A high-rebound anti-damping silica gel material and a preparation method thereof

Abstract

The application belongs to the technical field of polymer compound compositions, and particularly relates to a high-rebound anti-damping silica gel material and a preparation method thereof. The preparation method of the high-rebound anti-damping silica gel material comprises the following steps: S1, methylphenyl vinyl silicone rubber and 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol are mixed for modification treatment to obtain modified silicone rubber; S2, the modified silicone rubber, white carbon black, aerogel, silicone oil and defoaming agent are mixed, heated and stirred, and then subjected to dense mixing treatment to obtain a mixed rubber; and S3, the mixed rubber is mixed with a vulcanizing agent and subjected to vulcanization treatment to obtain the high-rebound anti-damping silica gel material. The functional components jointly ensure high rebound and simultaneously reduce the thermal conductivity of the material.

Description

Technical Field

[0001] This invention belongs to the technical field of polymer compound compositions, specifically relating to a high-rebound, damping-resistant silicone material and its preparation method. Background Technology

[0002] Silicone rubber is an advanced synthetic material that combines the weather resistance of inorganic materials with the processing characteristics of organic polymers. Its main chain is composed of alternating Si-O bonds, with at least one organic group attached to each silicon atom. It is a typical semi-inorganic, semi-organic linear polymer elastomer. Compared to C-C bonds, the Si-O bonds in the silicone rubber main chain have higher bond energies, longer bond lengths, and larger bond angles, allowing for free rotation, diverse molecular conformations, weak intermolecular forces, and very flexible molecular chain movement. Therefore, silicone rubber possesses many superior properties that cannot be replaced by other organic polymers, such as high and low temperature resistance, electrical insulation, weather resistance, and high air permeability. Its unique molecular structure endows the material with excellent temperature resistance and physicochemical stability, making it widely used in aerospace, automotive, electronics, and medical fields.

[0003] High-rebound silicone material is an advanced polymer material that can quickly absorb impact energy and recover to its original form after being compressed or subjected to dynamic stress. Its core advantage lies in its excellent dynamic buffering performance and high rebound characteristics, which can provide efficient and reliable vibration reduction solutions under complex working conditions. It has the following characteristics: (1) High rebound and low hysteresis loss. It can quickly recover its original shape after being compressed, with a high dynamic recovery rate. While maintaining high rebound, it can effectively reduce energy loss, which is very suitable for high-frequency vibration environments; (2) Low compression set. Under long-term or high-frequency compression loads, the material can still maintain its original shape and is not prone to permanent deformation; (3) It has excellent oil resistance, ozone resistance, ultraviolet resistance and anti-aging properties, and can maintain structural stability in extreme oil environments or harsh outdoor working conditions.

[0004] Chinese patent (publication number CN117777944A) discloses a high-resilience thermally conductive insulating silicone and its preparation method. This high-resilience thermally conductive insulating silicone comprises the following components by weight: 4.5–25 parts vinyl polysiloxane; 0.2–5 parts hydrogen-containing polysiloxane; 0.01–1 part dispersant; 0.05–5 parts adhesive; 0.05–1 part catalyst; 0.01–1 part inhibitor; and 90–180 parts thermally conductive filler. This high-resilience thermally conductive insulating silicone is an addition-type, single-component, high-temperature, fast-curing adhesive with low viscosity, easy use, and environmental friendliness. It has high bulk strength, good adhesion to nickel-plated metals and PCBs, high resilience, and high resilience retention at high temperatures, reducing silicone residue in components during rework and protecting corresponding chip components. It also has a certain thermal conductivity. However, existing silicone materials require low thermal conductivity to block heat transfer while maintaining good resilience for safety in order to better apply them.

