Organic silicon resin with low dielectric loss as well as preparation method and coating composition thereof

Abstract

The invention is applicable to the technical field of materials, and provides low-dielectric-loss organic silicon resin and a preparation method and a coating composition thereof, and the preparation method comprises the following steps: mixing bis (dimethylsilyl) benzene and platinum carbon powder, heating to 85 DEG C, continuously dropwise adding trivinyl phenyl silane, reacting for 1-1.5 hours at the temperature of 90-100 DEG C, and cooling to room temperature to obtain the low-dielectric-loss organic silicon resin. And adding activated carbon, stirring, filtering, and concentrating under reduced pressure to obtain the organic silicon resin with low dielectric loss. By virtue of the advantage of low dielectric constant of the organic silicon resin, the signal transmission quality and speed can be remarkably improved, and the harsh requirement of high-frequency and high-speed communication on the dielectric property of a material can be met; and secondly, by virtue of the characteristic of low dielectric loss, the conversion from electric energy to heat energy can be reduced to the greatest extent under the action of an electric field, so that the energy consumption can be reduced, the energy utilization efficiency can be improved, and the material performance reduction and equipment failure caused by heating can be effectively avoided.

Description

Technical Field

[0001] The present application belongs to the field of material technology, and in particular relates to a low dielectric loss organic silicon resin and a preparation method and a coating composition thereof. Background Art

[0002] With the rapid development of modern communication technology, the advent of the 5G and 6G high-frequency and high-speed communication era, and the continued growth in the demand for Internet information transmission, the demand for materials that can support high frequency and high speed and have low dielectric constant and low dielectric loss characteristics has become extremely urgent. In the field of large-capacity communication of image information, fast and accurate transmission of signals is the key to ensuring smooth playback of high-definition video and real-time sharing of big data.

[0003] In traditional communication technology and material applications, there are many factors that limit the current development of communication: First, the dielectric properties are limited. Some existing communication materials have a high dielectric constant, which will cause serious signal attenuation during high-frequency signal transmission. When the signal frequency increases, the high dielectric constant causes the electric field to produce a large polarization effect inside the material, consuming a large amount of signal energy, thereby reducing the transmission distance and quality of the signal. For example, in early communication cables, due to the use of insulating materials with relatively high dielectric constants, as the communication frequency increases, the signal loss problem becomes more prominent, limiting the communication speed and coverage. Dielectric loss is also a thorny issue. High dielectric loss means that the material will convert part of the electrical energy into heat energy under the action of the electric field, which not only causes energy waste, but also increases the material temperature, affecting the stability and life of the equipment. For high-frequency and high-speed communication circuit boards, excessive dielectric loss can cause signal distortion and interfere with the normal operation of other electronic components.

[0004] Therefore, developing a material with low dielectric constant and low dielectric loss is of great significance for meeting the needs of 5G and 6G high-frequency and high-speed communications and large-capacity communications of Internet image information, and promoting the development of application fields such as light-emitting diodes and high-speed transmission. Summary of the invention

[0005] The purpose of the embodiments of the present application is to provide a method for preparing a low dielectric loss silicone resin, aiming to solve the problem that existing communication materials have high dielectric constants and severe dielectric losses, which affect the stability and life of the equipment.

[0006] The embodiment of the present application is implemented as follows: a method for preparing a low dielectric loss silicone resin comprises:

[0007] Mix (bisdimethylsilyl)benzene and platinum carbon powder, heat to 85°C, continue to drop trivinylphenylsilane, and react at 90-100°C for 1-1.5 hours, add activated carbon, stir, filter, and concentrate under reduced pressure to obtain a silicone resin with low dielectric loss.

[0008] Another object of an embodiment of the present application is to provide a low dielectric loss coating composition, wherein the coating composition comprises the above-mentioned low dielectric loss silicone resin.

[0009] Another object of an embodiment of the present application is to provide a low dielectric loss coating composition, wherein the coating composition comprises the above-mentioned low dielectric loss silicone resin.

[0010] In the embodiment of the present application, after (bisdimethylsilyl)benzene, platinum carbon powder and trivinylphenylsilane are fully reacted under specific conditions, activated carbon is added for stirring, filtering, and decompression concentration treatment, and the obtained silicone resin has the characteristics of low dielectric constant and low dielectric loss. Among them, the silicone resin of the present application can significantly improve the transmission quality and speed of signals by virtue of its low dielectric constant, and meet the stringent requirements of high-frequency and high-speed communication on the dielectric properties of materials; secondly, by virtue of its low dielectric loss characteristics, it can minimize the conversion of electrical energy into thermal energy under the action of an electric field, which not only helps to reduce energy consumption and improve energy utilization efficiency, but also effectively avoids material performance degradation and equipment failure caused by heat. DETAILED DESCRIPTION

[0011] In order to make the purpose, technical solution and advantages of the present application more clear, the present application is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described here are only used to explain the present application and are not used to limit the present application.

