CN111117261A - High-temperature-resistant fluorine silicon rubber material - Google Patents
High-temperature-resistant fluorine silicon rubber material Download PDFInfo
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- CN111117261A CN111117261A CN202010012029.7A CN202010012029A CN111117261A CN 111117261 A CN111117261 A CN 111117261A CN 202010012029 A CN202010012029 A CN 202010012029A CN 111117261 A CN111117261 A CN 111117261A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a high-temperature-resistant fluorine-silicon rubber material which is prepared by uniformly mixing the following components in an internal mixer, an open mill or a kneading machine: raw fluorosilicone rubber, white carbon black, hydroxyl fluorosilicone oil, vinyl fluorosilicone oil, phenyl silicone oil, nano oxide and a vulcanizing agent. The fluorosilicone rubber material can be used in a high-temperature environment of 250-300 ℃ after being vulcanized, has excellent oil resistance, and is suitable for being used as a high-temperature sealing element and a high-temperature oil-resistant pipe.
Description
Technical Field
The invention relates to the technical field of organic silicon and fluorine materials, and mainly relates to a high-temperature-resistant fluorine-containing silicone rubber material.
Background
The fluorosilicone rubber has the characteristics of excellent high and low temperature resistance, high resilience, low pressure change, oil resistance, solvent resistance, chemical corrosion resistance, low surface tension and the like, and can be called as an elastomer material with the best comprehensive performance. After decades of development, the material becomes a special material which is irreplaceable in important fields (such as aerospace, national defense military industry, automobile industry and the like). Generally speaking, the long-term service temperature of the fluorosilicone rubber is-60 to 200 ℃, and at higher temperature, the fluorosilicone rubber is easy to cause thermal oxidation aging and fail. With the advancement of technology, many components are increasingly demanding in terms of materials. For example, the sealing ring of the new-generation missile turbofan engine has the advantages of high low-temperature sealing property, RP-3 jet fuel resistance and certain fluorine-silicon lubricating oil resistance and excellent long-term storage property, and is required to bear the high-temperature environment of 250 ℃ during working. With the rapid development of the turbocharging technology, the temperature resistance requirement of the turbocharging pipe material is higher and higher, and as the most ideal material of the turbocharging pipe, the high temperature resistance of the fluorosilicone rubber is gradually insufficient, so that the high temperature resistant fluorosilicone rubber has great use value.
At present, the fluorosilicone rubber material on the market can only be used below 250 ℃, the fluorosilicone rubber material which can be used in a high-temperature environment of 250-300 ℃ is few, and the high-temperature resistant fluorosilicone rubber material has urgent requirements.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant fluorine-containing silicone rubber material which can be used in an environment of 250-300 ℃.
In order to realize the purpose, the invention adopts the following formula and preparation process:
the rubber composition is prepared by uniformly mixing the following components in parts by weight in an internal mixer, an open mill or a kneading machine:
100 parts of crude fluorosilicone rubber
20 to 50 portions of white carbon black
0-15 parts of hydroxyl fluorine silicone oil
0-5 parts of vinyl fluorosilicone oil
0-10 parts of phenyl silicone oil
0 to 10 parts of nano oxide
0-3 parts of vulcanizing agent
The crude fluorosilicone rubber has the following molecular structure:
R1O[Si(CH3)(CH2CH2CF3)]x[Si(CH3)R2]y[Si(CH3)(CH=CH2)]zR1
wherein R is1is-H, -CH3、-CH2CH3、-Si(CH3)3、-Si(CH3)2(CH=CH2) or-Si (CH)3)2(C6H5)；R2is-H, -CH3、-CH2CH3or-C6H5；x=1000~8000, y=0~5000, z=1~100；
Further, the white carbon black has a specific surface area of not less than 50 m2(ii) nano silica per gram;
furthermore, the phenyl silicone oil contains-Si (CH) in the molecule3)(C6H5) An oligomer of O-structural units having a viscosity of 200 to 2000 mPas;
further, the nano oxide is at least one of iron oxide, cerium oxide, nickel oxide, tin oxide, cobalt oxide, copper oxide, manganese oxide and chromium oxide with the average particle size of 20-5000 nm.
Further, the vulcanizing agent is the vulcanizing agent, and the effective component of the vulcanizing agent is one of bis-tetra-bis-penta, benzoyl peroxide and dicumyl peroxide.
