CN111040454A - Novel high-temperature-resistant silicon rubber and preparation method thereof - Google Patents
Novel high-temperature-resistant silicon rubber and preparation method thereof Download PDFInfo
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- 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
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- 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
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- 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
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Abstract
The invention belongs to the technical field of silicone rubber materials, and relates to novel high-temperature-resistant silicone rubber and a preparation method thereof. The novel high-temperature-resistant silicon rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 2-10 parts of hydroxyl silicone oil, 2-10 parts of heat stabilizer, 10-40 parts of white carbon black, 1-2 parts of vulcanizing agent, 10-50 parts of melamine phosphate flame retardant, 1-2 parts of flame retardant synergist, 2-5 parts of silane coupling agent and 0.1-0.5 part of mold release agent. The novel high-temperature-resistant silicon rubber has the advantages of high temperature resistance, high strength, good elasticity, low density, good aging resistance, good flame retardant property and the like.
Description
Technical Field
The invention belongs to the technical field of silicone rubber materials, and relates to novel high-temperature-resistant silicone rubber and a preparation method thereof.
Background
The silicon rubber material has the characteristics of excellent high and low temperature resistance, weather resistance, electric insulation and the like, and is widely applied to the industrial field. The service temperature of the silicon rubber is generally below 200 ℃, and higher requirements are put forward on the high temperature resistance of the silicon rubber in the fields of high-power electronic devices, aerospace, national defense industry, special industrial equipment and the like.
The high-temperature resistant silicon rubber used at present can only be used for a short time at the temperature of more than 300 ℃. Therefore, the development and technical development of high temperature resistant rubber is urgent and necessary.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a novel high-temperature-resistant silicon rubber and a preparation method thereof. The novel high-temperature-resistant silicon rubber has the advantages of high temperature resistance, high strength, good elasticity, low density, good aging resistance, good flame retardant property and the like; the preparation method is simple to operate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the high-temperature-resistant silicon rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 2-10 parts of hydroxyl silicone oil, 2-10 parts of heat stabilizer, 10-40 parts of white carbon black, 1-2 parts of vulcanizing agent, 10-50 parts of melamine phosphate flame retardant, 1-2 parts of flame retardant synergist, 2-5 parts of silane coupling agent and 0.1-0.5 part of mold release agent.
The molecular weight of the methyl vinyl silicone rubber is between 600000 and 700000.
The vinyl content of the methyl vinyl silicone rubber is 0.1-0.2 mol%.
The white carbon black is treated by silazane, and the particle size is 10-50 nm.
The flame retardant is melamine phosphate.
The flame-retardant synergist is lanthanum oxide.
The heat stabilizer is cerium oxide or ferric oxide.
The vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide.
The preparation method specifically comprises the following steps:
1) adding the methyl vinyl silicone rubber, the white carbon black, the hydroxyl silicone oil, the heat stabilizer and the release agent into a kneading machine, and stirring without heating to obtain a molding material;
2) heating and stirring the molding material to 160 ℃ at 140 ℃, and keeping the temperature and stirring for 0.5-1 hour.
3) And (3) preserving the heat of the materials, vacuumizing and stirring for 0.5-1 hour.
4) Adding a flame retardant, a flame-retardant synergist and a silane coupling agent into the materials, and stirring for 0.5-1 hour under heat preservation to obtain a silicone rubber material;
5) adding the silicon rubber material and 2, 5-dimethyl-2, 5-di-tert-butyl alkyl peroxide into an open rubber mixing mill, mixing uniformly, and placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the high temperature resistant silicon rubber.
The invention has the beneficial effects that: the high-temperature resistant silicon rubber inhibits thermal cracking and thermal oxidation reaction, and improves the high-temperature resistance of the silicon rubber; tensile strength of the novel high-temperature silicone rubber>6.0MPa, elongation at break>500% hardness (Shore A)>45, density<1.25g/cm3The invention has good elasticity and low density; the vertical burning grade of the invention reaches UL94-V0, and the oxygen index>28, the flame retardant property of the invention is good.
Detailed Description
For a further understanding of the invention, reference will now be made to the following description of embodiments, but it will be understood that the description is intended to illustrate further features and advantages of the invention, and not to limit the scope of the claims.
< example 1>
The high-temperature-resistant silicon rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 2 parts of hydroxyl silicone oil, 4 parts of cerium oxide serving as a heat stabilizer, 30 parts of white carbon black, 1 part of a vulcanizing agent, 40 parts of a melamine phosphate flame retardant, 1 part of lanthanum oxide serving as a flame retardant synergist, 2 parts of a silane coupling agent and 0.2 part of a mold release agent.
The preparation method comprises the following steps:
1) adding methyl vinyl silicone rubber, white carbon black, hydroxyl silicone oil, cerium oxide and a release agent into a kneading machine, and stirring for 20 minutes without heating to obtain a molding material;
2) heating and stirring the formed material to 140 ℃, and keeping the temperature and stirring for 1 hour.
