High-temperature-resistant fluororubber material for seals and preparation method thereof

By surface-modifying carbon nanotubes and grafting fluoroalkyl chains, the problems of insufficient tensile and low-temperature properties of fluororubber were solved, and the overall performance of fluororubber was improved, especially in maintaining elasticity and reducing brittleness at low temperatures.

CN121108658BActive Publication Date: 2026-05-29GUANGDONG DECHUANGXIN MATERIAL CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
GUANGDONG DECHUANGXIN MATERIAL CO LTD
Filing Date
2025-09-28
Publication Date
2026-05-29

AI Technical Summary

Technical Problem

Fluororubber has shortcomings in tensile and low-temperature performance, and its high cost limits its application in certain fields.

Method used

By surface modification of carbon nanotubes and grafting dense fluoroalkyl chains onto them, their thermodynamic compatibility with the fluororubber matrix is ​​enhanced. Furthermore, through interfacial interactions and cross-linking network optimization, their elastic recovery and deformation resistance are improved, their glass transition temperature is reduced, and their low-temperature elastic range is broadened.

Benefits of technology

It significantly improves the tensile strength, tear strength and low-temperature brittleness temperature of fluororubber, and improves the overall performance of fluororubber, especially in maintaining elasticity and reducing brittleness at low temperatures.

✦ Generated by Eureka AI based on patent content.
Patent Text Reader

Abstract

The application relates to the technical field of fluorine rubber, and particularly discloses a high-temperature-resistant fluorine rubber material for a sealing element and a preparation method thereof. The fluorine rubber material comprises the following components in parts by weight: 80-120 parts of fluorine rubber, 3-6 parts of modified carbon nanotubes, 15-25 parts of reinforcing fillers, 1-3 parts of vulcanizing agents, 0.2-0.5 parts of accelerators, 2-5 parts of magnesium oxide and 1-2 parts of lubricants. The application also provides the preparation method. Compared with the prior art, the fluorine rubber material prepared by the application has good mechanical properties and low-temperature brittleness, can adapt to various specific use environments, and has a wide market application prospect.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of fluororubber technology, and in particular to a high-temperature resistant fluororubber material for sealing components and its preparation method. Background Technology

[0002] Fluororubber is a synthetic polymeric elastomer containing fluorine atoms on the carbon atoms of its main chain or side chains. Due to its unique molecular structure, it exhibits excellent high and low temperature resistance, chemical stability, weather resistance, and aging resistance, making it irreplaceable in many harsh environments. The superior performance of fluororubber is inextricably linked to its unique molecular structure. It belongs to the category of high-molecular-weight fluorinated polymers, where the hydrogen atoms in its main chain are replaced by more electronegative fluorine atoms. The introduction of fluorine atoms has a significant impact on the properties of fluororubber.

[0003] First, fluorine, as a halogen, is highly electronegative, which makes the fluorine-carbon covalent bond polar, thus significantly affecting the acidity / basicity, molecular configuration, and dipole moment of the molecule. Second, the radius of a fluorine atom is only slightly larger than that of a hydrogen atom, and the CF bond has an extremely high bond energy, between 435-485 kJ / mol. This results in a short CF bond length, allowing fluorine atoms to assemble closely around carbon atoms, effectively protecting the C-C bond. Finally, due to the high CF bond energy, fluorine atoms rarely form free radicals or ions, ensuring the stability of the CF bond and giving fluorine-containing compounds excellent chemical inertness. These properties are what give fluororubber its excellent high-temperature resistance and chemical resistance.

[0004] In terms of temperature resistance, fluororubber can be used for extended periods within a temperature range of -20℃ to 200℃. Some special varieties can even maintain good elasticity and sealing properties at extreme temperatures ranging from -40℃ to 260℃, making it highly favored in high-temperature operating environments such as aerospace and automotive engines. Chemical stability is another major advantage of fluororubber. It exhibits excellent resistance to fuels, lubricating oils, hydraulic fluids, and various chemical reagents, and is not easily corroded or swollen. Therefore, it is often used to manufacture seals, hoses, and other components that come into contact with these media.

