A perfluoroether rubber material with easy processing, high toughness, and low coefficient of thermal expansion, its preparation method and application.
By preparing perfluoroether rubber materials that are easy to process, have high toughness, and low coefficient of thermal expansion, the problems of dispersion and interfacial bonding of nano-silicon carbide in rubber systems were solved, and the high toughness and dimensional stability of the rubber materials were achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- IC SEAL CO LTD
- Filing Date
- 2026-06-11
- Publication Date
- 2026-07-17
AI Technical Summary
Existing nano-silicon carbide exhibits poor dispersion in rubber systems, is difficult to process, causes serious dust pollution, and has poor interfacial bonding with rubber, resulting in reduced toughness of composite materials.
Perfluoroether rubber material with easy processing, high toughness, and low coefficient of thermal expansion is prepared by mixing granulated silicon carbide with rubber elastomer and vulcanizing agent and processing through internal mixing and open milling.
It achieves easy processing and dust-free perfluoroether rubber materials, significantly improves toughness, and reduces the coefficient of thermal expansion, making it suitable for rubber products with high requirements for dimensional stability and crack resistance.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of perfluoroether rubber technology, and in particular to a perfluoroether rubber material that is easy to process, has high toughness, and low coefficient of thermal expansion, as well as its preparation method and application. Background Technology
[0002] Rubber, as a critical strategic material, is widely used in tires, seals, damping materials, and other fields. Since researchers discovered in 1904 that adding carbon black to rubber could significantly improve its mechanical properties, using nanofillers to reinforce rubber has become the most common reinforcement method in actual production. Compared to carbon black / silica, nano-silicon carbide, as a functional reinforcing filler, has significant advantages in the thermal conductivity and high-temperature stability of composite materials. However, conventional nano-silicon carbide has poor dispersibility in rubber systems, is difficult to process, causes serious dust pollution, and has poor interfacial bonding with rubber, easily leading to stress concentration and thus reducing the toughness of composite materials. Summary of the Invention
[0003] In view of the shortcomings of the prior art described above, the purpose of this invention is to provide a perfluoroether rubber material that is easy to process, has high toughness, and low coefficient of thermal expansion, as well as its preparation method and application.
[0004] To achieve the objectives of this invention, the following technical solution is adopted:
[0005] The present invention provides a perfluoroether rubber material comprising granulated silicon carbide, a rubber elastomer, and a vulcanizing agent, wherein the granulated silicon carbide comprises 10-45 parts by weight, the rubber elastomer comprises 100 parts, and the vulcanizing agent comprises 0.8-1.8 parts.
[0006] In some embodiments of the present invention, the granulated silicon carbide is spherical with a bulk density > 300 g / L, a D50 < 100 nm, and a specific surface area > 30 m². 2 / g.
[0007] In some embodiments of the present invention, the method for preparing the granulated silicon carbide includes: compressing and granulating silicon carbide particles.
[0008] In some embodiments of the present invention, the particle size of the silicon carbide nanoparticles is <100 nm, and the specific surface area of the silicon carbide nanoparticles is >30 m². 2 / g.
[0009] In some embodiments of the present invention, the particle size of the silicon carbide nanoparticles is <50 nm, and the specific surface area of the silicon carbide nanoparticles is >50 m². 2 / g.
[0010] In some embodiments of the present invention, the specific surface area of the granulated silicon carbide is at least 70% of the specific surface area of the silicon carbide nanoparticles.
[0011] In some preferred embodiments of the present invention, the specific surface area of the granulated silicon carbide is at least 90% of the specific surface area of the silicon carbide nanoparticles.
[0012] In some embodiments of the present invention, the granulated silicon carbide has a packing density of at least 500% of that of silicon carbide nanoparticles.
[0013] In some preferred embodiments of the present invention, the granulated silicon carbide has a packing density of at least 750% of that of silicon carbide nanoparticles.
[0014] Another aspect of the present invention provides a method for preparing a perfluoroether rubber material, the method comprising at least the following steps:
[0015] 1) The rubber elastomer and granulated silicon carbide are mixed by internal mixing or open milling to obtain internal compound;
[0016] 2) The internally mixed rubber from step 1) and the vulcanizing agent are mixed in a two-roll mill to obtain a compounded rubber;
[0017] 3) The compound obtained in step 2) is vulcanized to obtain perfluoroether rubber material.