Compared with the prior art, the invention has the beneficial effects that:
the invention can adopt but not limited to the following preparation processes: sequentially adding crude fluorosilicone rubber, hydroxyl fluorosilicone oil, vinyl fluorosilicone oil, phenyl silicone oil, white carbon black and nano oxide into an internal mixer or a kneading machine, uniformly mixing at 100-180 ℃, carrying out heat treatment at 100-180 ℃ for 0-4 h, and uniformly mixing the obtained rubber compound and a vulcanizing agent on an open mill to obtain the high-temperature-resistant fluorosilicone rubber compound.
The nanometer oxide and the phenyl silicone oil are used as the heat-resistant auxiliary agent of the fluorine-silicon adhesive, so that the heat resistance of the fluorine-silicon adhesive is obviously improved on the basis of not influencing the basic physical properties of the fluorine-silicon adhesive, and the fluorine-silicon adhesive has higher practicability.
Detailed Description
Example 1
Adding 100 parts by weight of fluorosilicone raw rubber (FSIR-0102, molecular weight 80 ten thousand, vinyl content 0.2 wt%) and 10 parts by weight of hydroxyfluorosilicone oil (FSIR-0901, average particle size 200 nm) into an internal mixer, uniformly mixing at 150 ℃, carrying out heat treatment at 150 ℃ for 2 hours, and uniformly mixing 1 part by weight of Bierwu and the mixed rubber on an open mill to obtain the high-temperature-resistant fluorosilicone mixed rubber.
And testing the basic performance and the aging performance of the rubber compound, wherein the primary vulcanization condition is 170 ℃ multiplied by 10min, the secondary vulcanization condition is 200 ℃ multiplied by 4 h, the compression permanent deformation test condition is 177 ℃ multiplied by 22 h, and the aging condition is 250 ℃ multiplied by 70 h. The samples were tested for hardness, tensile strength and elongation at break before and after aging according to ASTM D2240 and ASTM D412, respectively.
Example 2
Adding 100 parts by weight of fluorosilicone raw rubber (the content of vinyl structural units is 0.2 wt%), 4 parts by weight of phenyl silicone oil, 35 parts by weight of Aerosil R812 and 3 parts by weight of cerium oxide (the average particle size is 500 nm) into an internal mixer, uniformly mixing at 120 ℃, and then uniformly mixing 1 part by weight of dipentadine and the mixed rubber on an open mill to obtain the high-temperature-resistant fluorine-silicon mixed rubber material.
And testing the basic performance and the aging performance of the rubber compound, wherein the primary vulcanization condition is 170 ℃ multiplied by 10min, the secondary vulcanization condition is 200 ℃ multiplied by 4 h, the compression permanent deformation test condition is 177 ℃ multiplied by 22 h, and the aging condition is 250 ℃ multiplied by 70 h. The samples were tested for hardness, tensile strength and elongation at break before and after aging according to ASTM D2240 and ASTM D412, respectively.
Comparative example
And (3) uniformly mixing 100 parts by weight of Silastic LS4-9060 and 1 part by weight of Biwu on an open mill to obtain the fluorosilicone rubber compound.
And testing the basic performance and the aging performance of the rubber compound, wherein the primary vulcanization condition is 170 ℃ multiplied by 10min, the secondary vulcanization condition is 200 ℃ multiplied by 4 h, the compression permanent deformation test condition is 177 ℃ multiplied by 22 h, and the aging condition is 250 ℃ multiplied by 70 h. The samples were tested for hardness, tensile strength and elongation at break before and after aging according to ASTM D2240 and ASTM D412, respectively.
The test results of the examples and comparative examples are summarized as follows:
and (4) conclusion: in the comparative example, the performance of the imported fluorosilicone adhesive is seriously reduced after aging at 250 ℃ for 70 h, which indicates that the fluorosilicone adhesive can not be used at 250 ℃ for a long time. The rubber compound provided by the invention still keeps good performance after being aged under the same condition, which shows that the technical scheme provided by the invention has good effect, and the provided high-temperature resistant fluorine silica gel rubber compound can be used at 250 ℃.