[0005] CN115948010A discloses a fluororubber seal suitable for semiconductor processing and its preparation method. The seal's raw materials, by weight, comprise: 100 parts fluororubber, 5-15 parts fluororubber surface-modified graphene, 0-30 parts filler, 1-5 parts accelerator, 1-3 parts crosslinking agent, 0-5 parts acid scavenger, and 0-5 parts processing aid. This invention modifies fluororubber using surface-modified graphene, enabling the resulting fluororubber seal to better withstand complex media while meeting requirements for high hardness, high tensile strength, and high resistance to compression deformation.

[0006] CN119708731A discloses a tear-resistant fluororubber material and its preparation method, belonging to the field of fluororubber production technology. The raw materials for this tear-resistant fluororubber material include tetrapropylene fluororubber, modified carbon nanotubes, vulcanizing agents, accelerators, plasticizers, and antioxidants. The preparation steps of the modified carbon nanotubes are as follows: First, multi-walled carbon nanotubes are added to 2-phosphonobutane-1,2,4-tricarboxylic acid, and vacuum treatment is performed. Then, the mixture is heated and stirred, cooled, discharged, washed, and dried to obtain phosphonic acid modified carbon nanotubes. Next, phosphonic acid modified carbon nanotubes and thioacetamide are added to pure water, and after ultrasonic stirring, a metal nitrate is added. The mixture is then heated to 80-90℃ and stirred at a constant temperature for 8-10 hours. After cooling to room temperature, it is filtered, washed, and dried to finally obtain the modified carbon nanotubes. Testing shows that the fluororubber prepared by this invention possesses excellent tear resistance, mechanical properties, and flame retardant properties.

[0007] However, fluororubber also has some limitations, such as relatively poor elasticity, low-temperature performance that needs further improvement, and high cost. These limitations restrict its application in cost-sensitive fields or those requiring good low-temperature elasticity. Overall, however, thanks to its excellent comprehensive properties, fluororubber still holds an important position in industries such as manufacturing, aerospace, and automotive. Summary of the Invention

[0008] In view of the above-mentioned deficiencies of the prior art, the technical problem to be solved by the present invention is to provide a high-temperature resistant fluororubber material for sealing components and a method for preparing the same.

[0009] Fluororubber (FKM) is a highly saturated carbon-chain polymer with a large CF bond energy. The FH bonds form hydrogen bonds through strong van der Waals forces, tightly aligning around the carbon atoms and providing strong shielding for the polymer's CC backbone. The presence of fluorine atoms reduces the flexibility of the fluororubber macromolecular chain, increases its rigidity, and results in poor elasticity, low-temperature performance, and processability. Therefore, to compensate for the insufficient tensile properties of fluororubber, various fillers are often selected to improve its performance. Adding carbon-based fillers such as carbon nanotubes and carbon fibers to fluororubber can simultaneously improve elasticity and low-temperature brittleness under suitable conditions. By enhancing interfacial interactions and optimizing the crosslinking network, elastic recovery and resistance to deformation are improved; by lowering Tg and inhibiting crystallization, the elastic range at low temperatures is broadened, reducing brittle fracture. However, if carbon nanotubes or carbon fibers are unevenly dispersed in fluororubber (e.g., agglomeration), localized stress concentration can occur, failing to improve performance and potentially worsening elasticity and low-temperature brittleness. Therefore, surface modification is usually required to improve dispersion.

[0010] This invention provides a modified carbon nanotube, which is activated by acid followed by acylation and click addition, resulting in dense fluoroalkyl chains grafted onto the surface of the carbon nanotube. This enables it to be thermodynamically compatible with the fluororubber matrix, fundamentally solving the interfacial compatibility problem. Furthermore, the carbon nanotube itself enhances interfacial interactions and optimizes the crosslinking network, improving elastic recovery and deformation resistance, reducing Tg, inhibiting crystallization, broadening the elastic range of the material at low temperatures, improving the elasticity of fluororubber, and reducing the risk of low-temperature brittleness.

[0011] To achieve the above objectives, the present invention provides a high-temperature resistant fluororubber material for sealing components, comprising the following components in parts by weight: 80-120 parts of fluororubber, 3-6 parts of modified carbon nanotubes, 15-25 parts of reinforcing filler, 1-3 parts of vulcanizing agent, 0.2-0.5 parts of accelerator, 2-5 parts of magnesium oxide, and 1-2 parts of lubricant.