[0005] Therefore, there is an urgent need for a silicone material that uses silicone rubber as the matrix material, replaces thermally conductive fillers with thermally insulating fillers to ensure low thermal conductivity, and achieves high rebound and damping effects through multi-component synergy. Summary of the Invention

[0006] To address the shortcomings of existing technologies, the present invention aims to provide a high-rebound, damping silicone material and its preparation method. The invention first modifies methylphenyl vinyl silicone rubber by mixing it with 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol. Then, the modified silicone rubber, silica, aerogel, silicone oil, and defoamer are mixed, heated, and stirred, followed by intensive mixing to obtain a compound. Finally, the compound is mixed with a vulcanizing agent and vulcanized to obtain the high-rebound, damping silicone material. The combined effect of the functional components ensures high resilience while simultaneously reducing the material's thermal conductivity.

[0007] The technical solution adopted by the present invention to solve the above-mentioned technical problems is as follows: In a first aspect, the present invention provides a method for preparing a high-rebound, damping-resistant silicone material, comprising the following steps: S1. Methylphenyl vinyl silicone rubber and 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol were mixed and modified to obtain modified silicone rubber. S2. Mix modified silicone rubber, fumed silica, aerogel, silicone oil, and defoamer, heat and stir, and then perform intensive mixing to obtain a compound. S3. The compound rubber is mixed with a vulcanizing agent and then subjected to vulcanization treatment to obtain a high-rebound damping silicone material.

[0008] As a preferred technical solution of the present invention, the conditions for heating and stirring in step S2 are: temperature of 65~75℃ and time of 20~30min.

[0009] As a preferred technical solution of the present invention, the conditions for the internal mixing process in step S2 are as follows: heating to 100~110℃ and mixing for 90~100 min under a vacuum of -0.8MPa, followed by cooling and standing for 20~24 h.

[0010] As a preferred technical solution of the present invention, the vulcanization treatment conditions in step S3 are as follows: first vulcanize at 170~180℃ for 10~15min, and then vulcanize at 190~200℃ for 120~180min.

[0011] As a preferred technical solution of the present invention, each component includes, by weight: 80-90 parts modified silicone rubber, 15-25 parts fumed silica, 10-20 parts aerogel, 10-20 parts silicone oil, 1-2 parts vulcanizing agent, and 0.2-0.4 parts defoamer.

[0012] As a preferred embodiment of the present invention, the modified silicone rubber may be in the following weight proportions: 80 parts, 82 parts, 84 parts, 86 parts, 88 parts, or 90 parts, etc.

[0013] As a preferred embodiment of the present invention, the weight parts of the silica can be 15 parts, 17 parts, 19 parts, 21 parts, 23 parts, or 25 parts, etc.

[0014] As a preferred embodiment of the present invention, the aerogel may be in the following weight proportions: 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, or 20 parts, etc.

[0015] As a preferred embodiment of the present invention, the weight parts of the silicone oil may be 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, or 20 parts, etc.

[0016] As a preferred embodiment of the present invention, the weight parts of the vulcanizing agent may be 1.0 parts, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, or 2.0 parts, etc.

[0017] As a preferred embodiment of the present invention, the defoamer may be present in the following quantities: 0.2 parts, 0.3 parts, or 0.4 parts by weight.

[0018] As a preferred technical solution of the present invention, the modification treatment steps are as follows: by weight, 80-90 parts of methylphenyl vinyl silicone rubber are added to 400-500 parts of tetrahydrofuran and stirred for 50-60 minutes, then 4-6 parts of 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol are added and stirred for 30-40 minutes, then 0.6-0.8 parts of benzoin dimethyl ether are added and irradiated with 365nm wavelength light for 4-6 minutes. After the reaction is completed, 800-900 parts of anhydrous ethanol are added for flocculation, filtered, washed with anhydrous ethanol, and vacuum dried to obtain modified silicone rubber.

[0019] This invention uses methylphenyl vinyl silicone rubber and 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol as reactants and benzoin dimethyl ether as an initiator. Under ultraviolet light, benzoin dimethyl ether is excited to decompose and generate free radicals, thereby initiating the reaction between thiol groups and vinyl groups, and covalently grafting the triazine heterocycle onto the silicone rubber molecular chain, finally obtaining a modified silicone rubber with a triazine ring structure.