[0012] The present application embodiment provides a method for preparing a low dielectric loss organic silicone resin, comprising:

[0013] Mix (bisdimethylsilyl)benzene and platinum carbon powder, heat to 85°C, continue to drop trivinylphenylsilane, and react at 90-100°C for 1-1.5 hours, add activated carbon, stir, filter, and concentrate under reduced pressure to obtain a silicone resin with low dielectric loss.

[0014] In the embodiment of the present application, the mass ratio of (bisdimethylsilyl)benzene, platinum carbon powder and trivinylphenylsilane is (260-265): (3.5-4.5): (26-30).

[0015] In the embodiment of the present application, the mass ratio of the platinum carbon powder to the activated carbon is (3.5-4.5):(1.5-2.5).

[0016] In the embodiment of the present application, the mass fraction of the platinum carbon powder is 5%.

[0017] The embodiment of the present application also provides a low dielectric loss organosilicon resin, and the low dielectric loss organosilicon resin is prepared by the above-mentioned method for preparing the low dielectric loss organosilicon resin.

[0018] An embodiment of the present application also provides a low dielectric loss coating composition, wherein the coating composition includes the above-mentioned low dielectric loss silicone resin.

[0019] In the embodiment of the present application, the coating composition includes the following raw materials in parts by weight:

[0020] 70-80 parts of the above-mentioned low dielectric loss organic silicon resin, 112-118 parts of organic siloxane with a vinylbenzene mass fraction of 0, 8-10 parts of polysiloxane with a vinylbenzene mass fraction of 0.5, 0.0002-0.0004 parts of platinum-vinylbenzene silazane and 0.06-0.08 parts of 1-ethynylbenzene cycloethanol.

[0021] In the embodiments of the present application, the coating composition may be combined with ingredients such as antioxidants and inorganic fillers as needed.

[0022] In the cured product obtained by curing the low dielectric loss coating composition described in the present application, the addition reaction of the silicone resin may leave unconverted carbon-carbon double bonds, and these unsaturated bonds are prone to atmospheric oxidation, resulting in degradation of coating performance. By introducing hindered phenolic, sulfur-containing or methylene-bridged antioxidants (such as 2,6-di-tert-butyl-4-methylphenol, 2,5-di-tert-amylhydroquinone, etc.), the oxidation reaction can be effectively inhibited by free radical capture, metal chelation and synergistic enhancement mechanisms. The amount of antioxidant is 1~10000ppm (preferably 1000ppm) based on the mass of the silicone resin. This range can ensure that the free radical scavenging rate is ≥95% and maintain optical and dielectric properties such as transmittance ≥92%, tanδ≤0.0025, and avoid coloring (ΔE<2) or white turbidity caused by excessive use. This application achieves a balance between thermal stability and processing performance while inhibiting oxidation by precisely controlling the residual double bond concentration (0.05~0.1mmol / g) and developing a special compound system, significantly improving the long-term reliability of the coating.

[0023] The low dielectric loss coating composition described in this application can flexibly adjust the rheological properties according to application requirements while maintaining a dielectric constant of ≤2.8 through optimized formula design: by adding inorganic fillers such as nano-silica, fused silica, and crystalline silica (particle size 5-100nm, addition amount 5-30wt%), the viscosity of the composition can be effectively regulated (100-5000mPa・s), and the construction processability can be improved; the coating formed after curing has excellent mechanical properties. In particular, when surface-modified titanium oxide or aluminum oxide (the modifier is 3-glycidyloxypropyltrimethoxysilane) is added, the system can be evenly dispersed, with a dispersion of more than 98%, effectively inhibiting agglomeration, so that the coating can maintain low dielectric loss while increasing the photoluminescence efficiency by 15-20%, which is suitable for high-end display fields such as Mini LED backlight modules.

[0024] The following is a detailed description of the low dielectric loss silicone resin and its preparation method and coating composition with specific examples, as shown below. The experimental methods used in the following examples are conventional methods unless otherwise specified; the materials, reagents, etc. used can be obtained from commercial sources unless otherwise specified.

