号为：CN201911212819.3、申请日为2019.12.2的中国国家知识产权局的在先专利申请为优先权，该在先专利申请文本中的内容通过引用而完全加入本专利申请中。
技术领域
本发明属于绝缘材料技术领域，具体涉及一种双组份有机硅灌封胶及其应用方法，其主要应用于风发电机定子槽钢端部的灌封，也适用于大功率电子元器件、对散热和耐温要求较高的模块电源和线路板的灌封防护。
背景技术
灌封可以赋予电机、电子器件整体性，使内部元件、线路具有良好的耐外界冲击、震动的能力，避免内部元件、线路直接暴露，提高电子器件的防水、防潮和绝缘性能。环氧树脂灌封胶固化后质脆，耐热性差，与环氧树脂相比，有机硅灌封胶固化后质软，具有良好的韧性和耐高、低温性能，可以更加有效的消除内部应力，在相对宽的温度范围内，使电子器件表现出良好的对外界冲击、震动的抵抗力；同时由于其优异的耐热性能，在长期使用过程中，其也不易黄变；但是目前常用的有机硅灌封胶的导热性较差，不能及时地散除电子器件产生的热量，容易使电子器件内部温度过高以致损坏，甚至产生危险。
目前提高有机硅灌封胶导热性的方法主要是在有机硅灌封胶中添加导热材料，但导热材料在树脂中的分散性较差，虽然现有技术中采用对导热材料的表面进行改性后再填充进有机硅灌封胶中，但实际使用中仍然极大概率地出现分散不均匀，而且在使用或存放过程中出现粒子沉降现象，影响了产品导热效率及机械性能和电性能。同时为了获得高导热，导热材料的添加量较大、导热材料通常也选用的是纳米尺寸，进而一方面导致有机硅灌封胶的流动性不管是在常温还是加热条件下均较差，致使渗透性不好，不利于形成无气隙的整体绝缘结构，后期存在局部放电的现象；另一方面，纳米粒子即使是表面改性后在有机硅灌封胶的存放或使用过程中仍然极大概率地发生团聚现象，进而不仅使得前期购买纳米尺寸导热材料导致成本增加，后期还无法获得纳米尺寸的高导热性能。
发明内容
本发明的目的在于克服现有技术的不足，提供一种新型的双组份有机硅灌封胶，其不仅能够确保有机硅灌封胶具有高导热性能、绝缘性持久，而且避免了使用或存放 过程中出现粒子沉降现象，使得批次间的灌封胶质量保持均一稳定，同时还能兼具耐高低温性能(耐高温可达250℃，耐低温可至-60℃)以及优异的机械力学性能等。
本发明还提供了一种上述双组份有机硅灌封胶的应用方法。
为解决上述技术问题，本发明采取如下技术方案：
一种双组份有机硅灌封胶，包括A组分和B组分，所述A组分包括具有端基硅氧烷基的超支化有机硅树脂、乙烯基MQ树脂和第一导热材料，所述B组分包括含氢硅油、硅烷偶联剂和第二导热材料；其中，所述具有端基硅氧烷基的超支化有机硅树脂由甲基乙基乙烯基硅氧烷和二甲基烯丙基硅氧烷反应制成，所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的投料摩尔比为0.5-2∶1。
根据本发明的一些优选且具体的方面，所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的投料摩尔比为1-2∶1。
根据本发明的一些优选方面，以所述甲基乙基乙烯基硅氧烷和所述二甲基烯丙基硅氧烷的总投料摩尔百分量计，所述甲基乙基乙烯基硅氧烷占50-70％，所述二甲基烯丙基硅氧烷占30-50％。
根据本发明的一些优选方面，在所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的反应中，控制所述反应的温度为70-80℃。
根据本发明的一些优选方面，在所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的反应中，控制所述反应在保护气体存在下、在催化剂下进行。
