CN110845989B - Two-component organic silicon pouring sealant and application method thereof - Google Patents
Two-component organic silicon pouring sealant and application method thereof Download PDFInfo
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- CN110845989B CN110845989B CN201911212819.3A CN201911212819A CN110845989B CN 110845989 B CN110845989 B CN 110845989B CN 201911212819 A CN201911212819 A CN 201911212819A CN 110845989 B CN110845989 B CN 110845989B
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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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
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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
- 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
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- 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
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- 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
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- 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
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- 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
Abstract
The invention discloses a two-component organic silicon pouring sealant and an application method thereof, wherein the two-component organic silicon pouring sealant comprises A, B components, wherein the A component comprises hyperbranched organic silicon resin with terminal siloxane groups, vinyl MQ resin and a first heat conduction material, and the B component comprises hydrogen-containing silicone oil, a silane coupling agent and a second heat conduction material; the hyperbranched organic silicon resin with the terminal siloxane group is prepared by the reaction of methyl ethyl vinyl siloxane and dimethyl allyl siloxane with the feeding molar ratio of 0.5-2: 1; the application method comprises the following steps: when in application, A, B components are weighed according to the formula amount, mixed and stirred uniformly, poured on a device to be encapsulated and protected, and reacted and cured; the two-component organic silicon pouring sealant disclosed by the invention can ensure that the organic silicon pouring sealant has high heat-conducting property and lasting insulativity, and avoids the phenomenon of particle sedimentation in the using or storing process, so that the pouring sealant quality among batches is kept uniform and stable, and the two-component organic silicon pouring sealant also has high and low temperature resistance, excellent mechanical property and the like.
Description
Technical Field
The invention belongs to the technical field of insulating materials, and particularly relates to a two-component organic silicon pouring sealant and an application method thereof.
Background
The encapsulation can give motor, electron device wholeness, makes interior component, circuit have good external shock resistance, the ability of vibrations, avoids interior component, circuit directly to expose, improves electron device's waterproof, dampproofing and insulating properties. The epoxy resin potting adhesive is brittle after being cured and poor in heat resistance, compared with epoxy resin, the organic silicon potting adhesive is soft after being cured, has good toughness and high and low temperature resistance, can effectively eliminate internal stress, and enables electronic devices to show good resistance to external impact and vibration in a relatively wide temperature range; meanwhile, due to the excellent heat resistance, the paint is not easy to yellow in the long-term use process; however, the currently used silicone potting adhesive has poor thermal conductivity, cannot timely dissipate heat generated by an electronic device, and is easily damaged or even dangerous due to over-high internal temperature of the electronic device.
At present, the method for improving the heat conductivity of the organic silicon pouring sealant mainly comprises the steps of adding a heat conduction material into the organic silicon pouring sealant, but the dispersibility of the heat conduction material in resin is poor, and although the surface of the heat conduction material is modified and then is filled into the organic silicon pouring sealant in the prior art, the uneven dispersion still occurs in practical use at a very high probability, and the particle sedimentation phenomenon occurs in the using or storing process, so that the heat conduction efficiency, the mechanical property and the electrical property of the product are influenced. Meanwhile, in order to obtain high heat conduction, the addition amount of the heat conduction material is large, and the heat conduction material is usually selected to be in a nanometer size, so that on one hand, the flowability of the organic silicon pouring sealant is poor under normal temperature or heating condition, so that the permeability is poor, the formation of an integral insulation structure without air gaps is not facilitated, and the phenomenon of partial discharge exists in the later stage; on the other hand, the nanoparticles are still aggregated with a great probability in the storage or use process of the organic silicon pouring sealant even after the surface modification, so that the cost is increased due to the purchase of the nano-sized heat conduction material at the early stage, and the nano-sized high heat conduction performance cannot be obtained at the later stage.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a novel two-component organic silicon pouring sealant which not only can ensure that the organic silicon pouring sealant has high heat-conducting property and lasting insulativity, but also can avoid the particle sedimentation phenomenon in the using or storing process, so that the pouring sealant between batches keeps uniform and stable in quality, and simultaneously has high and low temperature resistance (the high temperature resistance can reach 250 ℃, and the low temperature resistance can reach-60 ℃) and excellent mechanical properties and the like.