[0020] As a preferred embodiment of the present invention, the aerogel is a highly elastic aerogel powder.

[0021] As a preferred technical solution of the present invention, the preparation method of the high elasticity aerogel powder is as follows: an elastic treatment agent is prepared using 2-amino-4-hydroxy-6-methylpyrimidine and hexamethylene diisocyanate as raw materials, and the elastic treatment agent and amino-modified cellulose aerogel are mixed and stirred to obtain high elasticity aerogel powder.

[0022] As a preferred technical solution of the present invention, the preparation steps of the elastic treatment agent are as follows: by weight, 10-12 parts of 2-amino-4-hydroxy-6-methylpyrimidine are added to a reaction vessel under a nitrogen atmosphere, the temperature is raised to 40-50°C, 70-80 parts of hexamethylene diisocyanate and 2-3 parts of N-methylpyrrolidone are added, and the mixture is stirred at 90-100°C for 16-20 hours. Then, 50-60 parts of chloroform are added and stirred for 50-60 minutes. A mixture of 400-450 parts of n-heptane and 50-100 parts of isopropyl ether is added to precipitate the precipitate. The precipitate is filtered, washed with anhydrous ethanol, and dried to obtain the elastic treatment agent.

[0023] As a preferred technical solution of the present invention, the stirring reaction step is as follows: by weight, 10-20 parts of amino-modified cellulose aerogel and 15-25 parts of elastic treatment agent are added to 180-200 parts of chloroform, 0.2-0.4 parts of dibutyltin dilaurate are added under a nitrogen atmosphere and the temperature is raised to 50-60°C for stirring reaction for 2-4 hours. After the reaction is completed, the mixture is filtered, washed with anhydrous ethanol, dried, and pulverized to obtain high-elasticity aerogel powder.

[0024] This invention first uses 2-amino-4-hydroxy-6-methylpyrimidine and hexamethylene diisocyanate as raw materials. By reacting the amino group on the pyrimidine ring with the isocyanate group of hexamethylene diisocyanate, a highly reactive isocyanate group is grafted onto the pyrimidine molecule, thereby obtaining an elastic treatment agent. Subsequently, the amino group on the surface of the amino-modified cellulose aerogel reacts with the unreacted isocyanate group on the side chain of the elastic treatment agent under the catalysis of dibutyltin dilaurate, finally obtaining a highly elastic aerogel powder.

[0025] As a preferred embodiment of the present invention, the silicone oil is selected from one or more of dimethyl silicone oil, hydroxyl silicone oil, hydrogen-containing silicone oil, epoxy silicone oil, and amino silicone oil.

[0026] As a preferred embodiment of the present invention, the silicone oil is epoxy silicone oil and amino silicone oil.

[0027] As a preferred embodiment of the present invention, the mass ratio of the epoxy silicone oil to the amino silicone oil is (1~3):1.

[0028] As a preferred embodiment of the present invention, the epoxy silicone oil is an end-epoxy polyether silicone oil, wherein the molecular weight of the end-epoxy polyether silicone oil is 5000~10000 and the epoxy value is 0.01~0.03mol / 100g.

[0029] As a preferred embodiment of the present invention, the amino silicone oil is a fluorinated amino silicone oil, wherein the fluorinated amino silicone oil has a viscosity of 2000~5000 cps at 25°C and an ammonia value of 0.2~0.8%.

[0030] The silicone oil of the present invention is selected from dimethyl silicone oil, hydroxyl silicone oil, hydrogen-containing silicone oil, epoxy silicone oil, and amino silicone oil. Preferably, terminal epoxy polyether silicone oil and fluorinated amino silicone oil are compounded. By controlling the mass ratio of the two, a good synergistic effect is achieved, which effectively improves the comprehensive performance of silicone materials.

