Organic silicon pouring sealant and preparation method thereof

Abstract

The invention discloses an organic silicon pouring sealant and a preparation method thereof, and belongs to the technical field of organic materials, the organic silicon pouring sealant comprises a component A and a component B. The component A comprises, by mass, 100 parts of vinyl silicone oil, 2-5 parts of a silane coupling agent, 10-22 parts of a conductive filler, 18-30 parts of a nano soft magnetic filler, 0.5-1.5 parts of an inhibitor and 1-3 parts of hydrogen-containing silicone oil; and the component B comprises 100 parts of vinyl silicone oil and 1-3 parts of a catalyst. The conductive filler, the nano soft magnetic filler and other substances are added into the organic silicon pouring sealant, so that the technical effect of improving the electromagnetic shielding performance of the pouring sealant is achieved.

Description

Technical Field

[0001] The present application relates to the technical field of organic materials, and in particular to an organic silicone potting compound and a preparation method thereof. Background Art

[0002] Electronic potting glue mainly includes epoxy resin, polyurethane, silicone, etc. Epoxy resin potting glue has good bonding and insulation properties and is cheap, but it is brittle after curing, has poor aging resistance, and poor moisture resistance. Polyurethane potting glue has excellent impact resistance, bonding performance, and good toughness, but the synthesis process is more complicated and the high temperature resistance is poor. Silicone potting glue has excellent anti-aging performance, weather resistance, high and low temperature resistance (-60℃~260℃), dielectric properties and insulation properties, and is moisture-proof and flame-retardant, but its adhesion is weak.

[0003] Silicone potting compounds are widely used, and electronic products will generate complex electromagnetic fields and certain electromagnetic interference during operation. For precision electronic products, improving electromagnetic shielding performance is even more important. Summary of the invention

[0004] The main purpose of the present application is to provide a silicone potting compound and a preparation method thereof, aiming to solve the technical problem that the current potting compound has poor electromagnetic shielding performance.

[0005] To achieve the above-mentioned purpose, the present application provides a silicone potting compound, comprising component A and component B. Component A comprises 100 parts of vinyl silicone oil, 2-5 parts of silane coupling agent, 10-22 parts of conductive filler, 18-30 parts of nano soft magnetic filler, 0.5-2 parts of inhibitor and 1-3 parts of hydrogen-containing silicone oil, and component B comprises 100 parts of vinyl silicone oil and 1-3 parts of catalyst, in parts by mass.

[0006] In one embodiment, the conductive filler includes stainless steel fibers and / or carbon nanotubes.

[0007] In one embodiment, the length of the carbon nanotubes is 0.5-2 μm.

[0008] In one embodiment, the nano soft magnetic filler includes nano crystals and / or Permalloy.

[0009] In one embodiment, the particle size of the nano soft magnetic filler is 30-150 nm.

[0010] In one embodiment, the silane coupling agent includes at least one of vinyl trimethoxy silane, vinyl triethoxy silane, and vinyl tri(β-methoxyethoxy) silane.

[0011] In one embodiment, the hydrogen content of the hydrogen-containing silicone oil is 0.5-1.5%.

[0012] In one embodiment, the inhibitor includes at least one of acetylene cyclohexanol, 2-methyl-3-butyn-2-ol, and 3-methyl-1-dodecyn-3-ol.

[0013] In one embodiment, the catalyst comprises a platinum catalyst.

