High-temperature-resistant and anti-aging fluorosilicone rubber and preparation method thereof

By using fluorosilicone-based polystyrene as a compatibilizer, the problem of poor compatibility between fluororubber and silicone rubber was solved, and a high-temperature resistant and anti-aging fluoro-silicone rubber with high tensile strength and toughness was prepared, which significantly improved its mechanical properties and heat aging resistance.

CN120699441BActive Publication Date: 2025-12-09DONGGUAN GENDIAN NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202511120158.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-08-12
Publication Date
2025-12-09
Estimated Expiration
2045-08-12

AI Technical Summary

Technical Problem

The significant difference in polarity between fluororubber and silicone rubber results in poor compatibility between the two, severely impacting the mechanical properties of blended rubbers.

Method used

Fluorosilicone-based polystyrene was used as a compatibilizer, and the mixture was prepared by mixing and vulcanization on an open mill to produce a high-temperature resistant and anti-aging fluoro-silicone rubber. The compatibility was improved by utilizing the siloxane and flexible phenyl ether bond structure of fluorosilicone-based polystyrene.

Benefits of technology

It improves the tensile properties and toughness of fluorosilicone rubber, enhances compatibility, improves high-temperature resistance and anti-aging properties, and significantly increases tensile strength and elongation at break.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to the technical field of rubber, and discloses a high-temperature-resistant and anti-aging fluorine-silicon rubber and a preparation method thereof. The high-temperature-resistant and anti-aging fluorine-silicon rubber is obtained by mixing, vulcanizing, etc. of silicon rubber, fluorosilicon-based polystyrene, fillers, fluorine rubber, a cross-linking aid, a vulcanizing agent and the like. The fluorosilicon-based polystyrene improves the compatibility between the fluorine rubber and the silicon rubber, and is beneficial to improving the tensile property and the high-temperature-resistant and anti-aging property of the fluorine-silicon rubber. The fluorosilicon-based polystyrene contains a polystyrene structure, has high strength, and is grafted with a large number of flexible phenyl ether structures. When the fluorosilicon-based polystyrene is added into the fluorine-silicon rubber, the strength and the toughness of the fluorine-silicon rubber can be improved, and the fluorine-silicon rubber has higher tensile strength and elongation at break.
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Description

TECHNICAL FIELD

[0001] The application relates to the rubber technology field, in particular to a high-temperature-resistant and anti-aging fluorine-silicon rubber and a preparation method thereof. BACKGROUND

[0002] The fluorine-silicon rubber has the high-temperature resistance and corrosion resistance of fluorine rubber and the low-temperature resistance, elasticity and electrical insulation of silicon rubber, and is widely applied in the fields of aerospace, automobile manufacturing, electronics and the like. However, the polarity difference between fluorine rubber and silicon rubber is large, which leads to poor compatibility of the two, and seriously affects the mechanical properties of the fluorine-silicon rubber.

[0003] It is a research difficulty to develop a new type of compatibilizer for fluorine rubber and silicon rubber. The patent with the publication number CN115678184B discloses a fluorine rubber and silicon rubber blend and a preparation method thereof. The long-chain fluorine-containing compatibilizing modifier is used to modify the silicon rubber, and the silicon rubber grafted with the fluorine-containing modifier is obtained, which is used as a compatibilizer to improve the problem of poor compatibility of fluorine rubber and silicon rubber. However, the elongation at break of the blend is low, and the toughness is poor. Compared with the patent, the fluorine-silicon rubber of the application improves the elongation at break and other tensile properties, high-temperature resistance and anti-aging properties of the fluorine-silicon rubber by using fluorine-silicon-based polystyrene. SUMMARY

[0004] (I) The technical problem solved by the application: in view of the deficiencies of the prior art, the application provides a high-temperature-resistant and anti-aging fluorine-silicon rubber and a preparation method thereof, solves the problem of poor compatibility of fluorine rubber and silicon rubber, and improves the mechanical properties, high-temperature resistance and anti-aging properties of the fluorine-silicon rubber.