[0031] As a preferred embodiment of the present invention, the vulcanizing agent is dicumyl peroxide or benzoyl peroxide.

[0032] As a preferred embodiment of the present invention, the defoamer is triethanolamine.

[0033] A second aspect of the present invention provides a high-rebound, damping-resistant silicone material prepared by the preparation method described in the first aspect.

[0034] Compared with the prior art, the present invention has the following beneficial effects: (1) The modified silicone rubber of the present invention introduces a triazine ring structure, which replaces the dense short chain crosslinking point as a three-dimensional crosslinking node, increases the length of the flexible silicon-oxygen chain segment between the crosslinking points, and the chain segment can reversibly stretch under pressure to ensure high resilience; on the other hand, the CN bond of the triazine ring does not match the vibration mode of the Si-O bond and Si-C bond of silicone, forming a large number of phonon scattering sites on the molecular chain, interrupting the continuous thermal conduction path and reducing the thermal conductivity of the material.

[0035] (2) The pyrimidine heterocyclic polar groups contained in the high elasticity aerogel powder of the present invention can form a large number of reversible hydrogen bonds. Under external force, the hydrogen bonds dissociate and dissipate stress and are then rebuilt after unloading, thereby giving the material excellent resilience. In addition, the ultra-high porosity of cellulose aerogel can block solid-phase heat conduction by the internal air layer, and the rigid heterocyclic heterostructure of pyrimidine can also scatter phonons to cut off the continuous heat conduction path, thereby significantly reducing the thermal conductivity of the material.

[0036] (3) The low internal rotational steric hindrance of the epoxy polyether silicone oil in the compound silicone oil of the present invention provides elastic energy storage, and the low intermolecular forces of the fluorinated amino silicone oil weaken the inter-chain friction. Combined with the covalent flexible nodes in the network constructed by epoxy and amino groups, good resilience is achieved by reducing the heat loss during deformation. In addition, the long epoxy polyether chain is inserted into the cross-linked network of silicone rubber to break the regular and continuous thermally conductive long chain. The fluorinated silicone chain segment becomes an effective scattering center for phonon propagation by causing local microphase separation in the system, which synergistically reduces the thermal conductivity of the material. Attached Figure Description

[0037] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0038] Figure 1 The images show the FTIR spectra of the methylphenyl vinyl silicone rubber and the modified silicone rubber in Example 1. Detailed Implementation

[0039] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.

[0040] The sources of some components in the examples and comparative examples are as follows: Methylphenyl vinyl silicone rubber, model MY3120, was purchased from Anhui Mingyi Silicon Industry Co., Ltd. 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol, product number D155487, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. 2-Amino-4-hydroxy-6-methylpyrimidine, CAS No. 3977-29-5, was purchased from Shanghai Maclean Biochemical Technology Co., Ltd. Hexamethylene diisocyanate, CAS No. 822-06-0, was purchased from Shanghai Maclean Biochemical Technology Co., Ltd. N-Methylpyrrolidone, CAS No. 872-50-4, was purchased from Shanghai Maclean Biochemical Technology Co., Ltd. Amino-modified cellulose aerogel, product number Q0325437, purchased from Xi'an Qiyue Biotechnology Co., Ltd. The epoxy polyether silicone oil, model PPE-8K500, has a molecular weight of 9000 and an epoxy value of 0.0222mol / 100g, and was purchased from Shandong Dongyue Organosilicon Materials Co., Ltd. Fluorinated amino silicone oil, model DYSIL, viscosity at 25℃ is 3000cps, ammonia value is 0.5%, purchased from Shandong Dongyue Organosilicon Materials Co., Ltd. Dimethyl silicone oil, model MF-1000, was purchased from Shandong Dongyue Organosilicon Materials Co., Ltd. Silica, model 180H, purchased from Shandong Lihua New Materials Co., Ltd. Dicumyl peroxide, CAS No. 80-43-3, purchased from Sinopharm Chemical Reagent Co., Ltd. Benzoyl peroxide, CAS No. 94-36-0, purchased from Sinopharm Chemical Reagent Co., Ltd. Triethanolamine, CAS No. 102-71-6, was purchased from Shanghai Maclean Biochemical Technology Co., Ltd.