The invention also provides an application method of the two-component organic silicon pouring sealant.
In order to solve the technical problems, the invention adopts the following technical scheme:
a two-component organic silicon pouring sealant comprises a component A and a component B, wherein the component A comprises hyperbranched organic silicon resin with terminal siloxane groups, vinyl MQ resin and a first heat conduction material, and the component B comprises hydrogen-containing silicone oil, a silane coupling agent and a second heat conduction material; the hyperbranched organic silicon resin with the terminal siloxane group is prepared by reacting methyl ethyl vinyl siloxane and dimethyl allyl siloxane, and the feeding molar ratio of the methyl ethyl vinyl siloxane to the dimethyl allyl siloxane is 0.5-2: 1.
According to some preferred and specific aspects of the present invention, the molar ratio of the methyl ethyl vinyl siloxane to the dimethyl allyl siloxane is 1-2: 1.
According to some preferred aspects of the present invention, the methyl ethyl vinyl siloxane comprises 50-70% and the dimethyl allyl siloxane comprises 30-50% by mole of the total charge of the methyl ethyl vinyl siloxane and the dimethyl allyl siloxane.
According to some preferred aspects of the present invention, in the reaction of the methyl ethyl vinyl siloxane with the dimethyl allyl siloxane, the temperature of the reaction is controlled to be 70-80 ℃.
According to some preferred aspects of the present invention, in the reaction of the methylethylvinylsiloxane with the dimethylallyl siloxane, the reaction is controlled to be carried out in the presence of a protective gas under a catalyst.
According to some specific and preferred aspects of the present invention, the catalyst includes, but is not limited to, chloroplatinic acid.
According to some specific aspects of the present invention, the shielding gas may be nitrogen, argon, or the like.
According to some preferred aspects of the invention, each molecule of the hyperbranched organic silicon resin with terminal siloxane groups contains 6-12 terminal siloxane groups, so that the hyperbranched organic silicon resin has a viscosity suitable for a system, the whole system can keep higher viscosity at normal temperature, a heat conduction material dispersed in the system is ensured to be stable, and the phenomenon of sedimentation of the heat conduction material in the storage process is reduced; meanwhile, the sealant can have excellent fluidity after being slightly heated, is beneficial to the permeation of the potting sealant, ensures the potting sealant to have excellent thermal conductivity, electric insulation performance and the like, and is fully filled.
According to some specific and preferred aspects of the present invention, in the a component, the hyperbranched silicone resin having a terminal siloxane group, the vinyl MQ resin, and the first heat conductive material are charged at a mass ratio of 7-14: 1: 5.5-12.
According to some specific and preferred aspects of the present invention, in the B component, the feeding mass ratio of the hydrogen-containing silicone oil, the silane coupling agent and the second heat conductive material is 13-25: 1: 3-10.
According to some preferred aspects of the present invention, the first and second heat conductive materials are composed of aluminum oxide and boron nitride, respectively.
According to some preferred aspects of the present invention, in the first heat conductive material and/or the second heat conductive material, the alumina accounts for 70-80% and the boron nitride accounts for 20-30% by mass percentage.
According to some preferred and specific aspects of the present invention, the alumina has an average particle size of 2 to 50 μm, preferably 3 to 20 μm, more preferably 5 to 15 μm.
According to some preferred aspects of the invention, the alumina is spherical alumina, and the mass percentage of the alumina in the first heat conducting material and/or the second heat conducting material is proportional to the size of the average particle size of the alumina.
According to a specific aspect of the invention, the first heat conduction material and the second heat conduction material are respectively composed of aluminum oxide and boron nitride which are fed in a mass ratio of 7: 3; wherein the alumina is spherical alumina with the average grain diameter of 6 +/-1 mu m.