[0005] (II) The technical solution of the application: a preparation method of a high-temperature-resistant and anti-aging fluorine-silicon rubber:

[0006] Step S1: silicon rubber is added to an open mill, and after the roller is wrapped, fluorine-silicon-based polystyrene, fillers and structure control agents are added. After mixing, thin passing and sheeting are performed, and the silicon rubber mixing rubber is obtained.

[0007] Step S2: fluorine rubber is added to the open mill, and after the roller is wrapped, an acid absorbent is added. After the material is eaten, a triangular bag and a roll are punched, the silicon rubber mixing rubber prepared in step S1 is added, and after mixing, an auxiliary crosslinking agent and a vulcanizing agent are added. Thin passing and sheeting are performed, and then vulcanization is performed, to obtain the high-temperature-resistant and anti-aging fluorine-silicon rubber.

[0008] Further, the mass ratio of the silicon rubber, the fluorine-silicon-based polystyrene, the fillers, the structure control agents, the fluorine rubber, the acid absorbent, the auxiliary crosslinking agent and the vulcanizing agent is (50-80):(5-20):(15-35):(3-7):(20-50):(3.6-8.2):(3-4):(2.4-3.2).

[0009] Further, the filler is carbon black or white carbon black.

[0010] Further, the structure control agent is hydroxyl silicone oil.

[0011] Further, the acid absorption agent includes calcium hydroxide, magnesium oxide.

[0012] Further, the vulcanizing agent includes dicumyl peroxide, bis-25.

[0013] Further, the auxiliary crosslinking agent is triallyl isocyanurate.

[0014] Further, the vulcanization process is first vulcanized in a flat vulcanizing machine at 160-170 DEG C for 3-6 min, and then vulcanized in a forced air drying oven at 230-250 DEG C for 2-3 h.

[0015] Further, the preparation method of the fluorosilicon-based polystyrene comprises:

[0016] (1) adding 100: (130-150) 1,1,3,3-tetramethyl-1,3-di[3-(epoxyethyl methoxy) propyl] disiloxane, 4,4'-bis(4-amino-2-trifluoromethyl phenoxy) diphenyl ether into isopropyl alcohol, heating to 40-60 DEG C, stirring for 8-12 h, filtering after cooling, washing the product with ethanol, and drying to obtain the fluorosilicon polymer.

[0017]

[0018] (2) adding chloromethyl polystyrene and the fluorosilicon polymer into N,N-dimethylformamide, stirring, and then adding sodium hydroxide aqueous solution, controlling the mass ratio of chloromethyl polystyrene, the fluorosilicon polymer and sodium hydroxide to be 100: (25-60): (4-10); heating to 60-75 DEG C, stirring for 18-24 h, diluting by adding water, filtering, and then washing the product with water, ethanol and dichloromethane in sequence, and drying to obtain the fluorosilicon-based polystyrene.

[0019] (Three) beneficial technical effects: the 1,1,3,3-tetramethyl-1,3-di[3-(epoxyethyl methoxy) propyl] disiloxane and 4,4'-bis(4-amino-2-trifluoromethyl phenoxy) diphenyl ether are subjected to ring-opening polymerization reaction to obtain the fluorosilicon-based polystyrene containing imino, siloxane and flexible phenyl ether bond, then under the catalysis of sodium hydroxide, the imino of the fluorosilicon-based polystyrene and the chloromethyl of the chloromethyl polystyrene are subjected to substitution reaction to obtain the fluorosilicon-based polystyrene, and finally the fluorosilicon-based polystyrene is mixed and vulcanized with silicone rubber, fluororubber and the like to obtain the high-temperature-resistant and anti-aging fluorine-silicone rubber.

[0020] The fluorosilicon-based polystyrene of the present application is grafted with siloxane and fluorine-containing groups, has high structural similarity with fluororubber and silicone rubber, can play a compatibilizing role, improves the compatibility between fluororubber and silicone rubber, is beneficial to improving the tensile properties of fluorine-silicone rubber, and makes the fluororubber and silicone rubber form a uniform dispersed phase, so that the rubber has better high-temperature resistance and aging resistance.