[0041] Example 1 This embodiment provides a method for preparing a high-rebound, damping-resistant silicone material, including the following steps: S1. By weight, 90 parts of methylphenyl vinyl silicone rubber were added to 500 parts of tetrahydrofuran and stirred for 60 min. Then, 6 parts of 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol were added and stirred for 40 min. Then, 0.8 parts of benzoin dimethyl ether were added and irradiated with 365 nm wavelength light for 6 min. After the reaction was completed, 900 parts of anhydrous ethanol were added for flocculation. The mixture was filtered, washed with anhydrous ethanol, and vacuum dried to obtain modified silicone rubber.

[0042] S2. Mix 90 parts modified silicone rubber, 25 parts fumed silica, 20 parts high-elasticity aerogel powder, 20 parts silicone oil (15 parts terminal epoxy polyether silicone oil and 5 parts fluorinated amino silicone oil), and 0.4 parts defoamer triethanolamine, heat to 75°C and stir for 20 min. Then, heat to 110°C under a vacuum of -0.8 MPa and knead for 90 min. Cool and let stand for 24 h to obtain the compound.

[0043] S3. The compound rubber is mixed with 2 parts of vulcanizing agent dicumyl peroxide and then vulcanized. First, it is vulcanized at 180°C for 10 minutes, and then vulcanized at 200°C for 120 minutes to obtain a high rebound damping silicone material.

[0044] Preparation of the high-elasticity aerogel powder: By weight, 12 parts of 2-amino-4-hydroxy-6-methylpyrimidine were added to a reaction vessel under a nitrogen atmosphere. After heating to 50°C, 80 parts of hexamethylene diisocyanate and 3 parts of N-methylpyrrolidone were added. The mixture was stirred at 100°C for 16 hours. Then, 60 parts of chloroform were added and stirred for 60 minutes. A mixture of 450 parts of n-heptane and 50 parts of isopropyl ether was added to precipitate the precipitate. The precipitate was filtered, washed with anhydrous ethanol, and dried to obtain the elastic treatment agent. 20 parts of amino-modified cellulose aerogel and 25 parts of the elastic treatment agent were added to 200 parts of chloroform. Under a nitrogen atmosphere, 0.4 parts of dibutyltin dilaurate were added and the mixture was heated to 60°C and stirred for 2 hours. After the reaction was completed, the mixture was filtered, washed with anhydrous ethanol, dried, and pulverized to obtain the high-elasticity aerogel powder.

[0045] Example 2 This embodiment provides a method for preparing a high-rebound, damping-resistant silicone material, including the following steps: S1. By weight, 80 parts of methylphenyl vinyl silicone rubber were added to 400 parts of tetrahydrofuran and stirred for 50 min. Then, 4 parts of 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol were added and stirred for 30 min. Then, 0.6 parts of benzoin dimethyl ether were added and irradiated with 365 nm wavelength light for 4 min. After the reaction was completed, 800 parts of anhydrous ethanol were added for flocculation, filtered, washed with anhydrous ethanol, and vacuum dried to obtain modified silicone rubber.

[0046] S2. Mix 80 parts modified silicone rubber, 15 parts fumed silica, 10 parts high-elasticity aerogel powder, 10 parts silicone oil (5 parts terminal epoxy polyether silicone oil and 5 parts fluorinated amino silicone oil), and 0.2 parts defoamer triethanolamine, heat to 65°C and stir for 30 min. Then, heat to 100°C under a vacuum of -0.8 MPa and knead for 100 min. Cool and let stand for 20 h to obtain the compound.