根据本发明的一些具体且优选的方面，所述催化剂包括但不限于氯铂酸。
根据本发明的一些具体方面，所述保护气体可以为氮气、氩气等等。
根据本发明的一些优选方面，每分子所述具有端基硅氧烷基的超支化有机硅树脂包含端基硅氧烷基6-12个，如此可以使得超支化有机硅树脂具有适合体系的粘度，使得整个体系在常温下能够保持较高粘度，确保分散在体系中的导热材料保持稳定，减少存放过程中出现的导热材料沉降现象；同时稍加温后又能够具有极佳的流动性，有利于灌封胶的渗透，使之填充充分，确保灌封胶具有优异的导热性以及电绝缘性能等。
根据本发明的一些具体且优选的方面，所述A组分中，所述具有端基硅氧烷基的超支化有机硅树脂、所述乙烯基MQ树脂和所述第一导热材料的投料质量比为7-14∶1∶5.5-12。
根据本发明的一些具体且优选的方面，所述B组分中，所述含氢硅油、所述硅烷偶联剂和所述第二导热材料的投料质量比为13-25∶1∶3-10。
根据本发明的一些优选方面，所述第一导热材料、所述第二导热材料分别由氧化铝和氮化硼构成。
根据本发明的一些优选方面，以质量百分含量计，所述第一导热材料和/或所述第二导热材料中，所述氧化铝占70-80％，所述氮化硼占20-30％。
根据本发明的一些优选且具体的方面，所述氧化铝的平均粒径为2-50μm，优选为3-20μm，更优选为5-15μm。
根据本发明的一些优选方面，所述氧化铝为球形氧化铝，且在所述第一导热材料和/或所述第二导热材料中，所述氧化铝的质量百分含量与其自身平均粒径的大小成正比。
根据本发明的一个具体方面，所述第一导热材料、所述第二导热材料分别由投料质量比为7∶3的氧化铝和氮化硼构成；其中所述氧化铝为球形氧化铝，平均粒径为6±1μm。
根据本发明的又一个具体方面，所述第一导热材料、所述第二导热材料分别由投料质量比为8∶2的氧化铝和氮化硼构成；其中所述氧化铝为球形氧化铝，平均粒径为14±1μm。
在本发明的特定体系中，优选地，采用上述组合的导热材料可进一步减少有机硅灌封胶在浇注过程中发生导热材料沉降的问题，进而能够确保制成的有机硅灌封胶具有较优的导热系数且不影响其它性能甚至还有提升作用。
根据本发明的一些优选方面，所述A组分与所述B组分的投料质量比为8-12∶1。
根据本发明的一些优选方面，以质量份数计，所述A组分中，所述具有端基硅氧烷基的超支化有机硅树脂500-700份、所述乙烯基MQ树脂50-70份和所述第一导热材料400-600份，还选择性的包括催化剂1-1.5份。
根据本发明的一些优选方面，以质量份数计，所述B组分中，所述含氢硅油200-250份、所述硅烷偶联剂10-15份和第二导热材料50-100份。
根据本发明的一些具体且优选的方面，所述乙烯基MQ树脂中乙烯基的含量为2.0-4.0％。
根据本发明的一些具体且优选的方面，所述含氢硅油的氢含量为1.55-1.85％。
根据本发明的一些具体方面，所述硅烷偶联剂包括：乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三(β-甲氧乙氧基)硅烷)等等。
本发明提供的又一技术方案：一种上述所述的双组份有机硅灌封胶的应用方法，所述应用方法包括如下步骤：在应用时，按照配方量称取所述A组分与所述B组分，混合搅拌均匀，然后浇注在待灌封保护的器件上，反应固化，即可。
根据本发明，所述待灌封保护的器件包括风发电机定子槽钢端部的灌封、大功率电子元器件、对散热和耐温要求较高的模块电源和线路板等等。
由于以上技术方案的实施，本发明与现有技术相比具有如下优点：