[0021] The fluorosilicon-based polystyrene of the present application contains a polystyrene structure, has high strength, and is grafted with a large number of flexible phenyl ether structures, so that when added to fluorine-silicone rubber, the strength and toughness of the fluorine-silicone rubber can be improved, and the fluorine-silicone rubber has higher tensile strength and elongation at break. DETAILED DESCRIPTION

[0022] In order to make the technical solutions of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. It should be noted that the following embodiments are only used to better understand the technical solutions of the present application, and should not be understood as a limitation of the present application.

[0023] The silicone rubber described below is methyl vinyl silicone rubber, model RBG-0611, from Guangzhou Shenkai Trade Co., Ltd. The fluororubber is model PFE 133TB, from Shanghai Xianshun Plastic Co., Ltd. The chloromethyl polystyrene resin is from Wuhan Yujing Jiaheng Pharmaceutical Co., Ltd.

[0024] 4,4'-bis(4-amino-2-trifluoromethylphenoxy) diphenyl ether is prepared according to the method in the journal “Polymer Bulletin”, January 2010, No. 1, document “Synthesis and characterization of polyimide film material based on phenyl ether type fluorine-containing diamine”, and has a structural formula of

[0025] Example 1

[0026] (1) 20 g (55.2 mmol) of 1,1,3,3-tetramethyl-1,3-di[3-(epoxyethylmethoxy)propyl] disiloxane, 28.7 g (55.2 mmol) of 4,4'-bis(4-amino-2-trifluoromethylphenoxy) diphenyl ether were added to 400 mL of isopropyl alcohol, heated to 60°C, stirred for 8 h, cooled, filtered, the product was washed with ethanol, and dried to obtain a fluorosilicon polymer.

[0027] (2) 60 g of chloromethyl polystyrene, 15 g of fluorosilicon polymer were added to 700 mL of N,N-dimethylformamide, 10 mL of an aqueous solution containing 2.4 g of sodium hydroxide was added after stirring, heated to 70°C, stirred for 24 h, diluted with water, filtered, and the product was washed with water, ethanol, and dichloromethane in sequence, and dried to obtain fluorosilicon-based polystyrene.

[0028] (3) Put 800 g of silicone rubber into an open mill, and after rolling, add 50 g of fluorosilicon-based polystyrene, 350 g of white carbon black, and 70 g of hydroxyl silicone oil. After mixing, thin pass and sheeting to obtain a silicone rubber mixing gum.

[0029] (4) Put 200 g of fluorine rubber into an open mill, and after rolling, add 12 g of calcium hydroxide and 24 g of magnesium oxide. After eating the material, make a triangular bag and a roll. Add the silicone rubber mixing gum prepared in (3). After mixing, add 30 g of triallyl isocyanurate and 27 g of dicumyl peroxide. Thin pass and sheeting, and then in a flat vulcanizing machine, vulcanize at 160°C for 6 min. Finally, in a blast drying oven, vulcanize at 250°C for 2 h to obtain a high-temperature-resistant and anti-aging fluorine-silicon rubber.

[0030] Example 2:

[0031] (1) Add 20 g of 1,1,3,3-tetramethyl-1,3-di[3-(epoxyethyl methoxy) propyl] disiloxane and 30 g of 4,4'-bis(4-amino-2-trifluoromethyl phenoxy) diphenyl ether to 400 mL of isopropyl alcohol. Heat to 60°C and stir for 8 h. After cooling, filter, wash the product with ethanol, and dry to obtain a fluorosilicon polymer.

[0032] (2) Add 60 g of chloromethyl polystyrene and 36 g of fluorosilicon polymer to 900 mL of N,N-dimethylformamide. After stirring, add 15 mL of an aqueous solution containing 6 g of sodium hydroxide. Heat to 60°C and stir for 24 h. Dilute with water, filter, and then wash the product with water, ethanol, and dichloromethane in sequence. Dry to obtain fluorosilicon-based polystyrene.