[0047] S3. The compound rubber is mixed with 1 part of benzoyl peroxide vulcanizing agent and then vulcanized. First, it is vulcanized at 170°C for 15 min, and then vulcanized at 190°C for 180 min to obtain a high rebound damping silicone material.

[0048] Preparation of the high-elasticity aerogel powder: By weight, 10 parts of 2-amino-4-hydroxy-6-methylpyrimidine were added to a reaction vessel under a nitrogen atmosphere. After heating to 40°C, 70 parts of hexamethylene diisocyanate and 2 parts of N-methylpyrrolidone were added. The mixture was stirred at 90°C for 20 h. Then, 50 parts of chloroform were added and stirred for 50 min. A mixture of 400 parts of n-heptane and 100 parts of isopropyl ether was added to precipitate the precipitate. The precipitate was filtered, washed with anhydrous ethanol, and dried to obtain the elastic treatment agent. 10 parts of amino-modified cellulose aerogel and 15 parts of the elastic treatment agent were added to 180 parts of chloroform. Under a nitrogen atmosphere, 0.2 parts of dibutyltin dilaurate were added and the mixture was heated to 50°C and stirred for 4 h. After the reaction was completed, the mixture was filtered, washed with anhydrous ethanol, dried, and pulverized to obtain the high-elasticity aerogel powder.

[0049] Example 3 This embodiment provides a method for preparing a high-rebound, damping-resistant silicone material, including the following steps: S1. By weight, 85 parts of methylphenyl vinyl silicone rubber were added to 450 parts of tetrahydrofuran and stirred for 56 min. Then, 5 parts of 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol were added and stirred for 34 min. Then, 0.7 parts of benzoin dimethyl ether were added and irradiated with 365 nm wavelength light for 5 min. After the reaction was completed, 840 parts of anhydrous ethanol were added for flocculation. The mixture was filtered, washed with anhydrous ethanol, and vacuum dried to obtain modified silicone rubber.

[0050] S2. Mix 88 parts modified silicone rubber, 17 parts fumed silica, 16 parts high-elasticity aerogel powder, 15 parts silicone oil (10 parts terminal epoxy polyether silicone oil and 5 parts fluorinated amino silicone oil), and 0.3 parts defoamer triethanolamine, heat to 68°C and stir for 24 min. Then, heat to 104°C under a vacuum of -0.8 MPa and knead for 98 min. Cool and let stand for 22 h to obtain the compound.

[0051] S3. The compound rubber is mixed with 1.4 parts of benzoyl peroxide vulcanizing agent and then vulcanized. First, it is vulcanized at 174°C for 14 min, and then vulcanized at 196°C for 130 min to obtain a high rebound damping silicone material.

[0052] Preparation of the high-elasticity aerogel powder: By weight, 11 parts of 2-amino-4-hydroxy-6-methylpyrimidine were added to a reaction vessel under a nitrogen atmosphere. After heating to 45°C, 76 parts of hexamethylene diisocyanate and 2.4 parts of N-methylpyrrolidone were added. The mixture was stirred at 94°C for 18 hours. Then, 56 parts of chloroform were added and stirred for 55 minutes. A mixture of 420 parts of n-heptane and 80 parts of isopropyl ether was added to precipitate the precipitate. The precipitate was filtered, washed with anhydrous ethanol, and dried to obtain the elastic treatment agent. 14 parts of amino-modified cellulose aerogel and 18 parts of the elastic treatment agent were added to 190 parts of chloroform. Under a nitrogen atmosphere, 0.3 parts of dibutyltin dilaurate were added and the mixture was heated to 56°C and stirred for 3 hours. After the reaction was completed, the mixture was filtered, washed with anhydrous ethanol, dried, and pulverized to obtain the high-elasticity aerogel powder.

[0053] Comparative Example 1 The difference between this comparative example and Example 1 is that methyl phenyl vinyl silicone rubber (model MY3120) was used instead of modified silicone rubber.