[0012] The method for preparing the modified carbon nanotubes includes the following steps:

[0013] X1. Multi-walled carbon nanotubes are added to concentrated nitric acid and dilute sulfuric acid for acidification to obtain activated carbon nanotubes.

[0014] X2. Disperse activated carbon nanotubes in dichloromethane, add undecenoyl chloride and pyridine, heat and stir for 20-30 hours, filter and wash before use in the next step;

[0015] X3. Disperse the product from the previous step with the fluorinated monomer in ethanol, add an initiator, and react under an inert atmosphere and ultraviolet light for 2-3 hours. After filtration, washing, and drying, the modified carbon nanotubes are obtained.

[0016] Furthermore, the mass ratio of the carbon nanotubes, concentrated nitric acid, and dilute sulfuric acid is 1:20~30:5~6.

[0017] Furthermore, the acidification is performed by ultrasonic dispersion at 5-10°C for 6-10 hours.

[0018] Furthermore, the mass ratio of the activated carbon nanotubes, dichloromethane, undecenoyl chloride, and pyridine is 1:100~150:4~5:1~3.

[0019] Furthermore, the mass ratio of the product from the previous step to ethanol, fluorinated monomer, and initiator is 1:50~100:8~12:0.1.

[0020] Furthermore, the fluorinated monomer is one of 1H,1H,2H,2H-perfluorodecylthiol, 1H,1H,2H,2H-perfluorooctylthiol, or 1H,1H,2H,2H-perfluorododecylthiol.

[0021] Preferably, the method for preparing the modified carbon nanotubes includes the following steps:

[0022] X1. Multi-walled carbon nanotubes were added to concentrated nitric acid and dilute sulfuric acid and ultrasonically dispersed at 5-10°C for 6-10 hours. After filtration and washing until neutral, activated carbon nanotubes were obtained. The mass ratio of carbon nanotubes, concentrated nitric acid and dilute sulfuric acid was 1:20-30:5-6.

[0023] X2. Disperse activated carbon nanotubes in dichloromethane, add undecenoyl chloride and pyridine, heat to 35~40℃ and stir for 20~30h, filter and wash before use in the next step. The mass ratio of activated carbon nanotubes, dichloromethane, undecenoyl chloride and pyridine is 1:100~150:4~5:1~3.

[0024] X3. Disperse the product from the previous step and the fluorinated monomer in ethanol, add an initiator, and react under an inert atmosphere and ultraviolet light for 2-3 hours. After filtration, washing, and drying, the modified carbon nanotubes are obtained. The mass ratio of the product from the previous step to ethanol, fluorinated monomer, and initiator is 1:50-100:8-12:0.1.

[0025] Furthermore, the reinforcing filler is silica.

[0026] Furthermore, the vulcanizing agent is bisphenol AF.

[0027] Furthermore, the accelerator is benzyltriphenylphosphine chloride.

[0028] Furthermore, the lubricant is stearic acid.

[0029] The present invention also discloses a method for preparing a high-temperature resistant fluororubber material for sealing components.

[0030] A method for preparing a high-temperature resistant fluororubber material for sealing components includes the following steps:

[0031] S1. After plasticizing the fluororubber thin-walled roll, add magnesium oxide, lubricant and reinforcing filler. After cutting the rubber left and right until it is fully absorbed, add modified carbon nanotubes. After cutting the rubber left and right, make a triangular wrap and thin-walled roll to disperse it evenly. After mixing for 10-20 minutes, wrap the roll and remove the sheet to obtain the masterbatch.

[0032] S2. After wrapping the masterbatch with the roller, mix it with the vulcanizing agent and accelerator. After cutting the rubber to the left and right, make triangular wraps and thin passes to disperse it evenly. After the sheet is produced, vulcanize it.

[0033] S3. Place the rubber compound into the preheated mold for a first-stage vulcanization. After completion, transfer it for a second-stage vulcanization. After completion, cool and mold to obtain the fluororubber material.