[0033] (3) Put 650 g of silicone rubber into an open mill, and after rolling, add 120 g of fluorosilicon-based polystyrene, 250 g of carbon black, and 50 g of hydroxyl silicone oil. After mixing, thin pass and sheeting to obtain a silicone rubber mixing gum.

[0034] (4) Put 350 g of fluorine rubber into an open mill, and after rolling, add 20 g of calcium hydroxide and 40 g of magnesium oxide. After eating the material, make a triangular bag and a roll. Add the silicone rubber mixing gum prepared in (3). After mixing, add 33 g of triallyl isocyanurate, 27 g of dicumyl peroxide, and 24 g of bis-25. Thin pass and sheeting, and then in a flat vulcanizing machine, vulcanize at 170°C for 3 min. Finally, in a blast drying oven, vulcanize at 230°C for 3 h to obtain a high-temperature-resistant and anti-aging fluorine-silicon rubber.

[0035] Example 3:

[0036] (1) To 300 mL of isopropyl alcohol, 20 g of 1,1,3,3-tetramethyl-1,3 di[3- (epoxyethylmethoxy) propyl] disiloxane, 26 g of 4,4'-bis (4-amino-2- trifluoromethylphenoxy) diphenyl ether were added, heated to 50°C, stirred for 8 h, after cooling, filtered, the product was washed with ethanol, dried to obtain fluorosilicon polymer.

[0037] (2) To 900 mL of N,N-dimethylformamide, 60 g of chloromethyl polystyrene, 25 g of fluorosilicon polymer were added, after stirring, 12 mL of 4 g of sodium hydroxide aqueous solution was added, heated to 75°C, stirred for 18 h, diluted with water, after filtration, the product was washed with water, ethanol, dichloromethane in turn, dried to obtain fluorosilicon-based polystyrene.

[0038] (3) 500 g of silicone rubber was added to the open mill, after rolling, 200 g of fluorosilicon-based polystyrene, 150 g of white carbon black, 30 g of hydroxyl silicone oil were added, after mixing, thin pass, sheeting, to obtain silicone rubber mixing rubber.

[0039] (4) 500 g of fluorine rubber was added to the open mill, after rolling, 30 g of calcium hydroxide, 52 g of magnesium oxide were added, after eating, triangle bag, roll, the silicone rubber mixing rubber prepared in (3) was added, after mixing, 40 g of triallyl isocyanurate, 32 g of dicumyl peroxide were added, thin pass, sheeting, then in the flat vulcanizing machine, 165°C vulcanization for 4 min, finally in the air drying oven, 250°C vulcanization for 2 h, to obtain high-temperature resistant and anti-aging fluorine-silicon rubber.

[0040] Comparative Example 1:

[0041] (1) 800 g of silicone rubber was added to the open mill, after rolling, 350 g of white carbon black, 70 g of hydroxyl silicone oil were added, after mixing, thin pass, sheeting, to obtain silicone rubber mixing rubber.

[0042] (2) 200 g of fluorine rubber was added to the open mill, after rolling, 12 g of calcium hydroxide, 24 g of magnesium oxide were added, after eating, triangle bag, roll, the silicone rubber mixing rubber prepared in (1) was added, after mixing, 30 g of triallyl isocyanurate, 27 g of dicumyl peroxide were added, thin pass, sheeting, then in the flat vulcanizing machine, 160°C vulcanization for 6 min, finally in the air drying oven, 250°C vulcanization for 2 h, to obtain fluorine-silicon rubber.

[0043] Comparative Example 2:

[0044] (1) 800 g of silicone rubber was added to the open mill, after rolling, 50 g of chloromethyl polystyrene, 350 g of white carbon black, 70 g of hydroxyl silicone oil were added, after mixing, thin pass, sheeting, to obtain silicone rubber mixing rubber.