[0025] Example 1

[0026] The preparation method of low dielectric loss silicone resin is as follows:

[0027] Mix 260 g (1.35 mol) of (bisdimethylsilyl)benzene and 3.5 g of 5% platinum carbon powder, heat to 85°C, then dropwise add 26 g of trivinylphenylsilane, and react at 95°C for 1.5 hours. Then, add 1.5 g of activated carbon, stir, filter, and concentrate under reduced pressure to obtain 99 g of low dielectric loss silicone resin (colorless and transparent, yield 80%).

[0028] The preparation method of the coating composition with low dielectric loss is:

[0029] Weigh the raw materials according to the following formula: 70 parts of the above-mentioned low dielectric loss silicone resin, 112 parts of organosiloxane with a vinylbenzene mass fraction of 0, 8-10 parts of polysiloxane with a vinylbenzene mass fraction of 0.5, 0.0002 parts of platinum-vinylbenzene silazane and 0.06 parts of 1-ethynylbenzene cycloethanol;

[0030] The above raw materials are mixed evenly to prepare a coating, and then cured at 150° C. for 4 hours to form a coating cured product.

[0031] Example 2

[0032] The preparation method of low dielectric loss silicone resin is as follows:

[0033] Mix 261 g (1.35 mol) of (bisdimethylsilyl)benzene and 3.7 g of 5% platinum carbon powder, heat to 85°C, then dropwise add 27 g of trivinylphenylsilane, and react at 95°C for 1.5 hours. Then, add 1.7 g of activated carbon, stir, filter, and concentrate under reduced pressure to obtain 99 g of low dielectric loss silicone resin (colorless and transparent, yield 82%).

[0034] The preparation method of the coating composition with low dielectric loss is:

[0035] Weigh the raw materials according to the following formula: 72 parts of the above-mentioned low dielectric loss silicone resin, 114 parts of organosiloxane with a vinylbenzene mass fraction of 0, 9 parts of polysiloxane with a vinylbenzene mass fraction of 0.5, 0.0002 parts of platinum-vinylbenzene silazane and 0.06 parts of 1-ethynylbenzene cycloethanol;

[0036] The above raw materials are mixed evenly to prepare a coating, and then cured at 150° C. for 4 hours to form a coating cured product.

[0037] Example 3

[0038] The preparation method of low dielectric loss silicone resin is as follows:

[0039] 263 g (1.35 mol) of (bisdimethylsilyl)benzene was mixed with 4.15 g of 5% platinum carbon powder, heated to 85°C, and then 28 g of trivinylphenylsilane was added dropwise. After reacting at 95°C for 1.5 hours, 2 g of activated carbon was added, stirred, filtered, and concentrated under reduced pressure to obtain 99 g of low dielectric loss silicone resin (colorless and transparent, yield 87%).

[0040] The preparation method of the coating composition with low dielectric loss is:

[0041] Weigh the raw materials according to the following formula: 75 parts of the above-mentioned low dielectric loss silicone resin, 115 parts of organosiloxane with a vinylbenzene mass fraction of 0, 9 parts of polysiloxane with a vinylbenzene mass fraction of 0.5, 0.0003 parts of platinum-vinylbenzene silazane and 0.07 parts of 1-ethynylbenzene cycloethanol;

[0042] The above raw materials are mixed evenly to prepare a coating, and then cured at 150° C. for 4 hours to form a coating cured product.

[0043] Example 4

[0044] The preparation method of low dielectric loss silicone resin is as follows:

[0045] 264 g (1.35 mol) of (bisdimethylsilyl)benzene was mixed with 4.3 g of 5% platinum carbon powder, heated to 85°C, and then 29 g of trivinylphenylsilane was added dropwise. After reacting at 95°C for 1.5 hours, 2.3 g of activated carbon was added, stirred, filtered, and concentrated under reduced pressure to obtain 99 g of low dielectric loss silicone resin (colorless and transparent, yield 84%).

[0046] The preparation method of the coating composition with low dielectric loss is:

[0047] Weigh the raw materials according to the following formula: 77 parts of the above-mentioned low dielectric loss silicone resin, 116 parts of organosiloxane with a vinylbenzene mass fraction of 0, 10 parts of polysiloxane with a vinylbenzene mass fraction of 0.5, 0.0003 parts of platinum-vinylbenzene silazane and 0.08 parts of 1-ethynylbenzene cycloethanol;

[0048] The above raw materials are mixed evenly to prepare a coating, and then cured at 150° C. for 4 hours to form a coating cured product.