本发明创新地采用具有特定成分的A、B组分构成双组份有机硅灌封胶，当存放时，A、B组分分别单独包装存放，而使用时，则可以直接混合A、B组分，浇注，反应固化即可，其中由于在双组份有机硅灌封胶的A组分中采用了特定的具有端基硅氧烷基的超支化有机硅树脂，赋予了体系在常温下具有适当的粘度，能够确保导热材料在体系中保持稳定，减少了存放过程中导热材料的沉降现象，使得批次间的灌封胶质量稳定，而且加温后又能够具有极佳的流动性，有利于灌封胶的渗透，进而填充时能够填充充分，不仅保证了体系较好的导热系数，而且机械力学性能和绝缘性能优异；同时该产品在交联固化后还具有耐温高(可达250℃)、耐低温(可低至-60℃)、耐老化性好、收缩小、防水防潮性优、粘结性好、固化后保持了良好的橡胶弹性等优点，进而使得本发明的双组份灌封胶尤其适用于风发电机定子槽钢端部的灌封，也适用于大功率电子元器件、对散热和耐温要求较高的模块电源和线路板的灌封防护。
具体实施方式
以下结合具体实施例对本发明做进一步详细说明。应理解，这些实施例用于说明本发明的基本原理、主要特征和优点，而本发明不受以下实施例的限制。实施例中采用的实施条件可以根据具体要求做进一步调整，未注明的实施条件通常为常规实验中的条件。实施例所用原料均为可商购的工业品。
下述实施例中，如无特殊说明，所有的原料基本来自于商购或者通过本领域的常规方法制备而得，下述中端基硅氧烷基的个数可以通过现有技术中常规的核磁共振测得。下述述及的甲基乙基乙烯基硅氧烷的结构式为：
Figure PCTCN2020121846-appb-000001
二甲基烯丙基硅氧烷的结构式为：
Figure PCTCN2020121846-appb-000002
实施例1具有端基硅氧烷基的超支化有机硅树脂的制备
称取1500g甲基乙基乙烯基硅氧烷与1500g二甲基烯丙基硅氧烷，混合并加入7g氯铂酸，然后在氮气保护下、在75±3℃下反应5.5小时，制成具有端基硅氧烷基的超支化有机硅树脂，测得每分子具有端基硅氧烷基6个。
实施例2具有端基硅氧烷基的超支化有机硅树脂的制备
称取2000g甲基乙基乙烯基硅氧烷与1000g二甲基烯丙基硅氧烷，混合并加入7g氯铂酸，然后在氮气保护下、在75±3℃下反应5.5小时，制成具有端基硅氧烷基的超支化有机硅树脂，测得每分子具有端基硅氧烷基12个。
实施例3具有端基硅氧烷基的超支化有机硅树脂的制备
称取1750g甲基乙基乙烯基硅氧烷与1250g二甲基烯丙基硅氧烷，混合并加入7g氯铂酸，然后在氮气保护下、在75±3℃下反应5.5小时，制成具有端基硅氧烷基的超支化有机硅树脂，测得每分子具有端基硅氧烷基8个。
实施例4-7
下述实施例4-7分别提供一种双组份有机硅灌封胶，包括A组分和B组分，A组分和B组分的投料质量比为10∶1，具体成分以及用量参见下表1。
表1
Figure PCTCN2020121846-appb-000003
Figure PCTCN2020121846-appb-000004
A组分的制备：按配方称取A组分中的各原料，然后混合备用；
B组分的制备：按配方称取B组分中的各原料，然后混合备用。
实际应用时，按照配方量各自称取A、B组分，然后混合，浇注于待灌封保护的器件上，固化，即可。
对比例
基本同实施例4，其区别仅在于：将A组分中按照实施例1制备的具有端基硅氧烷基的超支化有机硅树脂替换为常用的市售的同等质量份的双端乙烯基硅油(粘度约为60Mpa.s，购自建德市聚合新材料有限公司)，室温避光存放一年后可见桶底有大量填料沉积，严重的底部结块，上层是树脂，下层是填料，下层的填料沉积严重且倒不出来。
性能测试
将上述实施例4-7以及对比例所获得双组份有机硅灌封胶进行如下一些性能测试，具体结果参见表2所示。
表2
Figure PCTCN2020121846-appb-000005
Figure PCTCN2020121846-appb-000006