[0018] In some embodiments of the present invention, in step 1), the mixing temperature is 100~180°C.
[0019] In some embodiments of the present invention, in step 1), the roll gap of the open mill is 0.0~0.8mm.
[0020] In some embodiments of the present invention, in step 3), the vulcanization is divided into two stages: the first stage is a pressurized vulcanization at a temperature of 150~180℃, a pressure of 5~14MPa, and a time of 3~20min; the second stage is a vulcanization at a temperature of 200~300℃ and a time of 10~24h.
[0021] Another aspect of the present invention provides the use of the perfluoroether rubber material as described herein in sealing rings, shock-absorbing pads, and electronic packaging gaskets.
[0022] By adopting the aforementioned technical solution, the beneficial effects of the present invention are:
[0023] 1. The perfluoroether rubber material of the present invention is easy to process, easy to disperse, and produces no dust pollution;
[0024] 2. The perfluoroether rubber material of the present invention significantly improves toughness while maintaining high hardness;
[0025] 3. The perfluoroether rubber material of the present invention has a low coefficient of thermal expansion (CTE). This compound is suitable for rubber products with high requirements for dimensional stability and crack resistance, such as sealing rings, shock-absorbing pads, electronic packaging gaskets, etc. Detailed Implementation
[0026] The following details the implementation of the easily processed, high-toughness, low-thermal-expansion coefficient perfluoroether rubber material, its preparation method, and its applications provided by the present invention.
[0027] The "range" disclosed in this application is defined by a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of a particular range. Ranges defined in this way can include or exclude endpoints and can be arbitrarily combined; that is, any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60~120 and 80~110 are listed for a specific parameter, it is also expected that ranges of 60~110 and 80~120 are also included. Furthermore, if minimum range values of 1 and 2 are listed, and if maximum range values of 3, 4, and 5 are listed, then the following ranges are all expected: 1~3, 1~4, 1~5, 2~3, 2~4, and 2~5. In this application, unless otherwise stated, the numerical range "a~b" represents a shortened representation of any combination of real numbers between a and b, where a and b are real numbers. For example, the numerical range "0~5" indicates that all real numbers between "0~5" have been listed in this article; "0~5" is simply a shortened representation of these numerical combinations. Furthermore, when a parameter is stated as an integer ≥2, it is equivalent to disclosing that the parameter is, for example, an integer such as 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.
[0028] Through extensive research and exploration, the inventors of this invention have obtained a perfluoroether rubber material with easy processing, high toughness, and low coefficient of thermal expansion (CTE) by using silicon carbide granulated using a special method. Compared with rubber using ungranulated silicon carbide, the composite of this invention is easier to process and disperses better in rubber processing, produces no dust pollution, and significantly improves toughness while maintaining high hardness, effectively reducing the coefficient of thermal expansion (CTE). This composite is suitable for rubber products with high requirements for dimensional stability and crack resistance, such as sealing rings, shock-absorbing pads, and electronic packaging gaskets. This invention does not involve the silicon carbide granulation process itself, but rather provides a high-toughness, low-CTE rubber composite material solution based on the new applications and performance improvements of this special silicon carbide in rubber. This application was completed on this basis.
[0029] Perfluoroether rubber materials
[0030] This invention provides a perfluoroether rubber material, which comprises granulated silicon carbide, a rubber elastomer, and a vulcanizing agent.
[0031] In the perfluoroether rubber material provided by the present invention, the granulated silicon carbide is 10 to 45 parts by mass and any value between them or any two values, and can be selected as 10 to 15 parts by mass, 5 to 15 parts by mass, 15 to 20 parts by mass, or 20 to 45 parts by mass.
[0032] In the perfluoroether rubber material provided by the present invention, the rubber elastomer comprises 100 parts.
[0033] In the perfluoroether rubber material provided by this invention, the vulcanizing agent is 0.8 to 1.8 parts, or any value between them, or a range between any two values. It can be selected as 0.8 to 1.2 parts or 1.2 to 1.8 parts.