3) The materials are stirred for 0.5 hour after heat preservation and vacuum pumping.
4) Adding melamine phosphate, lanthanum oxide and a silane coupling agent into the materials, and stirring for 0.5 hour under heat preservation to obtain a silicone rubber material;
5) adding the silicon rubber material and 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide into an open rubber mixing mill, mixing uniformly, and placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the high temperature resistant silicon rubber.
< example 2>
The high-temperature-resistant silicon rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 3 parts of hydroxyl silicone oil, 8 parts of ferric oxide serving as a heat stabilizer, 35 parts of white carbon black, 1 part of a vulcanizing agent, 45 parts of a melamine phosphate flame retardant, 1.5 parts of lanthanum oxide serving as a flame retardant synergist, 2 parts of a silane coupling agent and 0.2 part of a mold release agent.
The preparation method comprises the following steps:
1) adding methyl vinyl silicone rubber, white carbon black, hydroxyl silicone oil, cerium oxide and a release agent into a kneading machine, and stirring for 20 minutes without heating to obtain a molding material;
2) heating and stirring the formed material to 150 ℃, and keeping the temperature and stirring for 1 hour.
3) The materials are stirred for 0.5 hour after heat preservation and vacuum pumping.
4) Adding melamine phosphate, lanthanum oxide and a silane coupling agent into the materials, and stirring for 1 hour under heat preservation to obtain a silicone rubber material;
5) adding the silicon rubber material and 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide into an open rubber mixing mill, mixing uniformly, and placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the high temperature resistant silicon rubber.
< example 3>
The high-temperature-resistant silicon rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 10 parts of hydroxyl silicone oil, 5 parts of cerium oxide serving as a heat stabilizer, 40 parts of white carbon black, 1 part of a vulcanizing agent, 50 parts of a melamine phosphate flame retardant, 1 part of lanthanum oxide serving as a flame retardant synergist, 2 parts of a silane coupling agent and 0.2 part of a mold release agent.
The preparation method comprises the following steps:
1) adding methyl vinyl silicone rubber, white carbon black, hydroxyl silicone oil, cerium oxide and a release agent into a kneading machine, and stirring for 20 minutes without heating to obtain a molding material;
2) heating and stirring the molding material to 160 ℃, and keeping the temperature and stirring for 0.5 hour.
3) The materials are stirred for 0.5 hour after heat preservation and vacuum pumping.
4) Adding melamine phosphate, lanthanum oxide and a silane coupling agent into the materials, and stirring for 0.5 hour under heat preservation to obtain a silicone rubber material;
5) adding the silicon rubber material and 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide into an open rubber mixing mill, mixing uniformly, and placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the high temperature resistant silicon rubber.
< modification example >
The high-temperature-resistant silicon rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 10 parts of hydroxyl silicone oil, 5 parts of cerium oxide serving as a heat stabilizer, 40 parts of white carbon black, 1 part of a vulcanizing agent, 50 parts of a melamine phosphate flame retardant, 1 part of basic nickel carbonate serving as a flame retardant synergist, 2 parts of a silane coupling agent and 0.2 part of a mold release agent.
The preparation method comprises the following steps:
1) adding methyl vinyl silicone rubber, white carbon black, hydroxyl silicone oil, cerium oxide and a release agent into a kneading machine, and stirring for 20 minutes without heating to obtain a molding material;
2) heating and stirring the molding material to 160 ℃, and keeping the temperature and stirring for 0.5 hour.
3) The materials are stirred for 0.5 hour after heat preservation and vacuum pumping.
4) Adding melamine phosphate, lanthanum oxide and a silane coupling agent into the materials, and stirring for 0.5 hour under heat preservation to obtain a silicone rubber material;
5) adding the silicon rubber material and 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide into an open rubber mixing mill, mixing uniformly, and placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the high temperature resistant silicon rubber.
Performance detection
The hardness (Shore A) is tested according to the GB/T531-1999 standard; tensile strength and elongation at break were tested according to GB/T528-1998 standard; the heat-resistant air aging performance is tested according to the GB/T3512-2001 standard, and the aging condition is multiplied by 24 hours at 300 ℃; the oxygen index was tested according to GB/T2406 + 1993 standard; the vertical combustion performance is tested according to the GB/T2408 + 2008 standard, and the thickness of the test sample is 2 mm; the density was tested according to GB/T533-2008 standard.
The high temperature resistant silicone rubbers prepared in examples 1-3 were tested for properties and compared to foreign standards and other products, and the results are shown in Table 1.
Table 1 comparison of the performance index of the high temperature resistant silicone rubber prepared in examples 1-3 with foreign standards and other products.