[0049] Example 5

[0050] The preparation method of low dielectric loss silicone resin is as follows:

[0051] Mix 265 g (1.35 mol) of (bisdimethylsilyl)benzene and 4.5 g of 5% platinum carbon powder, heat to 85°C, then dropwise add 30 g of trivinylphenylsilane, and react at 95°C for 1.5 hours. Then, add 2.5 g of activated carbon, stir, filter, and concentrate under reduced pressure to obtain 99 g of low dielectric loss silicone resin (colorless and transparent, yield 83%).

[0052] The preparation method of the coating composition with low dielectric loss is:

[0053] Weigh the raw materials according to the following formula: 80 parts of the above-mentioned low dielectric loss silicone resin, 118 parts of organosiloxane with a vinylbenzene mass fraction of 0, 10 parts of polysiloxane with a vinylbenzene mass fraction of 0.5, 0.0004 parts of platinum-vinylbenzene silazane and 0.08 parts of 1-ethynylbenzene cycloethanol;

[0054] The above raw materials are mixed evenly to prepare a coating, and then cured at 150° C. for 4 hours to form a coating cured product.

[0055] The hardness, dielectric constant and dielectric loss of the cured coatings prepared in the above Examples 1-5 were tested, wherein the coating hardness was tested using a Shore D durometer in the Shore Hardness Test, and the hardness value was calculated by measuring the depth of the indenter pressed into the coating surface under a specified load (Shore D type is 584.8g) according to the ASTM D2240 standard; the dielectric constant and dielectric loss of the coating were tested using the parallel plate capacitor method based on the ASTM D150 standard. The test results are shown in Table 1.

[0056] Table 1

[0057]

[0058] In summary, the low dielectric constant insulating coating material described in this application has a colorless and transparent appearance, a hardness of Shore D52-D55, a dielectric constant as low as 2.3-2.7, a dielectric loss of only 0.001-0.002, and excellent properties such as high transparency (transmittance ≥ 92%) and medium rigidity (D55). It can effectively reduce high-frequency signal attenuation and is suitable for 5G / 6G electronic components, Mini LED packaging and high temperature resistant scenarios. Through formula optimization, a synergistic breakthrough in optical, mechanical and electrical properties has been achieved.

[0059] The above-mentioned embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the present application. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the attached claims.

[0060] The above description is only a preferred embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present application should be included in the protection scope of the present application.

Claims

1. A method for preparing a low dielectric loss silicone resin, characterized in that: include: Mix (bisdimethylsilyl)benzene and platinum carbon powder, heat to 85°C, continue to drop trivinylphenylsilane, and react at 90-100°C for 1-1.5 hours, add activated carbon, stir, filter, and concentrate under reduced pressure to obtain a silicone resin with low dielectric loss.

2. The method for preparing a low dielectric loss organic silicone resin according to claim 1, characterized in that: The mass ratio of the (bisdimethylsilyl)benzene, platinum carbon powder and trivinylphenylsilane is (260-265): (3.5-4.5): (26-30).

3. The method for preparing a low dielectric loss silicone resin according to claim 1, characterized in that: The mass ratio of the platinum carbon powder to the activated carbon is (3.5-4.5):(1.5-2.5).

4. The method for preparing a low dielectric loss silicone resin according to claim 1, characterized in that: The mass fraction of the platinum carbon powder is 5%.

5. A low dielectric loss organic silicon resin, characterized in that: The low dielectric loss organic silicone resin is prepared by the preparation method of the low dielectric loss organic silicone resin according to any one of claims 1-4.

6. A coating composition with low dielectric loss, characterized in that: The coating composition comprises the low dielectric loss organic silicone resin according to claim 5.

7. The low dielectric loss coating composition according to claim 6, characterized in that: The coating composition comprises the following raw materials in parts by weight: 70-80 parts of the low dielectric loss silicone resin according to claim 5, 112-118 parts of an organosiloxane with a vinylbenzene mass fraction of 0, 8-10 parts of a polysiloxane with a vinylbenzene mass fraction of 0.5, 0.0002-0.0004 parts of platinum-vinylbenzene silazane and 0.06-0.08 parts of 1-ethynylbenzene cycloethanol.

8. The low dielectric loss coating composition according to claim 7, characterized in that: The coating composition also includes an antioxidant and an inorganic filler.

9. The low dielectric loss coating composition according to claim 8, characterized in that: The antioxidant is one or more of 2,6-di-tert-butyl-4-methylphenol and 2,5-di-tert-amylhydroquinone.

10. The low dielectric loss coating composition according to claim 8, characterized in that: The inorganic filler is one or more of nano-silicon dioxide, fused silicon dioxide, crystalline silicon dioxide, titanium oxide and aluminum oxide.

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