[0034] In the perfluoroether rubber material provided by this invention, the granulated silicon carbide is spherical with a bulk density > 300 g / L, D50 < 100 nm, and specific surface area > 30 m². 2 / g.
[0035] The perfluoroether rubber material provided by this invention includes a method for preparing the granulated silicon carbide, comprising: compressing and granulating silicon carbide particles. The specific method is as follows: compacting the silicon carbide nanoparticles using equipment capable of providing high pressure. The equipment providing high pressure can be, for example, a dry granulation machine with pressure rollers. The particle size of the silicon carbide nanoparticles is <100nm, and can be <90nm, <80nm, <70nm, <60nm, or <50nm. More preferably, it is <50nm; the specific surface area of the silicon carbide nanoparticles is >30m². 2 / g, can be selected as >35m 2 / g、>40m 2 / g、>45m 2 / g、>50m 2 / g. Preferably greater than 50m 2 / g.
[0036] In this compression granulation method, no coupling agent is added for surface modification of silicon carbide nanoparticles, nor is any binder added to increase their adhesion. This is to avoid uncontrollable situations (such as self-polymerization or desorption) during the chemical reaction of the coupling agent, reduce the risk of agglomeration, and avoid the risk of introducing harmful impurities at high temperatures.
[0037] In this compression granulation method, it is not necessary to sinter the silicon carbide nanoparticles at temperatures exceeding 400°C. This is because high temperatures can cause new covalent bonds to form between the nanofillers, thereby reducing the specific surface area of the nanoparticles or affecting their nanoscale properties.
[0038] The silicon carbide particles processed by this method are granulated silicon carbide, and their specific surface area is at least 70% of the specific surface area of silicon carbide nanoparticles. Optionally, the specific surface area of the granulated silicon carbide is at least 75%, 80%, 85%, or 90% of the specific surface area of the silicon carbide nanoparticles. Preferably, the specific surface area of the granulated silicon carbide is at least 90% of the specific surface area of the silicon carbide nanoparticles.
[0039] The silicon carbide particles processed by this method are granulated silicon carbide, and their bulk density is at least 500% of the bulk density of silicon carbide nanoparticles. Optionally, the bulk density of the granulated silicon carbide is at least 550%, 600%, 650%, 700%, or 750% of the bulk density of silicon carbide nanoparticles. Preferably, the bulk density of the granulated silicon carbide is at least 750% of the bulk density of silicon carbide nanoparticles.
[0040] Preparation methods for perfluoroether rubber materials
[0041] The present invention also provides a method for preparing a perfluoroether rubber material, the method comprising at least the following steps:
[0042] 1) The rubber elastomer and granulated silicon carbide are mixed by internal mixing or open milling to obtain internal compound;
[0043] 2) The internally mixed rubber from step 1) and the vulcanizing agent are mixed in a two-roll mill to obtain a compounded rubber;
[0044] 3) The compound obtained in step 2) is vulcanized to obtain perfluoroether rubber material.
[0045] In the preparation method of the perfluoroether rubber material provided by this invention, step 1) involves mixing a rubber elastomer and granulated silicon carbide using a mixing mill or open mill to obtain a mixed rubber. Specifically:
[0046] In step 1), the mixing temperature is 100~180℃ and any value between them or any two values, and can be selected as 100~150℃, 150~180℃, 100~130℃, or 130~150℃.
[0047] In step 1), the gap between the open mill rolls is 0.0~0.8mm and any value between them or any two values, and can be selected as 0.0~0.4mm, 0.4~0.8mm, 0.0~0.2mm, 0.2~0.4mm, 0.4~0.6mm, or 0.6~0.8mm.
[0048] In the preparation method of perfluoroether rubber material provided by the present invention, step 2) is to mix the internal rubber compound described in step 1) with the vulcanizing agent in a two-roll mill to obtain a compound.