[0045] (2) Put 200 g of fluorine rubber into an open mill, after rolling, add 12 g of calcium hydroxide and 24 g of magnesium oxide, after eating the material, make a triangular bag and a roll, add the silicone rubber compound prepared in (1), after mixing, add 30 g of triallyl isocyanurate and 27 g of dicumyl peroxide, thin pass and sheeting, then in a flat vulcanizing machine, vulcanize at 160 °C for 6 min, finally in a blast drying oven, vulcanize at 250 °C for 2 h, to obtain fluorine-silicon rubber.

[0046] Comparative Example 3

[0047] (1) Add 20 g of 1,1,3,3-tetramethyl-1,3-di[3-(epoxyethyl methoxy) propyl] disiloxane, 18.4 g (55.2 mmol) of 2,2-bis(4-aminophenyl) hexafluoropropane (CAS No. 1095-78-9) to 400 mL of isopropyl alcohol, heat to 60 °C, stir for 8 h, cool and filter, wash the product with ethanol and dry to obtain a fluorosilicon polymer.

[0048] (2) Add 60 g of chloromethyl polystyrene and 15 g of fluorosilicon polymer to 700 mL of N,N-dimethylformamide, after stirring, add 10 mL of an aqueous solution containing 2.4 g of sodium hydroxide, heat to 70 °C, stir for 24 h, dilute with water, filter, and wash the product with water, ethanol and dichloromethane in turn, and dry to obtain fluorosilicon-based polystyrene.

[0049] (3) Put 800 g of silicone rubber into an open mill, after rolling, add 50 g of fluorosilicon-based polystyrene, 350 g of white carbon black and 70 g of hydroxyl silicone oil, after mixing, thin pass and sheeting to obtain a silicone rubber compound.

[0050] (4) Put 200 g of fluorine rubber into an open mill, after rolling, add 12 g of calcium hydroxide and 24 g of magnesium oxide, after eating the material, make a triangular bag and a roll, add the silicone rubber compound prepared in (3), after mixing, add 30 g of triallyl isocyanurate and 27 g of dicumyl peroxide, thin pass and sheeting, then in a flat vulcanizing machine, vulcanize at 160 °C for 6 min, finally in a blast drying oven, vulcanize at 250 °C for 2 h, to obtain fluorine-silicon rubber.

[0051] Comparative Example 4

[0052] (1) Add 9.6 g (55.2 mmol) of ethylene glycol diglycidyl ether and 27.2 g of 4,4'-bis(4-amino-2-trifluoromethyl phenoxy) diphenyl ether to 400 mL of isopropyl alcohol, heat to 60 °C, stir for 8 h, cool and filter, wash the product with ethanol and dry to obtain a fluorine-containing polymer.

[0053] (2) Into 700 mL of N,N-dimethylformamide, 60 g of chloromethyl polystyrene and 15 g of fluorine-containing polymer were added, after stirring, 10 mL of an aqueous solution containing 2.4 g of sodium hydroxide was added, heated to 70°C, and stirred for 24 h. After dilution with water, the product was filtered and washed with water, ethanol, and dichloromethane in sequence, and dried to obtain fluorine-containing polystyrene.

[0054] (3) 800 g of silicone rubber was added to an open mill, and after wrapping the roller, 50 g of fluorine-containing polystyrene, 350 g of white carbon black, and 70 g of hydroxyl silicone oil were added. After mixing, thin passing and sheeting were performed to obtain a silicone rubber mixing gum.

[0055] (4) 200 g of fluorine-containing rubber was added to an open mill, and after wrapping the roller, 12 g of calcium hydroxide and 24 g of magnesium oxide were added. After eating the material, a triangular bag and a roll were punched. The silicone rubber mixing gum prepared in (3) was added, and after mixing, 30 g of triallyl isocyanurate and 27 g of dicumyl peroxide were added. Thin passing and sheeting were performed, and then in a flat vulcanizing machine, 160°C vulcanization was performed for 6 min. Finally, in a blast drying oven, 250°C vulcanization was performed for 2 h to obtain a fluorine-silicone rubber.