According to another specific aspect of the invention, the first heat conduction material and the second heat conduction material are respectively composed of aluminum oxide and boron nitride which are fed in a mass ratio of 8: 2; wherein the alumina is spherical alumina with the average grain diameter of 14 +/-1 mu m.
In the specific system of the invention, preferably, the heat conduction material adopting the combination can further reduce the problem of heat conduction material sedimentation of the organic silicon pouring sealant in the pouring process, thereby ensuring that the prepared organic silicon pouring sealant has better heat conduction coefficient, does not influence other performances and even has a promotion effect.
According to some preferred aspects of the present invention, the feed mass ratio of the A component to the B component is 8-12: 1.
According to some preferred aspects of the invention, in the component A, 700 parts by mass of the hyperbranched silicone resin with terminal siloxane groups, 50-70 parts by mass of the vinyl MQ resin and 600 parts by mass of the first heat conduction material 400, and optionally 1-1.5 parts by mass of a catalyst are included.
According to some preferred aspects of the present invention, in the component B, on a mass part basis, the hydrogen-containing silicone oil is 200-250 parts, the silane coupling agent is 10-15 parts, and the second heat conductive material is 50-100 parts.
According to some specific and preferred aspects of the present invention, the vinyl content of the vinyl MQ resin is 2.0 to 4.0%.
According to some specific and preferred aspects of the present invention, the hydrogen content of the hydrogen-containing silicone oil is 1.55 to 1.85%.
According to some specific aspects of the present invention, the silane coupling agent comprises: vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (. beta. -methoxyethoxy) silane), and the like.
The invention provides another technical scheme that: an application method of the two-component organic silicon pouring sealant comprises the following steps: when the epoxy resin is applied, the component A and the component B are weighed according to the formula, mixed and stirred uniformly, then poured on a device to be encapsulated and protected, and reacted and cured.
According to the invention, the devices to be encapsulated and protected comprise encapsulation at the end part of a wind turbine stator channel steel, high-power electronic components, module power supplies and circuit boards with high requirements on heat dissipation and temperature resistance, and the like.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention innovatively adopts A, B components with specific components to form the two-component organic silicon pouring sealant, when the A, B components are stored separately, they can be mixed directly A, B components, cast, reacted and solidified, wherein, the component A of the two-component organic silicon pouring sealant adopts the specific hyperbranched organic silicon resin with terminal siloxane groups, so that the system has proper viscosity at normal temperature, the heat conduction material can be ensured to be kept stable in the system, and the sedimentation phenomenon of the heat conduction material in the storage process is reduced, so that the pouring sealant between batches has stable quality, and has excellent fluidity after being heated, thereby being beneficial to the permeation of the pouring sealant, the filling can be fully carried out during filling, so that the better heat conductivity coefficient of the system is ensured, and the mechanical property and the insulating property are excellent; meanwhile, the product has the advantages of high temperature resistance (up to 250 ℃), low temperature resistance (down to-60 ℃), good aging resistance, small shrinkage, excellent waterproof and moisture resistance, good cohesiveness, good rubber elasticity after curing and the like after cross-linking and curing, so that the two-component pouring sealant disclosed by the invention is particularly suitable for pouring and sealing the end part of the channel steel of the stator of the wind driven generator, and is also suitable for pouring and sealing protection of high-power electronic components, module power supplies and circuit boards with high requirements on heat dissipation and temperature resistance.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that these examples are for the purpose of illustrating the general principles, essential features and advantages of the present invention, and the present invention is not limited by the following examples. The implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments. The raw materials used in the examples are all commercially available commercial products.