[0054] Comparative Example 2 The difference between this comparative example and Example 1 is that no highly elastic aerogel powder is added.

[0055] Comparative Example 3 The difference between this comparative example and Example 1 is that amino-modified cellulose aerogel (item number Q0325437) is used instead of high-elasticity aerogel powder.

[0056] Comparative Example 4 The difference between this comparative example and Example 1 is that the silicone oil used is replaced with 20 parts of end-epoxy polyether silicone oil (model PPE-8K500).

[0057] Comparative Example 5 The difference between this comparative example and Example 1 is that the silicone oil was replaced with 20 parts of fluorinated amino silicone oil (model DYSIL).

[0058] Comparative Example 6 The difference between this comparative example and Example 1 is that the silicone oil used is replaced with 20 parts of dimethyl silicone oil (model MF-1000).

[0059] The performance of the above embodiments and comparative examples was tested using the following methods: the dielectric constant was tested according to the requirements of GB / T1693-2007, the thermal conductivity was tested according to the requirements of ASTM C518, and the resilience was tested according to the requirements of GB / T1681-2009.

[0060] The performance test data above are shown in Table 1.

[0061] Table 1 Performance Test Results

[0062] As can be seen from the above, the present invention first modifies methylphenyl vinyl silicone rubber by mixing and modifying 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol to obtain modified silicone rubber. Then, an elastic treatment agent is prepared using 2-amino-4-hydroxy-6-methylpyrimidine and hexamethylene diisocyanate as raw materials and mixed with amino-modified cellulose aerogel for stirring reaction to obtain high-elasticity aerogel powder. Then, modified silicone rubber, silica, high-elasticity aerogel powder, silicone oil, and defoamer are mixed, heated and stirred for intensive mixing to obtain compound. Finally, the compound is mixed with a vulcanizing agent and vulcanized to obtain high-rebound damping silicone material (Examples 1 to 3), which has better comprehensive performance.

[0063] Compared to Example 1, using methylphenyl vinyl silicone rubber (model MY3120) instead of modified silicone rubber resulted in a lack of the effect of the triazine ring in the modified silicone rubber, leading to increased thermal conductivity and decreased resilience (Comparative Example 1); compared to Example 1, not adding high-elasticity aerogel powder resulted in a lack of the effect of the high-elasticity aerogel powder, leading to increased thermal conductivity and decreased resilience (Comparative Example 2); compared to Example 1, using amino-modified cellulose aerogel (product number Q0325437) instead of high-elasticity aerogel powder resulted in a lack of the effect of the elasticity treatment agent, leading to increased thermal conductivity and decreased resilience (Comparative Example 3). Compared to Example 1, the silicone oil was changed to 20 parts of terminal epoxy polyether silicone oil (model PPE-8K500), which lacked the compounding of fluorinated amino silicone oil, resulting in increased thermal conductivity and decreased resilience (Comparative Example 4); compared to Example 1, the silicone oil was changed to 20 parts of fluorinated amino silicone oil (model DYSIL), which lacked the compounding of terminal epoxy polyether silicone oil, resulting in increased thermal conductivity and decreased resilience (Comparative Example 5); compared to Example 1, the silicone oil was changed to 20 parts of dimethyl silicone oil (model MF-1000), which was not effective, resulting in increased thermal conductivity and decreased resilience (Comparative Example 6).

Claims

1. A method for preparing a high-rebound, damping-resistant silicone material, characterized in that, Includes the following steps: S1. Methylphenyl vinyl silicone rubber and 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol were mixed and modified to obtain modified silicone rubber. S2. Mix modified silicone rubber, fumed silica, aerogel, silicone oil, and defoamer, heat and stir, and then perform intensive mixing to obtain a compound. S3. The compound rubber is mixed with a vulcanizing agent and then subjected to vulcanization treatment to obtain a high-rebound damping silicone material.