[0014] In addition, to achieve the above-mentioned purpose, the present application also provides a method for preparing an organosilicon potting compound, which is used to prepare the organosilicon potting compound as described above, and the method for preparing the organosilicon potting compound comprises the following steps:

[0015] Vinyl silicone oil, silane coupling agent, conductive filler, inhibitor and hydrogen-containing silicone oil are taken according to mass parts, mixed evenly, and then nano soft magnetic filler is added, and after uniform dispersion, component A is prepared;

[0016] Vinyl silicone oil and catalyst are mixed evenly according to the mass fractions to obtain component B;

[0017] Equal amounts of the component A and the component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0018] The silicone potting compound provided by the present application includes component A and component B. In terms of mass fractions, component A includes 100 parts of vinyl silicone oil, 2-5 parts of silane coupling agent, 10-22 parts of conductive filler, 18-30 parts of nano soft magnetic filler, 0.5-1.5 parts of inhibitor and 1-3 parts of hydrogen-containing silicone oil; component B includes 100 parts of vinyl silicone oil and 1-3 parts of catalyst. The conductive filler in component A can enhance the conductivity and provide certain electromagnetic shielding performance. The nano soft magnetic filler can form a magnetic conductive path in the potting compound to guide the magnetic lines of force generated by the electronic devices in contact with the potting compound, providing strong electromagnetic shielding performance. The silane coupling agent can enhance the compatibility between the conductive filler and the nano soft magnetic filler and the vinyl silicone oil, and promote the uniform dispersion of the conductive filler and the nano soft magnetic filler. Therefore, the present application greatly improves the electromagnetic shielding performance of the potting compound under the synergistic effect of the conductive filler and the nano soft magnetic filler. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present drawings or related technologies, the drawings required for use in the embodiments or related technical descriptions will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present drawings. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying any creative work.

[0020] Figure 1 The figure is a schematic diagram of the process of preparing the organic silicone potting compound according to the embodiment of the present application.

[0021] The realization of the purpose, functional features and advantages of this application will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION

[0022] It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0023] Hereinafter, the embodiments of the silicone potting compound and the preparation method thereof of the present application are specifically disclosed in detail with appropriate reference to the accompanying drawings. However, there may be cases where unnecessary detailed descriptions are omitted. For example, there are cases where detailed descriptions of well-known matters and repeated descriptions of actually the same structures are omitted. This is to avoid the following description from becoming unnecessarily lengthy and to facilitate the understanding of those skilled in the art. In addition, the drawings and the following descriptions are provided for those skilled in the art to fully understand the present application and are not intended to limit the subject matter described in the claims.

[0024] "Scope" disclosed in the present application is limited in the form of lower limit and upper limit, and a given range is limited by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundary of a special range. The scope limited in this way can be including end values ​​or not including end values, and can be arbitrarily combined, that is, any lower limit can be combined with any upper limit to form a scope. For example, if the scope of 60-120 and 80-110 is listed for a specific parameter, it is understood that the scope of 60-110 and 80-120 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following scope can be all expected: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In the present application, unless otherwise specified, the numerical range "ab" represents the abbreviation of any real number combination between a and b, wherein a and b are real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" are listed in this document, and "0-5" is just an abbreviation of these numerical combinations. In addition, when a parameter is expressed as an integer ≥ 2, it is equivalent to disclosing that the parameter is, for example, an integer of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0025] Unless otherwise specified, all embodiments and optional embodiments of the present application can be combined with each other to form a new technical solution.

[0026] Unless otherwise specified, all technical features and optional technical features of this application can be combined with each other to form a new technical solution.

[0027] If there is no special explanation, all steps of the present application can be performed sequentially or randomly, preferably sequentially. For example, the method includes steps (a) and (b), which means that the method may include steps (a) and (b) performed sequentially, or may include steps (b) and (a) performed sequentially. For example, the method may further include step (c), which means that step (c) may be added to the method in any order. For example, the method may include steps (a), (b) and (c), or may include steps (a), (c) and (b), or may include steps (c), (a) and (b), etc.

[0028] If there is no special explanation, the "include" and "comprising" mentioned in this application are open-ended or closed-ended. For example, the "include" and "comprising" may mean that other components not listed may also be included or only the listed components may be included or only the listed components may be included.