[0056] Comparative Example 5:

[0057] (1) The silicone rubber grafted with methyl methacrylate-2,2,2-trifluoroethyl ester was prepared according to the method of the literature “Compatibilization of Fluororubber / Silicone Rubber Blends by MVQ-g-TFEMA” in the journal “Elastomer” 2010, No. 2, 25-28.

[0058] (2) 800 g of silicone rubber was added to an open mill, and after wrapping the roller, 50 g of silicone rubber grafted with methyl methacrylate-2,2,2-trifluoroethyl ester, 350 g of white carbon black, and 70 g of hydroxyl silicone oil were added. After mixing, thin passing and sheeting were performed to obtain a silicone rubber mixing gum.

[0059] (3) 200 g of fluorine-containing rubber was added to an open mill, and after wrapping the roller, 12 g of calcium hydroxide and 24 g of magnesium oxide were added. After eating the material, a triangular bag and a roll were punched. The silicone rubber mixing gum prepared in (2) was added, and after mixing, 30 g of triallyl isocyanurate and 27 g of dicumyl peroxide were added. Thin passing and sheeting were performed, and then in a flat vulcanizing machine, 160°C vulcanization was performed for 6 min. Finally, in a blast drying oven, 250°C vulcanization was performed for 2 h to obtain a fluorine-silicone rubber.

[0060] The tensile properties of the fluorine-silicone rubber were tested according to GB / T 528-2009. The fluorine-silicone rubber was placed in a blast drying oven and heat aged at 180°C for 120 h. The rubber was taken out and left to stand at room temperature for 24 h before testing the tensile properties.

[0061] Table 1 Performance Test

[0062]

[0063] The fluororubber and silicone rubber of Comparative Example 1 have poor compatibility, resulting in low tensile strength and elongation at break of the fluorine-silicon rubber, and low retention rate of the tensile strength and elongation at break of the rubber after heat aging, poor high-temperature resistance and aging resistance.

[0064] Examples 1 to 3 add fluorosilicon-based polystyrene, which is grafted with polystyrene containing siloxane and fluorine-containing groups, and has high structural similarity with fluororubber and silicone rubber, which can play a role in compatibilization of fluorosilicon-based polystyrene, improve the compatibility between fluororubber and silicone rubber, and be beneficial to improve the tensile properties of fluorine-silicon rubber. The fluororubber and silicone rubber form a uniform dispersed phase, so that the rubber has better high-temperature resistance and aging resistance. After heat aging, the rubber has high retention rate of tensile strength and elongation at break. At the same time, fluorosilicon-based polystyrene contains polystyrene structure with high strength, and a large number of flexible phenyl ether structures, which can improve the strength and toughness of the rubber when added to the fluorine-silicon rubber, and has higher tensile strength and elongation at break.

[0065] Comparative Example 2 only adds chloromethyl polystyrene, which cannot play a role in compatibilization of fluororubber and silicone rubber, and the reinforcing and compatibilizing effect of chloromethyl polystyrene is poor, resulting in low tensile properties of the rubber, and low retention rate of tensile strength and elongation at break after heat aging, poor high-temperature resistance and aging resistance.

[0066] 2,2-bis(4-aminophenyl) hexafluoropropane of Comparative Example 3 does not contain flexible phenyl ether bonds, and the prepared fluorosilicon polymer and fluorosilicon-based polystyrene do not contain flexible phenyl ether bonds, which is difficult to effectively improve the toughness and elongation at break of the fluorine-silicon rubber, and is significantly lower than Example 1.

[0067] Ethylene glycol diglycidyl ether of Comparative Example 4 does not contain siloxane bonds, and the prepared fluorine-containing polymer and fluorine-containing polystyrene do not contain siloxane bonds, which cannot play a role in compatibilization of fluororubber and silicone rubber, resulting in low tensile properties of the fluorine-silicon rubber, and low retention rate of tensile strength and elongation at break after heat aging, poor high-temperature resistance and aging resistance.