Claims (5)
1. The high-temperature-resistant fluorine-silicon rubber material is characterized by being prepared by uniformly mixing the following components in parts by weight in an internal mixer, an open mill or a kneading machine:
100 parts of crude fluorosilicone rubber
20 to 50 portions of white carbon black
0-15 parts of hydroxyl fluorine silicone oil
0-5 parts of vinyl fluorosilicone oil
0-10 parts of phenyl silicone oil
0 to 10 parts of nano oxide
0-3 parts of vulcanizing agent
The crude fluorosilicone rubber has the following molecular structure:
R1O[Si(CH3)(CH2CH2CF3)]x[Si(CH3)R2]y[Si(CH3)(CH=CH2)]zR1
wherein R is1is-H, -CH3、-CH2CH3、-Si(CH3)3、-Si(CH3)2(CH=CH2) or-Si (CH)3)2(C6H5)；R2is-H, -CH3、-CH2CH3or-C6H5；x=1000~8000, y=0~5000, z=1~100。
2. The high temperature resistant fluorosilicone rubber material of claim 1, wherein: the white carbon black has a specific surface area of not less than 50 m2Per g of nanosilica.
3. The high temperature resistant fluorosilicone rubber material of claim 1, wherein: phenyl silicone oil is a silicone oil containing-Si (CH) in the molecule3)(C6H5) An oligomer of O-structural units having a viscosity of 200 to 2000 mPas.
4. The high temperature resistant fluorosilicone rubber material of claim 1, wherein: the nano oxide is at least one of iron oxide, cerium oxide, nickel oxide, tin oxide, cobalt oxide, copper oxide, manganese oxide and chromium oxide with the average particle size of 20-5000 nm.
5. The high temperature resistant fluorosilicone rubber material of claim 1, wherein: the vulcanizing agent is the vulcanizing agent, and the effective component of the vulcanizing agent is one of bis-tetra-bis-penta, benzoyl peroxide and dicumyl peroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010012029.7A CN111117261A (en) | 2020-01-07 | 2020-01-07 | High-temperature-resistant fluorine silicon rubber material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010012029.7A CN111117261A (en) | 2020-01-07 | 2020-01-07 | High-temperature-resistant fluorine silicon rubber material |
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| CN111117261A true CN111117261A (en) | 2020-05-08 |
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| CN202010012029.7A Pending CN111117261A (en) | 2020-01-07 | 2020-01-07 | High-temperature-resistant fluorine silicon rubber material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114085542A (en) * | 2021-11-30 | 2022-02-25 | 常州玖翔电子有限公司 | High-temperature-resistant material and high-temperature-resistant loudspeaker |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6417263B1 (en) * | 1998-04-13 | 2002-07-09 | Dow Corning Corporation | Heat curable silicone rubber composition with improved resistance to engine oils and coolants |
| CN106280495A (en) * | 2016-08-26 | 2017-01-04 | 山东华夏神舟新材料有限公司 | A kind of high strength and high hardness Fluorosilicone rubber composition and preparation method thereof |
| CN108410181A (en) * | 2018-03-26 | 2018-08-17 | 山东冬瑞高新技术开发有限公司 | A kind of low temperature resistant fluorine silicone rubber sizing material and preparation method thereof |
| CN109762346A (en) * | 2018-12-26 | 2019-05-17 | 福建拓烯新材料科技有限公司 | A kind of Fluorosilicone rubber composition and preparation method |
-
2020
- 2020-01-07 CN CN202010012029.7A patent/CN111117261A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6417263B1 (en) * | 1998-04-13 | 2002-07-09 | Dow Corning Corporation | Heat curable silicone rubber composition with improved resistance to engine oils and coolants |
| CN106280495A (en) * | 2016-08-26 | 2017-01-04 | 山东华夏神舟新材料有限公司 | A kind of high strength and high hardness Fluorosilicone rubber composition and preparation method thereof |
| CN108410181A (en) * | 2018-03-26 | 2018-08-17 | 山东冬瑞高新技术开发有限公司 | A kind of low temperature resistant fluorine silicone rubber sizing material and preparation method thereof |
| CN109762346A (en) * | 2018-12-26 | 2019-05-17 | 福建拓烯新材料科技有限公司 | A kind of Fluorosilicone rubber composition and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 董浚修: "《润滑原理及润滑油》", 30 September 1998 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114085542A (en) * | 2021-11-30 | 2022-02-25 | 常州玖翔电子有限公司 | High-temperature-resistant material and high-temperature-resistant loudspeaker |
| CN114085542B (en) * | 2021-11-30 | 2023-02-10 | 常州玖翔电子有限公司 | High-temperature-resistant material and high-temperature-resistant loudspeaker |
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Application publication date: 20200508 |