In the following examples, all starting materials are essentially commercially available or prepared by methods conventional in the art, unless otherwise specified, and the number of terminal siloxanyl groups described below can be determined by nuclear magnetic resonance as is conventional in the art. The structural formula of the methyl ethyl vinyl siloxane described below is:
the structural formula of the dimethylallyl siloxane is as follows:
example 1 preparation of hyperbranched Silicone resins having terminal siloxane groups
1500g of methyl ethyl vinyl siloxane and 1500g of dimethyl allyl siloxane are weighed, mixed and added with 7g of chloroplatinic acid, and then reacted for 5.5 hours at 75 +/-3 ℃ under the protection of nitrogen to prepare the hyperbranched organic silicon resin with the terminal siloxane groups, and 6 siloxane groups with the terminal groups are measured in each molecule.
Example 2 preparation of hyperbranched Silicone resins having terminal siloxane groups
2000g of methyl ethyl vinyl siloxane and 1000g of dimethyl allyl siloxane are weighed, mixed and added with 7g of chloroplatinic acid, and then reacted for 5.5 hours at 75 +/-3 ℃ under the protection of nitrogen to prepare the hyperbranched organic silicon resin with the terminal siloxane groups, and the number of the terminal siloxane groups in each molecule is measured to be 12.
Example 3 preparation of hyperbranched Silicone resins having terminal siloxane groups
1750g of methyl ethyl vinyl siloxane and 1250g of dimethyl allyl siloxane are weighed, mixed and added with 7g of chloroplatinic acid, and then reacted for 5.5 hours at 75 +/-3 ℃ under the protection of nitrogen to prepare the hyperbranched organic silicon resin with the terminal siloxane groups, and 8 terminal siloxane groups are measured in each molecule.
Examples 4 to 7
The following embodiments 4 to 7 respectively provide a two-component silicone pouring sealant, which comprises a component A and a component B, wherein the feeding mass ratio of the component A to the component B is 10: 1, and the specific components and the dosage are shown in the following table 1.
TABLE 1
Preparation of component A: weighing the raw materials in the component A according to the formula, and then mixing for later use;
preparation of the component B: weighing the raw materials in the component B according to the formula, and then mixing for later use.
In actual application, A, B components are respectively weighed according to the formula amount, then mixed, poured on a device to be encapsulated and protected, and cured.
Comparative example
Basically, the method is the same as the method in example 4, and only differs from the method in that: the hyperbranched silicone resin with terminal siloxane groups prepared according to example 1 in the component A is replaced by the common commercial double-end vinyl silicone oil (with the viscosity of about 60Mpa.s, purchased from New polymeric Material Co., Ltd. of Jiande), and after the hyperbranched silicone resin is stored for one year at room temperature in a dark place, a large amount of filler is deposited at the bottom of a barrel, the bottom of the barrel is seriously caked, the upper layer is resin, the lower layer is filler, and the lower layer is seriously sedimented and can not fall out.
Performance testing
The following performance tests were performed on the two-component silicone pouring sealant obtained in the above examples 4-7 and comparative examples, and the specific results are shown in table 2.
TABLE 2
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (10)
1. A two-component organic silicon pouring sealant comprises a component A and a component B, and is characterized in that the component A comprises hyperbranched organic silicon resin with terminal siloxane groups, vinyl MQ resin and a first heat conduction material, the feeding mass ratio of the hyperbranched organic silicon resin with terminal siloxane groups, the vinyl MQ resin and the first heat conduction material is 7-14: 1: 5.5-12, the component B comprises hydrogen-containing silicone oil, a silane coupling agent and a second heat conduction material, and the feeding mass ratio of the hydrogen-containing silicone oil, the silane coupling agent and the second heat conduction material is 13-25: 1: 3-10; wherein the hyperbranched organic silicon resin with the terminal siloxane groups is prepared by reacting methyl ethyl vinyl siloxane and dimethyl allyl siloxane, the feeding molar ratio of the methyl ethyl vinyl siloxane to the dimethyl allyl siloxane is 0.5-2: 1, and the hyperbranched organic silicon resin with the terminal siloxane groups contains 6-12 terminal siloxane groups per molecule.