As can be seen from Table 1, the tensile strength of the novel high-temperature silicone rubber is more than 6MPa, is close to that of the Jihua institute, and is more than the foreign standard; the elongation at break of the invention is more than 500 percent, which is more than 336 percent of the products of Jihua institute and the foreign standards. The Shore hardness is lower than the standard of Jihua institute and foreign countries, which shows that the invention has good softness and elasticity. The change of elongation at break/% (300 ℃ multiplied by 24h) is between-25% and-30%, which accords with the foreign standard and shows that the invention has strong aging resistance. The vertical burning grade of the invention reaches UL-94VO grade, and the oxygen index exceeds 28, which shows that the invention has good flame retardant property. The density of the invention is lower than 1.25g/cm3And the cost can be effectively reduced.
It should be understood that the detailed description of the present invention is only for illustrating the present invention and is not limited by the technical solutions described in the embodiments of the present invention, and those skilled in the art should understand that the present invention can be modified or substituted equally to achieve the same technical effects; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (9)
1. The high-temperature-resistant silicon rubber is characterized by being prepared from the following raw materials in parts by weight:
2. the high temperature resistant silicone rubber of claim 1, wherein: the molecular weight of the methyl vinyl silicone rubber is between 600000 and 700000.
3. The high temperature resistant silicone rubber of claim 1, wherein: the vinyl content of the methyl vinyl silicone rubber is 0.1-0.2 mol%.
4. The high temperature resistant silicone rubber of claim 1, wherein: the white carbon black is treated by silazane, and the particle size is 10-50 nm.
5. The high temperature resistant silicone rubber of claim 1, wherein: the flame retardant is melamine phosphate.
6. The high temperature resistant silicone rubber of claim 1, wherein: the flame-retardant synergist is lanthanum oxide.
7. The high temperature resistant silicone rubber of claim 1, wherein: the heat stabilizer is cerium oxide or ferric oxide.
8. The high temperature resistant silicone rubber of claim 1, wherein: the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide.
9. The high temperature resistant silicone rubber according to claim 1, wherein the preparation method specifically comprises:
1) adding the methyl vinyl silicone rubber, the white carbon black, the hydroxyl silicone oil, the heat stabilizer and the release agent into a kneading machine, and stirring without heating to obtain a molding material;
2) heating and stirring the molding material to 160 ℃ at 140 ℃, and keeping the temperature and stirring for 0.5-1 hour.
3) And (3) preserving the heat of the materials, vacuumizing and stirring for 0.5-1 hour.
4) Adding a flame retardant, a flame-retardant synergist and a silane coupling agent into the materials, and stirring for 0.5-1 hour under heat preservation to obtain a silicone rubber material;
5) adding the silicon rubber material and 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide into an open rubber mixing mill, mixing uniformly, and placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the high-temperature-resistant silicon rubber.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995870A (en) * | 2020-09-09 | 2020-11-27 | 溧阳市宏大电子电器绝缘材料有限公司 | Silicone rubber composition with good aging resistance and processing technology thereof |
| CN115074026A (en) * | 2022-06-30 | 2022-09-20 | 马鞍山欧凯新材料科技有限公司 | Carbon fiber corona roller for lithium battery aluminum foil |
| CN117567867A (en) * | 2024-01-16 | 2024-02-20 | 江苏中煜橡塑科技有限公司 | Flame-retardant silica gel material and preparation method and application thereof |
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| CN105400208A (en) * | 2015-11-24 | 2016-03-16 | 安徽都邦电器有限公司 | High-temperature-resistant high-fire-retardant silicone tube |
| CN107513273A (en) * | 2017-09-11 | 2017-12-26 | 江苏天辰新材料股份有限公司 | A kind of flame-proof heat-resistant silicon rubber and preparation method thereof |
| CN107778870A (en) * | 2016-08-30 | 2018-03-09 | 沈阳顺风新材料有限公司 | A kind of novel fire resistant silicon rubber and preparation method thereof |
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2019
- 2019-12-30 CN CN201911396788.1A patent/CN111040454A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004092278A1 (en) * | 2003-04-15 | 2004-10-28 | Dow Corning Toray Co. Ltd. | Thermoconductive addition-curable liquid silicone rubber composition and coated fixing roll |
| CN105400208A (en) * | 2015-11-24 | 2016-03-16 | 安徽都邦电器有限公司 | High-temperature-resistant high-fire-retardant silicone tube |
| CN107778870A (en) * | 2016-08-30 | 2018-03-09 | 沈阳顺风新材料有限公司 | A kind of novel fire resistant silicon rubber and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995870A (en) * | 2020-09-09 | 2020-11-27 | 溧阳市宏大电子电器绝缘材料有限公司 | Silicone rubber composition with good aging resistance and processing technology thereof |
| CN115074026A (en) * | 2022-06-30 | 2022-09-20 | 马鞍山欧凯新材料科技有限公司 | Carbon fiber corona roller for lithium battery aluminum foil |
| CN117567867A (en) * | 2024-01-16 | 2024-02-20 | 江苏中煜橡塑科技有限公司 | Flame-retardant silica gel material and preparation method and application thereof |
| CN117567867B (en) * | 2024-01-16 | 2024-04-05 | 江苏中煜橡塑科技有限公司 | Flame-retardant silica gel material and preparation method and application thereof |
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