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围，凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (10)

  1. 一种双组份有机硅灌封胶，包括A组分和B组分，其特征在于，所述A组分包括具有端基硅氧烷基的超支化有机硅树脂、乙烯基MQ树脂和第一导热材料，所述B组分包括含氢硅油、硅烷偶联剂和第二导热材料；其中，所述具有端基硅氧烷基的超支化有机硅树脂由甲基乙基乙烯基硅氧烷和二甲基烯丙基硅氧烷反应制成，所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的投料摩尔比为0.5-2∶1。
  2. 根据权利要求1所述的双组份有机硅灌封胶，其特征在于，所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的投料摩尔比为1-2∶1。
  3. 根据权利要求1或2所述的双组份有机硅灌封胶，其特征在于，以所述甲基乙基乙烯基硅氧烷和所述二甲基烯丙基硅氧烷的总投料摩尔百分量计，所述甲基乙基乙烯基硅氧烷占50-70％，所述二甲基烯丙基硅氧烷占30-50％。
  4. 根据权利要求1或2所述的双组份有机硅灌封胶，其特征在于，在所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的反应中，控制所述反应的温度为70-80℃；和/或，在所述甲基乙基乙烯基硅氧烷与所述二甲基烯丙基硅氧烷的反应中，控制所述反应在保护气体存在下、在催化剂下进行，所述催化剂包括氯铂酸。
  5. 根据权利要求1或2所述的双组份有机硅灌封胶，其特征在于，每分子所述具有端基硅氧烷基的超支化有机硅树脂包含端基硅氧烷基6-12个。
  6. 根据权利要求1或2所述的双组份有机硅灌封胶，其特征在于，所述A组分中，所述具有端基硅氧烷基的超支化有机硅树脂、所述乙烯基MQ树脂和所述第一导热材料的投料质量比为7-14∶1∶5.5-12；和/或，所述B组分中，所述含氢硅油、所述硅烷偶联剂和所述第二导热材料的投料质量比为13-25∶1∶3-10。
  7. 根据权利要求1或2所述的双组份有机硅灌封胶，其特征在于，所述第一导热材料、所述第二导热材料分别由氧化铝和氮化硼构成；其中以质量百分含量计，所述氧化铝占70-80％，所述氮化硼占20-30％，所述氧化铝的平均粒径为2-50μm，优选为3-20μm，更优选为5-15μm。
  8. 根据权利要求7所述的双组份有机硅灌封胶，其特征在于，所述氧化铝为球形氧化铝，且在所述第一导热材料和/或所述第二导热材料中，所述氧化铝的质量百分含量与其自身平均粒径的大小成正比。
  9. 根据权利要求1或2所述的双组份有机硅灌封胶，其特征在于，所述A组分与所述B组分的投料质量比为8-12∶1；其中，以质量份数计，所述A组分中，所述具有端基硅氧烷基的超支化有机硅树脂500-700份、所述乙烯基MQ树脂50-70份和所述第一导热材料400-600份，还选择性的包括催化剂1-1.5份；以质量份数计， 所述B组分中，所述含氢硅油200-250份、所述硅烷偶联剂10-15份和第二导热材料50-100份；和/或，
    所述乙烯基MQ树脂中乙烯基的含量为2.0-4.0％；和/或，所述含氢硅油的氢含量为1.55-1.85％。
  10. 一种权利要求1-9中任一项权利要求所述的双组份有机硅灌封胶的应用方法，其特征在于，所述应用方法包括如下步骤：在应用时，按照配方量称取所述A组分与所述B组分，混合搅拌均匀，然后浇注在待灌封保护的器件上，反应固化，即可。
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