2. The two-component silicone pouring sealant as claimed in claim 1, wherein the molar ratio of the methyl ethyl vinyl siloxane to the dimethyl allyl siloxane is 1-2: 1.
3. The two-component silicone pouring sealant according to claim 1 or 2, wherein the methyl ethyl vinyl siloxane accounts for 50-70% and the dimethyl allyl siloxane accounts for 30-50% of the total molar percentage of the methyl ethyl vinyl siloxane and the dimethyl allyl siloxane.
4. The two-component silicone pouring sealant according to claim 1 or 2, characterized in that in the reaction of the methyl ethyl vinyl siloxane and the dimethyl allyl siloxane, the temperature of the reaction is controlled to be 70-80 ℃; and/or, in the reaction of the methyl ethyl vinyl siloxane and the dimethyl allyl siloxane, controlling the reaction to be carried out in the presence of protective gas and under the action of a catalyst, wherein the catalyst comprises chloroplatinic acid.
5. The two-component silicone pouring sealant according to claim 1 or 2, wherein the first heat-conducting material and the second heat-conducting material are respectively composed of aluminum oxide and boron nitride; wherein the aluminum oxide accounts for 70-80% by mass percentage, the boron nitride accounts for 20-30% by mass percentage, and the average grain diameter of the aluminum oxide is 2-50 μm.
6. The two-component silicone pouring sealant as claimed in claim 5, wherein the average particle size of the aluminum oxide is 3 to 20 μm.
7. The two-component silicone pouring sealant according to claim 6, wherein the average particle size of the aluminum oxide is 5 to 15 μm.
8. The two-component silicone pouring sealant according to claim 5, wherein the aluminum oxide is spherical aluminum oxide, and the mass percentage of the aluminum oxide in the first heat conduction material and/or the second heat conduction material is proportional to the size of the average particle diameter of the aluminum oxide.
9. The two-component silicone pouring sealant as claimed in claim 1 or 2, characterized in that the mass ratio of the component A to the component B is 8-12: 1; wherein, in the component A, the hyperbranched silicone resin with terminal siloxane groups comprises 700 parts by mass, the vinyl MQ resin comprises 50-70 parts by mass and the first heat conductive material comprises 400-600 parts by mass, and the component A also comprises 1-1.5 parts by mass of a catalyst; in the component B, by mass, the hydrogen-containing silicone oil is 200-250 parts, the silane coupling agent is 10-15 parts, and the second heat conduction material is 50-100 parts; and/or the presence of a gas in the gas,
the content of vinyl in the vinyl MQ resin is 2.0-4.0%; and/or the hydrogen content of the hydrogen-containing silicone oil is 1.55-1.85%.
10. The application method of the two-component silicone pouring sealant as claimed in any one of claims 1 to 9, characterized in that the application method comprises the following steps: when the epoxy resin is applied, the component A and the component B are weighed according to the formula, mixed and stirred uniformly, then poured on a device to be encapsulated and protected, and reacted and cured.
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| CN201911212819.3A CN110845989B (en) | 2019-12-02 | 2019-12-02 | Two-component organic silicon pouring sealant and application method thereof |
| PCT/CN2020/121846 WO2021109730A1 (en) | 2019-12-02 | 2020-10-19 | Two-component organosilicon potting sealant and application method therefor |
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| CN114802426B (en) * | 2022-06-02 | 2023-05-05 | 阿维塔科技(重庆)有限公司 | Power-assisted motor and protection method for electronic and electric parts thereof |
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| CN110845989A (en) | 2020-02-28 |
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Denomination of invention: A two-component silicone potting adhesive and its application method Effective date of registration: 20220530 Granted publication date: 20210903 Pledgee: CITIC Bank Limited by Share Ltd. Suzhou branch Pledgor: SUZHOU TAIHU ELECTRIC ADVANCED MATERIAL Co.,Ltd. Registration number: Y2022320010170 |