[0034] Furthermore, the conditions for the first stage of vulcanization are 170~180℃, 10~20MPa, and 10~20min.

[0035] Furthermore, the conditions for the second-stage vulcanization are 220~240℃ for 6~10h.

[0036] The beneficial effects of this invention are:

[0037] This invention fundamentally solves the interfacial compatibility problem by grafting dense fluoroalkyl chains onto the surface of carbon nanotubes, making them thermodynamically compatible with the fluororubber matrix. Adding the modified carbon nanotubes to fluororubber enhances elastic recovery and deformation resistance, broadens the elastic range of the material at low temperatures, and reduces the risk of low-temperature brittleness. Detailed Implementation

[0038] 1H,1H,2H,2H-Perfluorodecylthiol, CAS No.: 34143-74-3.

[0039] 1H,1H,2H,2H-Perfluorooctylthiol, CAS No.: 34451-26-8.

[0040] 1H,1H,2H,2H-Perfluorododecylthiol, CAS No.: 34451-28-0.

[0041] Photoinitiator 2959 is derived from BASF.

[0042] Fluororubber, grade: FKM246, originates from Shandong Dongyue Huaxia Shenzhou.

[0043] Multi-walled carbon nanotubes with a specific surface area of ​​230~270 m² 2 / g, particle size D 50 ≤10μm, sourced from Core Nano.

[0044] Concentrated nitric acid, 12 mol / L.

[0045] Dilute sulfuric acid, 6 mol / L. Example 1

[0046] A method for preparing a high-temperature resistant fluororubber material for sealing components includes the following steps, in parts by weight:

[0047] S1. After plasticizing 100 parts of fluororubber through a thin pass and roller, add 3 parts of magnesium oxide, 1 part of stearic acid and 20 parts of silica. After cutting the rubber left and right until the powder is fully absorbed, add 4 parts of modified carbon nanotubes. After cutting the rubber left and right, make a triangular pass and thin pass to disperse it evenly. After mixing for 15 minutes, roll the rubber out to obtain the masterbatch.

[0048] S2. After wrapping the masterbatch with rollers, mix it with 2 parts of bisphenol AF and 0.4 parts of benzyltriphenylphosphine chloride. After cutting the rubber on the left and right sides, make triangular wraps and thin passes to make it evenly dispersed. After sheeting, vulcanize it.

[0049] S3. Place the rubber compound into the preheated mold and perform a first-stage vulcanization at 175℃ and 15MPa for 15 minutes. After completion, transfer it to perform a second-stage vulcanization at 230℃ for 8 hours. After completion, cool and mold to obtain the fluororubber material.

[0050] The method for preparing the modified carbon nanotubes includes the following steps:

[0051] X1. Multi-walled carbon nanotubes were added to concentrated nitric acid and dilute sulfuric acid and ultrasonically dispersed at 5°C for 8 hours. After filtration and washing until neutral, activated carbon nanotubes were obtained. The mass ratio of carbon nanotubes, concentrated nitric acid and dilute sulfuric acid was 1:25:6.

[0052] X2. Activated carbon nanotubes are dispersed in dichloromethane, undecenoyl chloride and pyridine are added, the mixture is heated to 40°C and stirred for 24 hours, filtered and washed before being used in the next step. The mass ratio of activated carbon nanotubes, dichloromethane, undecenoyl chloride and pyridine is 1:120:4.7:2.

[0053] X3. Disperse the product from the previous step with 1H,1H,2H,2H-perfluorooctylthiol in ethanol, add photoinitiator 2959, and then incubate under nitrogen atmosphere and 365nm ultraviolet light (1000mW / cm²). 2 The reaction was carried out for 3 hours, and the modified carbon nanotubes were obtained by filtration, washing and drying. The mass ratio of the product from the previous step to ethanol, 1H,1H,2H,2H-perfluorooctyl mercaptan and photoinitiator 2959 was 1:80:10:0.1. Example 2

[0054] The example is basically the same as Example 1, except that 1H,1H,2H,2H-perfluorodecylthiol is used instead of 1H,1H,2H,2H-perfluorooctylthiol. Example 3

[0055] The example is essentially the same as Example 1, except that 1H,1H,2H,2H-perfluorododecylthiol is used instead of 1H,1H,2H,2H-perfluorooctylthiol.