[0029] If not specifically stated, in this application, the term "or" is inclusive. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, any of the following conditions satisfies the condition "A or B": A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0030] In order to make the above-mentioned purposes, features and advantages of the present application more obvious and understandable, the technical solution of the present application is further described below in conjunction with the accompanying drawings and embodiments. However, the present application is not limited to the listed embodiments, and should also include any other known changes within the scope of the rights claimed in the present application.

[0031] First, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present application. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.

[0032] The embodiment of the present application provides a silicone potting compound, including component A and component B. In parts by mass, component A includes 100 parts of vinyl silicone oil, 2-5 parts of silane coupling agent, 10-22 parts of conductive filler, 18-30 parts of nano soft magnetic filler, 0.5-1.5 parts of inhibitor and 1-3 parts of hydrogen-containing silicone oil; component B includes 100 parts of vinyl silicone oil and 1-3 parts of catalyst.

[0033] Vinyl silicone oil is a basic polymer in silicone potting adhesive. It is understandable that this embodiment is based on 100 parts by mass of vinyl silicone oil.

[0034] Conductive filler is a filler with electrical conductivity. It can improve the electrical conductivity when added to the silicone potting compound. The amount of conductive filler added in this embodiment is 10-22 parts, for example, 10 parts, 13 parts, 15 parts, 18 parts, 20 parts, 22 parts, etc. It can be understood that if the amount of conductive filler added is too little, the conductivity of the silicone potting compound is poor and it cannot effectively play the role of electromagnetic shielding; if the amount of conductive filler added is too much, it is difficult to disperse evenly in the silicone potting compound, and even the properties of the silicone potting compound are changed. By controlling the amount of conductive filler added within the above range, a certain degree of electrical conductivity can be obtained without having a significant impact on the dispersion of substances in the silicone potting compound.

[0035] In some feasible embodiments, the conductive fillers that can be used include stainless steel fibers and / or carbon nanotubes. It is understandable that both stainless steel fibers and carbon nanotubes have good electrical conductivity, and both have thermal conductivity and good heat dissipation performance. Specifically, the length of the carbon nanotubes used can be 0.5-2 μm, for example, 0.5 μm, 1.8 μm, 1 μm, 1.5 μm, 1.8 μm, 2 μm, etc. The surface of the carbon nanotube can be loaded with nano soft magnetic fillers, and the longer the length, the more nano soft magnetic fillers can be loaded to form a magnetic conductive path.

[0036] Nano soft magnetic filler refers to nano materials with soft magnetic properties. After being added to the silicone potting compound, it can improve the magnetic conductivity and provide good electromagnetic shielding performance. In this embodiment, the amount of nano soft magnetic filler added is 18-30 parts, for example, 18 parts, 20 parts, 25 parts, 28 parts, 30 parts, etc. It can be understood that if the amount of nano soft magnetic filler added is too little, the magnetic conductivity of the silicone potting compound is insufficient; if the amount of nano soft magnetic filler added is too much, it is difficult to evenly disperse in the silicone potting compound. By controlling the amount of nano soft magnetic filler added within the above range, good magnetic conductivity can be obtained, providing a good electromagnetic shielding effect for electronic devices.

[0037] In some feasible embodiments, the nano soft magnetic filler that can be used includes nano crystals and / or Permalloy. Specifically, Permalloy can be prepared into nano Permalloy powder. In the silicone potting system, a part of the added nano soft magnetic filler can be loaded on the stainless steel fiber and the carbon nanotube, and the other part is dispersed in the vinyl silicone oil. The nano soft magnetic filler loaded on the stainless steel fiber and the carbon nanotube is further dispersed in the vinyl silicone oil by the stainless steel fiber and the carbon nanotube to form a three-dimensional magnetic conductive network, thereby enhancing the magnetic conductive performance when the added amount is certain.

[0038] Silane coupling agents can enhance the bonding between organic and inorganic matrices. In this embodiment, the conductive filler and the nano soft magnetic filler are inorganic materials. Adding silane coupling agents can promote their uniform dispersion in the silicone potting system. In some feasible embodiments, the usable silane coupling agent includes at least one of vinyl trimethoxy silane, vinyl triethoxy silane, and vinyl tri (β-methoxyethoxy) silane.