2. The method for preparing a high-rebound, damping-resistant silicone material according to claim 1, characterized in that, The components, by weight, include: 80-90 parts modified silicone rubber, 15-25 parts silica, 10-20 parts aerogel, 10-20 parts silicone oil, 1-2 parts vulcanizing agent, and 0.2-0.4 parts defoamer.

3. The method for preparing a high-rebound, damping-resistant silicone material according to claim 1, characterized in that, The modification process is as follows: by weight, 80-90 parts of methylphenyl vinyl silicone rubber are added to 400-500 parts of tetrahydrofuran and stirred for 50-60 minutes. Then, 4-6 parts of 6-(dibutylamino)-1,3,5-triazine-2,4-dithiol are added and stirred for 30-40 minutes. Next, 0.6-0.8 parts of benzoin dimethyl ether are added and irradiated with 365nm wavelength light for 4-6 minutes. After the reaction is completed, 800-900 parts of anhydrous ethanol are added for flocculation, filtered, washed with anhydrous ethanol, and vacuum dried to obtain modified silicone rubber.

4. The method for preparing a high-rebound, damping-resistant silicone material according to claim 1, characterized in that, The aerogel is a highly elastic aerogel powder; The high-elasticity aerogel powder is prepared by: using 2-amino-4-hydroxy-6-methylpyrimidine and hexamethylene diisocyanate as raw materials to prepare an elastic treatment agent; mixing the elastic treatment agent with amino-modified cellulose aerogel and stirring to obtain the high-elasticity aerogel powder.

5. The method for preparing a high-rebound, damping-resistant silicone material according to claim 4, characterized in that, The preparation steps of the elastic treatment agent are as follows: by weight, 10-12 parts of 2-amino-4-hydroxy-6-methylpyrimidine are added to a reaction vessel under a nitrogen atmosphere. After heating to 40-50°C, 70-80 parts of hexamethylene diisocyanate and 2-3 parts of N-methylpyrrolidone are added. The mixture is stirred at 90-100°C for 16-20 hours. Then, 50-60 parts of chloroform are added and stirred for 50-60 minutes. A mixture of 400-450 parts of n-heptane and 50-100 parts of isopropyl ether is added to precipitate the precipitate. The precipitate is filtered, washed with anhydrous ethanol, and dried to obtain the elastic treatment agent.

6. The method for preparing a high-rebound, damping-resistant silicone material according to claim 4, characterized in that, The stirring reaction steps are as follows: by weight, 10-20 parts of amino-modified cellulose aerogel and 15-25 parts of elastic treatment agent are added to 180-200 parts of chloroform, 0.2-0.4 parts of dibutyltin dilaurate are added under a nitrogen atmosphere and the temperature is raised to 50-60℃ for stirring reaction for 2-4 hours. After the reaction is completed, the mixture is filtered, washed with anhydrous ethanol, dried, and pulverized to obtain high elasticity aerogel powder.

7. The method for preparing a high-rebound, damping-resistant silicone material according to claim 1, characterized in that, The silicone oil is selected from one or more of dimethyl silicone oil, hydroxyl silicone oil, hydrogen-containing silicone oil, epoxy silicone oil, and amino silicone oil.

8. The method for preparing a high-rebound, damping-resistant silicone material according to claim 7, characterized in that, The silicone oil is epoxy silicone oil and amino silicone oil; The mass ratio of epoxy silicone oil to amino silicone oil is (1~3):

1.

9. The method for preparing a high-rebound, damping-resistant silicone material according to claim 8, characterized in that, The epoxy silicone oil is an epoxy polyether silicone oil with a molecular weight of 5000~10000 and an epoxy value of 0.01~0.03mol / 100g. The amino silicone oil is a fluorinated amino silicone oil, which has a viscosity of 2000~5000 cps at 25°C and an ammonia value of 0.2~0.8%.

10. A high-rebound, damping-resistant silicone material, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 9.

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