[0049] In the preparation method of perfluoroether rubber material provided by this invention, step 3) involves vulcanizing the compound obtained in step 2) to obtain the perfluoroether rubber material. Specifically:
[0050] In step 3) of this invention, vulcanization is divided into two stages. The first stage involves pressurized vulcanization at a temperature of 150-180℃ or any value between these two temperatures, specifically 150-160℃ or 160-180℃. The first stage involves pressurized vulcanization at a pressure of 5-14 MPa or any value between these two temperatures, specifically 5-8 MPa, 8-10 MPa, or 10-14 MPa. The first stage involves pressurized vulcanization at a time of 3-20 min or any value between these two temperatures, specifically 3-10 min, 10-15 min, or 15-20 min. The second stage involves vulcanization at a temperature of 200-300℃ or any value between these two temperatures, specifically 200-250℃ or 250-300℃. The time range is 10 to 24 hours and any value in between, or any range between two values, and can be selected as 10 to 15 hours, 15 to 20 hours, or 20 to 24 hours.
[0051]
application
[0052] The present invention also provides the use of perfluoroether rubber materials as described herein in sealing rings, shock-absorbing pads, and electronic packaging gaskets.
[0053] The beneficial effects of the present invention will be further illustrated below with reference to the embodiments.
[0054] To make the inventive objectives, technical solutions, and beneficial effects of this invention clearer, the invention is further described in detail below with reference to embodiments. However, it should be understood that the embodiments of this invention are merely for illustrative purposes and not for limiting the invention, and the embodiments are not limited to those given in the specification. Unless otherwise specified, specific experimental or operational conditions in the embodiments were prepared under conventional conditions or according to the conditions recommended by the material supplier.
[0055] Furthermore, it should be understood that the existence of other method steps before or after the combined steps, or the insertion of other method steps between these explicitly mentioned steps, does not preclude the existence of other method steps before or after the combined steps, or the insertion of other method steps between these explicitly mentioned steps, unless otherwise stated. It should also be understood that the combined connection relationship between one or more devices / apparatus mentioned in this invention does not preclude the existence of other devices / apparatus before or after the combined devices / apparatus, or the insertion of other devices / apparatus between these explicitly mentioned devices / apparatus, unless otherwise stated. Moreover, unless otherwise stated, the numbering of each method step is merely a convenient tool for identifying each method step, and not for limiting the order of the method steps or limiting the scope of the invention. Changes or adjustments to their relative relationships, without substantially altering the technical content, should also be considered within the scope of the invention.
[0056] In the following embodiments, unless otherwise specified, all the raw materials of the present invention are commercially available or prepared according to conventional methods in the art.
[0057] 3M™ Dyneon™ PFE 133TB was purchased from 3M Company, USA; Tecnoflon® PFR 95HT was purchased from Synesqo Company, USA; BOAP: 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane, CAS No.: 83558-87-6, was purchased from Tokyo Chemical Industry Co., Ltd.; TX101: 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, CAS No.: 78-63-7, was purchased from Tokyo Chemical Industry Co., Ltd.
[0058] SiC was purchased from Titan Technology Exploration Platform, model: β phase (3C), with a particle size of 32nm and a specific surface area of 50m². 2 / g,
[0059] N990 was purchased from Orion Engineered Carbons, model: CORAX® N990; R972 was purchased from Evonik, model: AEROSIL® R972.
[0060] Shore A test method: ASTM D2240;
[0061] Tensile strength test method: ASTM D412;
[0062] 100% Modulus Test Method: ASTM D412;
[0063] Elongation at break test method: ASTM D412;
[0064] Tear strength test method: ASTM D624;
[0065] Toughness test method: GB / T 528-2009;
[0066] CTE test method: ASTM E831.
[0067] Preparation Example 1:
[0068] Granulated silicon carbide (SiC-Gr)
[0069] Silicon carbide nanoparticles were compacted using a dry roller granulation machine. A multi-stage tandem extrusion system, employing large, medium-sized, and small roller mills, was used to gradually compact the silicon carbide through multi-stage extrusion and degassing, resulting in silicon carbide particles with high bulk density. The granulated silicon carbide was nearly spherical, with an average bulk density of 337 g / L, a D50 of 31 nm, and a S... BET 53m 2 / g.