[0039] Hydrogen-containing silicone oil can be used as a crosslinking agent. In some feasible embodiments, the hydrogen content of the hydrogen-containing silicone oil in this embodiment is 0.5-1.5%, for example, 0.5%, 0.8%, 1.0%, 1.2%, 1.5%. It is understandable that the hydrogen content of the hydrogen-containing silicone oil will affect the mechanical properties of the silicone potting compound. The higher the hydrogen content, the greater the crosslinking density, the increased tensile strength and hardness, and the reduced elongation at break. By controlling the hydrogen content of the hydrogen-containing silicone oil within the above range, a silicone potting compound with good mechanical properties can be obtained.

[0040] Inhibitors can control the reaction speed, and catalysts can speed up the reaction speed. In the present embodiment, the addition amount of the inhibitor is 0.5-2 parts, for example, 0.5 parts, 0.8 parts, 1 parts, 1.3 parts, 1.5 parts, 1.8 parts, 2 parts, etc. In the present embodiment, the addition amount of the catalyst is 1-3 parts, for example, 1 parts, 1.3 parts, 1.5 parts, 1.8 parts, 2 parts, 2.3 parts, 2.5 parts, 2.7 parts, 3 parts, etc. Inhibitors and catalysts belong to different components respectively, and mixing in the process of preparing silicone potting glue can effectively regulate the reaction process. In some feasible embodiments, the inhibitor that can be used includes at least one of acetylene cyclohexanol, 2-methyl-3-butyne-2-ol, and 3-methyl-1-dodecyne-3-ol, and the catalyst includes a platinum catalyst, such as chloroplatinic acid.

[0041] In this embodiment, the silicone potting compound includes component A and component B. In terms of mass fraction, component A includes 100 parts of vinyl silicone oil, 2-5 parts of silane coupling agent, 10-22 parts of conductive filler, 18-30 parts of nano soft magnetic filler, 0.5-1.5 parts of inhibitor and 1-3 parts of hydrogen-containing silicone oil; component B includes 100 parts of vinyl silicone oil and 1-3 parts of catalyst. The conductive filler in component A can enhance the conductivity and provide certain electromagnetic shielding performance. The nano soft magnetic filler can form a magnetic conductive path in the potting compound to guide the magnetic lines of force generated by the electronic devices in contact with the potting compound, providing strong electromagnetic shielding performance. The silane coupling agent can enhance the compatibility between the conductive filler and the nano soft magnetic filler and the vinyl silicone oil, and promote the uniform dispersion of the conductive filler and the nano soft magnetic filler. Therefore, the present application greatly improves the electromagnetic shielding performance of the potting compound under the synergistic effect of the conductive filler and the nano soft magnetic filler.

[0042] The present application also provides a method for preparing an organic silicone potting compound. In this embodiment, the method for preparing the organic silicone potting compound comprises:

[0043] Step S10, taking vinyl silicone oil, silane coupling agent, conductive filler, inhibitor and hydrogen silicone oil according to mass fractions, mixing them evenly, adding nano soft magnetic filler, and preparing component A after evenly dispersing them;

[0044] Step S20, mixing the vinyl silicone oil and the catalyst in parts by mass to obtain component B;

[0045] Step S30, taking equal amounts of the component A and the component B, mixing them, and subjecting them to vacuum degassing treatment to obtain the silicone potting adhesive.

[0046] It is understandable that among the above-mentioned raw materials, the nano soft magnetic filler can be used to prepare component A after annealing. Different raw materials are added to the vinyl silicone oil in sequence so that the conductive filler and the nano soft magnetic filler can be evenly dispersed. And the conductive filler is added before the nano soft magnetic filler, and the larger conductive filler is dispersed first, so that the nano soft magnetic filler can not only be evenly dispersed in the vinyl silicone oil matrix after being added, but also can be loaded on the conductive filler.