[0056] Compare with Example 1

[0057] A method for preparing a high-temperature resistant fluororubber material for sealing components includes the following steps, in parts by weight:

[0058] S1. After plasticizing 100 parts of fluororubber onto a thin roller, add 3 parts of magnesium oxide, 1 part of stearic acid and 20 parts of silica. After cutting the rubber from left to right until the powder is fully absorbed, mix for 15 minutes and then roll it off the roller to obtain the masterbatch.

[0059] S2. After wrapping the masterbatch with rollers, mix it with 2 parts of bisphenol AF and 0.4 parts of benzyltriphenylphosphine chloride. After cutting the rubber on the left and right sides, make triangular wraps and thin passes to make it evenly dispersed. After sheeting, vulcanize it.

[0060] S3. Place the rubber compound into the preheated mold and perform a first-stage vulcanization at 175℃ and 15MPa for 15 minutes. After completion, transfer it to perform a second-stage vulcanization at 230℃ for 8 hours. After completion, cool and mold to obtain the fluororubber material.

[0061] Compare with Example 2

[0062] A method for preparing a high-temperature resistant fluororubber material for sealing components includes the following steps, in parts by weight:

[0063] S1. After plasticizing 100 parts of fluororubber, add 3 parts of magnesium oxide, 1 part of stearic acid and 20 parts of silica. After cutting the rubber left and right until it is fully absorbed, add 4 parts of multi-walled carbon nanotubes. After cutting the rubber left and right, make a triangular wrap and thin pass to disperse it evenly. After mixing for 15 minutes, wrap the rubber with rollers and sheet it to obtain the masterbatch.

[0064] S2. After wrapping the masterbatch with rollers, mix it with 2 parts of bisphenol AF and 0.4 parts of benzyltriphenylphosphine chloride. After cutting the rubber on the left and right sides, make triangular wraps and thin passes to make it evenly dispersed. After sheeting, vulcanize it.

[0065] S3. Place the rubber compound into the preheated mold and perform a first-stage vulcanization at 175℃ and 15MPa for 15 minutes. After completion, transfer it to perform a second-stage vulcanization at 230℃ for 8 hours. After completion, cool and mold to obtain the fluororubber material.

[0066] Compare with Example 3

[0067] A method for preparing a high-temperature resistant fluororubber material for sealing components includes the following steps, in parts by weight:

[0068] S1. After plasticizing 100 parts of fluororubber through a thin pass and roller, add 3 parts of magnesium oxide, 1 part of stearic acid and 20 parts of silica. After cutting the rubber left and right until the powder is fully absorbed, add 4 parts of modified carbon nanotubes. After cutting the rubber left and right, make a triangular pass and thin pass to disperse it evenly. After mixing for 15 minutes, roll the rubber out to obtain the masterbatch.

[0069] S2. After wrapping the masterbatch with rollers, mix it with 2 parts of bisphenol AF and 0.4 parts of benzyltriphenylphosphine chloride. After cutting the rubber on the left and right sides, make triangular wraps and thin passes to make it evenly dispersed. After sheeting, vulcanize it.

[0070] S3. Place the rubber compound into the preheated mold and perform a first-stage vulcanization at 175℃ and 15MPa for 15 minutes. After completion, transfer it to perform a second-stage vulcanization at 230℃ for 8 hours. After completion, cool and mold to obtain the fluororubber material.

[0071] The method for preparing the modified carbon nanotubes includes the following steps:

[0072] Multi-walled carbon nanotubes were added to concentrated nitric acid and dilute sulfuric acid and ultrasonically dispersed at 5°C for 8 hours. After filtration and washing until neutral, modified carbon nanotubes were obtained. The mass ratio of carbon nanotubes, concentrated nitric acid and dilute sulfuric acid was 1:25:6.

[0073] Test Example 1

[0074] The tensile strength and tear strength of the fluororubber materials prepared in the examples and control examples were tested in accordance with GB / T528-2009 "Determination of tensile stress-strain properties of vulcanized rubber or thermoplastic rubber" and GB / T529-2008 "Determination of tear strength of vulcanized rubber or thermoplastic rubber".