[0068] Comparative Example 5 uses conventional rubber grafted methyl methacrylate-2,2,2-trifluoroethyl ester as a compatibilizer for fluororubber and silicone rubber, which does not contain polystyrene molecular chains and flexible phenyl ether bonds, resulting in significantly lower tensile strength and elongation at break of the fluorine-silicon rubber than Example 1.

Claims

1. A process for the preparation of a high temperature and ageing resistant fluoro-silicone rubber, characterized in that, The preparation method comprises the following steps: S1, adding silicone rubber into an open mill, adding fluorosilicon-based polystyrene, filler, structure control agent after roll wrapping, thin passing after mixing, sheeting down to obtain silicone rubber mixing rubber; S2, adding fluoro rubber into the open mill, adding acid absorbent after roll wrapping, triangular bagging and rolling after material eating, adding the silicone rubber mixing rubber prepared in step S1, adding auxiliary crosslinking agent and vulcanizing agent after mixing, thin passing, sheeting down, and then vulcanizing to obtain high-temperature-resistant and anti-aging fluorine-silicon rubber. The mass ratio of the silicone rubber, fluorosilicon-based polystyrene, filler, structure control agent, fluoro rubber, acid absorbent, auxiliary crosslinking agent and vulcanizing agent is (50-80):(5-20):(15-35):(3-7):(20-50):(3.6-8.2):(3-4):(2.4-3.2). The preparation method of the fluorosilicon-based polystyrene comprises the following steps: (1) adding 1,1,3,3-tetramethyl-1,3-di[3-(epoxyethyl methoxy) propyl] disiloxane and 4,4'-bis(4-amino-2-trifluoromethyl phenoxy) diphenyl ether into isopropyl alcohol, heating to 40-60 DEG C, stirring for 8-12 h, filtering after cooling, washing the product, and drying to obtain fluorosilicon polymer; (2) adding chloromethyl polystyrene and fluorosilicon polymer into N,N-dimethyl formamide, stirring, adding sodium hydroxide aqueous solution, heating to 60-75 DEG C, stirring for 18-24 h, diluting with water, filtering, washing the product, and drying to obtain fluorosilicon-based polystyrene. The filler is carbon black or white carbon black, and the structure control agent is hydroxyl silicone oil.

2. The process for the preparation of high temperature and ageing resistant fluoro-silicone rubber according to claim 1, characterized in that, The acid absorbent is one or more of calcium hydroxide and magnesium oxide.

3. The process for the preparation of high temperature and ageing resistant fluoro-silicone rubber according to claim 1, characterized in that, The vulcanizing agent is dicumyl peroxide or bis-25, and the auxiliary crosslinking agent is triallyl isocyanurate.

4. The process for preparing high temperature resistant and anti-aging fluoro-silicone rubber according to claim 1, characterized in that, The vulcanizing process is first vulcanizing at 160-170 DEG C for 3-6 min in a flat vulcanizing machine, and then middle vulcanizing at 230-250 DEG C for 2-3 h in a blast drying oven.

5. The process for preparing high temperature resistant and anti-aging fluoro-silicone rubber according to claim 1, characterized in that, The mass ratio of 1,1,3,3-tetramethyl-1,3-di[3-(epoxyethyl methoxy) propyl] disiloxane and 4,4'-bis(4-amino-2-trifluoromethyl phenoxy) diphenyl ether in step (1) is 100:(130-150).

6. The process for the preparation of high temperature and ageing resistant fluoro-silicone rubber according to claim 1, characterized in that, The mass ratio of chloromethyl polystyrene, fluorosilicon polymer and sodium hydroxide in step (2) is 100:(25-60):(4-10).

7. The process for the preparation of high temperature and aging resistant fluoro-silicone rubber according to claim 1, characterized in that, 8. High-temperature-resistant and anti-aging fluorine-silicon rubber prepared by the preparation method in any one of claims 1-7. ​

Citation Information

Patent Citations

  • A kind of fluororubber and silicone rubber combined rubber and preparation method thereof

    CN115678184B

  • Blend of fluorubber and silastic, and preparation thereof

    CN101412835A

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    CN112646294A