[0047] In the silicone potting compound prepared in this embodiment, the conductive filler in component A can enhance the conductivity and provide certain electromagnetic shielding performance. The nano soft magnetic filler can form a magnetic conductive path in the potting compound to guide the magnetic lines of force generated by the electronic devices in contact with the potting compound, thereby providing stronger electromagnetic shielding performance. The silane coupling agent can enhance the compatibility between the conductive filler and the nano soft magnetic filler and the vinyl silicone oil, and promote the uniform dispersion of the conductive filler and the nano soft magnetic filler. Therefore, under the synergistic effect of the conductive filler and the nano soft magnetic filler, the electromagnetic shielding performance of the potting compound is greatly improved in this application.

[0048] The present application is described in detail below with reference to specific embodiments and comparative examples, but they should not be construed as limiting the scope of protection of the present application.

[0049] Example 1

[0050] Take 100 parts of vinyl silicone oil, 3 parts of silane coupling agent, 15 parts of conductive filler, 1.5 parts of inhibitor and 2 parts of hydrogen-containing silicone oil (hydrogen content 1%), mix them evenly, add 25 parts of nano soft magnetic filler, and prepare component A after uniform dispersion;

[0051] Take 100 parts of vinyl silicone oil and 2 parts of catalyst and mix them evenly to obtain component B;

[0052] Equal amounts of component A and component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0053] Example 2

[0054] Take 100 parts of vinyl silicone oil, 2 parts of silane coupling agent, 10 parts of conductive filler, 1.5 parts of inhibitor and 2 parts of hydrogen-containing silicone oil (hydrogen content 1%), mix them evenly, add 18 parts of nano soft magnetic filler, and prepare component A after uniform dispersion;

[0055] Take 100 parts of vinyl silicone oil and 2 parts of catalyst and mix them evenly to obtain component B;

[0056] Equal amounts of component A and component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0057] Example 3

[0058] Take 100 parts of vinyl silicone oil, 5 parts of silane coupling agent, 22 parts of conductive filler, 1.5 parts of inhibitor and 2 parts of hydrogen-containing silicone oil (hydrogen content 1%), mix them evenly, add 30 parts of nano soft magnetic filler, and prepare component A after uniform dispersion;

[0059] Take 100 parts of vinyl silicone oil and 2 parts of catalyst and mix them evenly to obtain component B;

[0060] Equal amounts of component A and component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0061] Example 4

[0062] Take 100 parts of vinyl silicone oil, 3 parts of silane coupling agent, 20 parts of conductive filler, 1.5 parts of inhibitor and 2 parts of hydrogen-containing silicone oil (hydrogen content 1%), mix them evenly, add 28 parts of nano soft magnetic filler, and prepare component A after uniform dispersion;

[0063] Take 100 parts of vinyl silicone oil and 2 parts of catalyst and mix them evenly to obtain component B;

[0064] Equal amounts of component A and component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0065] Comparative Example 1

[0066] 100 parts of vinyl silicone oil, 3 parts of silane coupling agent, 1.5 parts of inhibitor and 2 parts of hydrogen-containing silicone oil (hydrogen content 1%) are uniformly dispersed to prepare component A;

[0067] Take 100 parts of vinyl silicone oil and 2 parts of catalyst and mix them evenly to obtain component B;

[0068] Equal amounts of component A and component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0069] Comparative Example 2

[0070] 100 parts of vinyl silicone oil, 3 parts of silane coupling agent, 20 parts of conductive filler, 1.5 parts of inhibitor and 2 parts of hydrogen-containing silicone oil (hydrogen content 1%) are uniformly dispersed to prepare component A;

[0071] Take 100 parts of vinyl silicone oil and 2 parts of catalyst and mix them evenly to obtain component B;

[0072] Equal amounts of component A and component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0073] Comparative Example 3