[0070] Preparation Example 2:
[0071] Granulated silicon carbide (SIC-Gr-2)
[0072] Silicon carbide nanoparticles were compacted using a dry roller granulation machine, without employing a multi-stage tandem extrusion system; i.e., a single extrusion was used. The granulated silicon carbide was nearly spherical, with an average bulk density of 156 g / L, a D50 of 32 nm, and a S... BET 54m 2 / g.
[0073] Comparative Example 1
[0074] 100 parts of rubber elastomer 133TB and 1.8 parts of vulcanizing agent BOAP were mixed evenly in a two-roll mill with a roll gap of 0.8 mm. The sample was obtained after a first-stage vulcanization and a second-stage vulcanization. The first-stage vulcanization was carried out at a temperature of 188℃, a pressure of 5 MPa, and a time of 900 s. The second-stage vulcanization was carried out at a temperature of 250℃ for 16 h.
[0075] Comparative Example 2
[0076] 100 parts of rubber elastomer 133TB and 15 parts of inorganic filler SiC were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After resting for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a temperature of 188℃, a pressure of 5MPa, and a time of 900s. The second stage of vulcanization was carried out at a temperature of 250℃ and a time of 16 hours.
[0077] Comparative Example 3
[0078] 100 parts of rubber elastomer 95HT and 15 parts of inorganic filler SiC were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After standing for 24 hours, the internally mixed rubber compound was uniformly mixed with 0.8 parts of vulcanizing agent TX101 in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a temperature of 160℃, a pressure of 5MPa, and a time of 360s. The second stage of vulcanization was carried out at a temperature of 230℃ and a time of 4 hours.
[0079] Example 1
[0080] 100 parts of rubber elastomer 133TB and 15 parts of inorganic filler SiC-Gr were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After resting for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0081] Example 2
[0082] 100 parts of rubber elastomer 95HT and 15 parts of inorganic filler SIC-Gr were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After standing for 24 hours, the internally mixed rubber compound was uniformly mixed with 0.8 parts of vulcanizing agent TX101 in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 160℃ and a pressure of 5MPa for 360 seconds. The second stage of vulcanization was carried out at a temperature of 230℃ for 4 hours.
[0083] Table 1
[0084]
[0085] In Table 1, ** ×, △, ◎ The degree ranges from poor to good.
[0086] In both cyano-based and peroxide-based systems, compared with SiC-filled systems, SiC-Gr significantly improves processing efficiency and reduces dust pollution. While maintaining the same high hardness and high modulus, SiC-Gr can provide greater tear strength, toughness, and a lower coefficient of linear thermal expansion (CTE).
[0087] Comparative Example 4
[0088] 100 parts of rubber elastomer 133TB and 5 parts of inorganic filler SiC-Gr were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After resting for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0089] Example 3
[0090] 100 parts of rubber elastomer 133TB and 10 parts of inorganic filler SIC-Gr were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After standing for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0091] Example 4
[0092] 100 parts of rubber elastomer 133TB and 20 parts of inorganic filler SiC-Gr were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain a mixed rubber compound. After resting for 24 hours, the mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0093] Comparative Example 5
[0094] 100 parts of rubber elastomer 133TB and 50 parts of inorganic filler SiC-Gr were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After resting for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0095] Table 2
[0096]
[0097] ** ×、△、 ◎ The degree ranges from poor to good
[0098] When the amount of SiC-Gr used is in the range of 10 to 20 parts, there is no significant change in processing efficiency or dust pollution as the amount of SiC-Gr increases. However, when the amount of SiC-Gr is no more than 5 parts, such as in Comparative Example 4, it cannot guarantee that the formulation has high hardness and high modulus, and the linear coefficient of thermal expansion (CTE) is not significantly improved. When the amount of SiC-Gr is no less than 50 parts, such as in Comparative Example 5, the formulation cannot be molded.
[0099] Comparative Example 6
[0100] 100 parts of rubber elastomer 133TB and 15 parts of filler SIC-Gr-2 were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After resting for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0101] Comparative Example 7
[0102] 100 parts of rubber elastomer 133TB and 15 parts of filler N990 were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After resting for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0103] Comparative Example 8
[0104] 100 parts of rubber elastomer 133TB and 15 parts of filler R972 were uniformly mixed in a high-temperature internal mixer (temperature 120℃) to obtain an internally mixed rubber compound. After resting for 24 hours, the internally mixed rubber compound was uniformly mixed with 1.8 parts of vulcanizing agent BOAP in an open mill to obtain a compounded rubber compound. After one stage of vulcanization and two stages of vulcanization, a sample was obtained. The first stage of vulcanization was carried out at a pressure of 188℃ and a pressure of 5MPa for 900s. The second stage of vulcanization was carried out at a temperature of 250℃ for 16 hours.