[0075] Table 1

[0076] Experimental protocol Tensile strength / MPa Tear strength / kN / m Example 1 >18.6 46.7 Example 2 >18.6 48.3 Example 3 >18.6 50.2 Compare with Example 1 12.3 30.1 Compare with Example 2 15.1 36.3 Compare with Example 3 17.2 41.4

[0077] As shown in Table 1, the addition of carbon nanotubes effectively improves tensile and tear strength. Carbon nanotubes themselves possess extremely high axial tensile strength, far exceeding that of the fluororubber matrix. When uniformly dispersed in fluororubber, carbon nanotubes act as a nanoscale reinforcing framework, sharing external tensile stress and delaying overall material deformation and fracture. The nanoscale size of carbon nanotubes restricts the free slippage of rubber molecular chains. Especially during stretching, their physical entanglement hinders the directional flow and separation of molecular chains, further enhancing the material's resistance to tensile failure. When the material has micro-cracks and is subjected to stress, the path deflection caused by the nanotubes increases the energy consumption for crack propagation. Carbon nanotubes spanning cracks can also connect the matrix on both sides of the crack, transferring stress through their own tension or bonding force with the matrix, preventing further tearing of the crack.

[0078] However, the test results of the comparative examples show that the modification of carbon nanotubes is crucial for performance improvement. This is because the surface of carbon nanotubes is usually inert and prone to aggregation due to van der Waals forces, making it difficult to disperse uniformly in the polymer matrix. Modification of the carbon nanotube surface enhances the interfacial bonding force with the fluororubber molecular chains. This strong bonding effectively transfers stress from the rubber matrix to the carbon nanotubes, preventing premature fracture due to stress concentration at the interface, thereby improving the overall tensile strength. The modified carbon nanotubes have a tight bond with the fluororubber interface, making it less prone to microcracks at the interface under localized stress, thus reducing the number of tear initiation points. Therefore, the tensile strength and tear strength of Comparative Example 3 are higher than those of Comparative Example 2.

[0079] In the examples, the modified carbon nanotubes were activated with acid followed by acylation and click addition, resulting in dense fluoroalkyl chains grafted onto the surface of the carbon nanotubes. This enabled thermodynamic compatibility with the fluororubber matrix, fundamentally solving the interfacial compatibility problem. Therefore, the performance improvement of the fluororubber was more significant compared to Comparative Example 3. The 1H,1H,2H,2H-perfluorododecanethiol in Example 3 had the longest long-chain alkyl spacer arms compared to Examples 1-2. Tearing is essentially a crack propagation process, and the core role of the long-chain alkyl spacer arms is to greatly hinder and delay this process. When the crack tip extends to the vicinity of the carbon nanotube, the flexible long alkyl chains can effectively absorb and dissipate energy through their significant conformational changes. The flexible long chains firmly anchored to the CNTs are difficult for the crack to directly sever, thus significantly improving the tear strength.

[0080] Test Example 2

[0081] The fluororubber materials prepared in the examples and control examples were tested for low-temperature brittleness in accordance with GB / T 15256-2014 "Determination of Low-Temperature Brittleness of Vulcanized Rubber or Thermoplastic Rubber".

[0082] Table 2

[0083] Experimental protocol Low-temperature brittleness temperature / ℃ Example 1 –32 Example 2 –34 Example 3 –42 Compare with Example 1 –21 Compare with Example 2 –25 Compare with Example 3 –28

[0084] Carbon nanotubes can lower the glass transition temperature (Tg), inhibit crystallization, broaden the elastic range of materials at low temperatures, improve the elasticity of fluororubber, and reduce the risk of low-temperature brittleness. As shown in Table 2, compared to the control example, the fluororubber material in the examples exhibits a lower low-temperature brittleness temperature. This may be because the compatibility issue was fundamentally solved by grafting fluoroalkyl chains onto the surface of the carbon nanotubes in the examples. Furthermore, the long-chain alkyl spacer chains in Example 3, acting as flexible chains, maintain a certain degree of molecular mobility even at lower temperatures. The movement of these flexible chain segments helps lower the effective glass transition temperature of the interface region, allowing the material to maintain a certain degree of flexibility at lower temperatures rather than becoming completely rigid and brittle. Due to its excellent stress dissipation and toughening capabilities, it can withstand temperatures lower than the point at which embrittlement occurs.