[0074] Take 100 parts of vinyl silicone oil, 3 parts of silane coupling agent, 1.5 parts of inhibitor and 2 parts of hydrogen-containing silicone oil (hydrogen content 1%), mix them evenly, add 28 parts of nano soft magnetic filler, and prepare component A after uniform dispersion;

[0075] Take 100 parts of vinyl silicone oil and 2 parts of catalyst and mix them evenly to obtain component B;

[0076] Equal amounts of component A and component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

[0077] The silicone potting adhesives of Examples 1-4 and Comparative Examples 1-3 were potted into electronic devices of the same model and specification, and the same voltage was applied to perform a radio frequency electromagnetic field shielding effectiveness test, and the test results shown in Table 1 below were obtained.

[0078] Table 1

[0079]

[0080]

[0081] It can be seen from the results in Table 1 that the silicone potting adhesives of Examples 1-4 of the present application all have excellent electromagnetic shielding performance, while Comparative Example 1 without adding conductive fillers and nano-soft magnetic fillers has almost no electromagnetic shielding performance, and the simultaneous addition of conductive fillers and nano-soft magnetic fillers can play a synergistic role and improve the electromagnetic shielding performance to a greater extent.

[0082] The serial numbers of the above-mentioned embodiments of the present application are for description only and do not represent the advantages or disadvantages of the embodiments.

[0083] The above are only preferred embodiments of the present application, and are not intended to limit the patent scope of the present application. Any equivalent structure or equivalent process transformation made using the contents of the present application specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present application.

Claims

1. A silicone potting compound, characterized in that: The organic silicone potting compound comprises component A and component B. In parts by mass, component A comprises 100 parts of vinyl silicone oil, 2-5 parts of silane coupling agent, 10-22 parts of conductive filler, 18-30 parts of nano soft magnetic filler, 0.5-2 parts of inhibitor and 1-3 parts of hydrogen-containing silicone oil; component B comprises 100 parts of vinyl silicone oil and 1-3 parts of catalyst.

2. The organic silicone potting adhesive according to claim 1, characterized in that: The conductive filler includes stainless steel fibers and / or carbon nanotubes.

3. The organic silicone potting adhesive according to claim 2, characterized in that: The length of the carbon nanotubes is 0.5-2 μm.

4. The organic silicone potting adhesive according to claim 1, characterized in that: The nano soft magnetic filler includes nano crystals and / or Permalloy.

5. The organic silicone potting adhesive according to claim 4, characterized in that: The particle size of the nano soft magnetic filler is 30-150nm.

6. The organic silicone potting adhesive according to claim 1, characterized in that: The silane coupling agent includes at least one of vinyl trimethoxy silane, vinyl triethoxy silane and vinyl tri (β-methoxyethoxy) silane.

7. The organic silicone potting adhesive according to claim 1, characterized in that: The hydrogen content of the hydrogen-containing silicone oil is 0.5-1.5%.

8. The organic silicone potting adhesive according to claim 1, characterized in that: The inhibitor includes at least one of acetylene cyclohexanol, 2-methyl-3-butyn-2-ol, and 3-methyl-1-dodecyn-3-ol.

9. The organic silicone potting adhesive according to claim 1, characterized in that: The catalyst includes a platinum catalyst.

10. A method for preparing a silicone potting compound, characterized in that: For preparing the organic silicone potting adhesive according to any one of claims 1 to 9, the preparation method of the organic silicone potting adhesive comprises the following steps: Vinyl silicone oil, silane coupling agent, conductive filler, inhibitor and hydrogen-containing silicone oil are taken according to mass parts, mixed evenly, and then nano soft magnetic filler is added, and after uniform dispersion, component A is prepared; Vinyl silicone oil and catalyst are mixed evenly according to the mass fractions to obtain component B; Equal amounts of the component A and the component B are mixed and subjected to vacuum degassing to obtain the silicone potting adhesive.

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