[0105] Table 3
[0106]
[0107] Compared to SiC-Gr-2, SiC-Gr filling results in formulations with higher tear strength and a lower coefficient of linear thermal expansion.
[0108] Compared with filled carbon black N990 and silica R972, the formulation filled with SIC-Gr has higher tear strength and lower linear coefficient of thermal expansion.
[0109] In summary, this invention effectively overcomes the various shortcomings of the prior art and has high industrial application value.
[0110] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any form or substance. It should be noted that those skilled in the art can make various improvements and additions without departing from the method of the present invention, and these improvements and additions should also be considered within the scope of protection of the present invention. Any modifications, alterations, and equivalent changes made by those skilled in the art based on the above-disclosed technical content without departing from the spirit and scope of the present invention are equivalent embodiments of the present invention. Furthermore, any modifications, alterations, and evolutions made to the above embodiments based on the essential technology of the present invention still fall within the scope of the technical solution of the present invention.
Claims
1. A perfluoroether rubber material, characterized in that, The perfluoroether rubber material comprises granulated silicon carbide, a rubber elastomer, and a vulcanizing agent, wherein the granulated silicon carbide comprises 10-45 parts by weight, the rubber elastomer comprises 100 parts, and the vulcanizing agent comprises 0.8-1.8 parts.
2. The perfluoroether rubber material according to claim 1, characterized in that, Granulated silicon carbide is spherical with a bulk density >300 g / L, D50 <100 nm, and specific surface area >30 m². 2 / g.
3. The perfluoroether rubber material according to claim 1, characterized in that, The method for preparing granulated silicon carbide includes: compressing and granulating silicon carbide particles.
4. The perfluoroether rubber material according to claim 3, characterized in that, The silicon carbide nanoparticles have a particle size <100 nm and a specific surface area >30 m². 2 / g.
5. The perfluoroether rubber material according to claim 4, characterized in that, The silicon carbide nanoparticles have a particle size < 50 nm and a specific surface area > 50 m². 2 / g.
6. The perfluoroether rubber material according to claim 3, characterized in that, It also includes one or more of the following conditions: A1) The specific surface area of the granulated silicon carbide is at least 70% of the specific surface area of the silicon carbide nanoparticles; A2) The granulated silicon carbide has a packing density of at least 500% of that of silicon carbide nanoparticles.
7. The perfluoroether rubber material according to claim 6, characterized in that, It also includes one or more of the following conditions: A11) The specific surface area of the granulated silicon carbide is at least 90% of the specific surface area of the silicon carbide nanoparticles; A21) The granulated silicon carbide has a packing density of at least 750% of that of silicon carbide nanoparticles.
8. The method for preparing the perfluoroether rubber material according to any one of claims 1 to 7, characterized in that, The preparation method includes at least the following steps: 1) The rubber elastomer and granulated silicon carbide are mixed by internal mixing or open milling to obtain internal compound; 2) The internally mixed rubber from step 1) is mixed with the vulcanizing agent in a two-roll mill to obtain a compound rubber; 3) The compound obtained in step 2) is vulcanized to obtain perfluoroether rubber material.
9. The method for preparing the perfluoroether rubber material according to claim 8, characterized in that, It also includes one or more of the following conditions: B1) In step 1), the mixing temperature is 100~180℃; B2) In step 1), the open mill roll gap is 0.0~0.8mm; In step 3) of B3), vulcanization is divided into two stages: the first stage is under pressure at a temperature of 150~180℃ and a pressure of 5~14MPa for 3~20min; the second stage is under pressure at a temperature of 200~300℃ for 10~24h.
10. The use of the perfluoroether rubber material according to claims 1 to 7 in sealing rings, shock-absorbing pads, and electronic packaging gaskets.