[0085] The preferred embodiments of the present invention have been described in detail above. It should be understood that those skilled in the art can make numerous modifications and variations based on the concept of the present invention without creative effort. Therefore, all technical solutions that can be obtained by those skilled in the art based on the concept of the present invention through logical analysis, reasoning, or limited experimentation on the basis of existing technology should be within the scope of protection defined by the claims.

Claims

1. A high-temperature resistant fluororubber material for sealing components, characterized in that, It comprises the following components in parts by weight: 80-120 parts of fluororubber, 3-6 parts of modified carbon nanotubes, 15-25 parts of reinforcing filler, 1-3 parts of vulcanizing agent, 0.2-0.5 parts of accelerator, 2-5 parts of magnesium oxide, and 1-2 parts of lubricant; The method for preparing the modified carbon nanotubes includes the following steps: X1. Multi-walled carbon nanotubes are added to concentrated nitric acid and dilute sulfuric acid for acidification to obtain activated carbon nanotubes. X2. Disperse activated carbon nanotubes in dichloromethane, add undecenoyl chloride and pyridine, heat and stir for 20-30 hours, filter and wash before use in the next step; X3. Disperse the product from the previous step with the fluorinated monomer in ethanol, add an initiator, and react under an inert atmosphere and ultraviolet light for 2-3 hours. After filtration, washing, and drying, the modified carbon nanotubes are obtained.

2. The high-temperature resistant fluororubber material for sealing components as described in claim 1, characterized in that, The mass ratio of the carbon nanotubes, concentrated nitric acid, and dilute sulfuric acid is 1:20~30:5~6.

3. The high-temperature resistant fluororubber material for sealing components as described in claim 1, characterized in that, The acidification process involves ultrasonic dispersion at 5-10°C for 6-10 hours.

4. The high-temperature resistant fluororubber material for sealing components as described in claim 1, characterized in that, The mass ratio of activated carbon nanotubes, dichloromethane, undecenoyl chloride and pyridine is 1:100~150:4~5:1~3.

5. The high-temperature resistant fluororubber material for sealing components as described in claim 1, characterized in that, The mass ratio of the product from the previous step to ethanol, fluorinated monomer, and initiator is 1:50~100:8~12:0.

1.

6. The high-temperature resistant fluororubber material for sealing components as described in claim 1, characterized in that, The reinforcing filler is silica and the vulcanizing agent is bisphenol AF.

7. The high-temperature resistant fluororubber material for sealing components as described in claim 1, characterized in that, The accelerator is benzyltriphenylphosphine chloride, and the lubricant is stearic acid.

8. A method for preparing a high-temperature resistant fluororubber material for sealing components as described in any one of claims 1 to 7, characterized in that, Includes the following steps: S1. After plasticizing the fluororubber thin-walled roll, add magnesium oxide, lubricant and reinforcing filler. After cutting the rubber left and right until it is fully absorbed, add modified carbon nanotubes. After cutting the rubber left and right, make a triangular wrap and thin-walled roll to disperse it evenly. After mixing for 10-20 minutes, wrap the roll and remove the sheet to obtain the masterbatch. S2. After wrapping the masterbatch with the roller, mix it with the vulcanizing agent and accelerator. After cutting the rubber to the left and right, make triangular wraps and thin passes to disperse it evenly. After the sheet is produced, vulcanize it. S3. Place the rubber compound into the preheated mold for a first-stage vulcanization. After completion, transfer it for a second-stage vulcanization. After completion, cool and mold to obtain the fluororubber material.

9. The method for preparing high-temperature resistant fluororubber material for sealing components as described in claim 8, characterized in that, The conditions for the first stage of vulcanization are 170~180℃, 10~20MPa, and 10~20min.

10. The method for preparing high-temperature resistant fluororubber material for sealing components as described in claim 8, characterized in that, The conditions for the two-stage vulcanization are 220~240℃ for 6~10h.