CN114031945A - Silicone rubber material with good hydrophobicity and flame retardance and preparation method thereof - Google Patents
Silicone rubber material with good hydrophobicity and flame retardance and preparation method thereof Download PDFInfo
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- CN114031945A CN114031945A CN202111560377.9A CN202111560377A CN114031945A CN 114031945 A CN114031945 A CN 114031945A CN 202111560377 A CN202111560377 A CN 202111560377A CN 114031945 A CN114031945 A CN 114031945A
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- 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
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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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
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- 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
- C08K2003/2293—Oxides; Hydroxides of metals of nickel
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a silicone rubber composite material with good hydrophobicity and flame retardance, which is prepared from the following raw materials: methyl vinyl crude rubber, hydrophobic fumed silica, vulcanizing agent (DCP), zinc stearate, hydroxyl silicone oil, titanium dioxide or tungsten trioxide or nickel oxide, magnesium hydroxide, aluminum hydroxide and silane coupling agent (KH 550). A preparation method of a silicone rubber material with good hydrophobicity and flame retardance comprises the following steps: material modification, filler and matrix mixing, plate vulcanization and performance test. The silicone rubber prepared by the invention has good elasticity, good flame retardance and hydrophobicity, simple operation and can meet the use requirement of insulating materials.
Description
Technical Field
The invention relates to the technical field of silicone rubber materials, in particular to a silicone rubber material with good hydrophobicity and flame retardance and a preparation method thereof.
Background
In the electric power system of China, the composite insulating material is widely applied, insulators play the roles of fixing, supporting and insulating in high-voltage transmission and distribution, the application rate of the composite insulators is increased year by year, and the new online insulators are basically the composite insulators in nearly fifteen years. The composite insulator has the advantages of light weight, good antifouling performance, strong artificial damage prevention performance and the like. Under the action of the external environment, the electric field and the magnetic field, the aging of the composite insulator is promoted, so that the stability of electric power transportation is influenced, and potential safety hazards exist. Particularly in high-altitude, cold and humid areas, the hydrophobic and antifouling capabilities of the composite insulator are particularly important.
The silicon rubber is a high molecular polymer, the silicon-oxygen bond is taken as a main chain, and hydrophobic methyl or vinyl is taken as a branched chain. The bond energy of the silicon-oxygen bond is large, so that the silicon rubber has good stress resistance, stability and insulation. The present scholars develop the special performance of the silicon rubber composite system by using silicon rubber as a substrate and adding nano-filler, and the main characteristics are breakdown field strength, flame retardance, hydrophobicity, aging resistance, corona prevention and the like. In a humid environment, the surface of the silicon rubber with hydrophobicity only forms isolated water drops and does not form a continuous water film, and meanwhile, the hydrophobic surface also has good antifouling capacity, so that the insulator flashover accident along the surface can be effectively prevented. The service temperature range of the common silicon rubber is-50-180 ℃. With the continuous development of science and technology, the application field of the silicon rubber is wider and wider, and the silicon rubber is popular in the fields of electronic appliances, aerospace, mechanical manufacturing and the like, so that higher requirements on hydrophobicity and flame retardance of the silicon rubber are provided. On the whole, the traditional silicon rubber has low structural strength, unsatisfactory hydrophobic effect and insufficient flame retardance, can not meet the use requirement and has certain limitation. Therefore, the silicone rubber material with good hydrophobicity and flame retardance and the preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide a silicone rubber material with good hydrophobicity and flame retardance and a preparation method thereof, and provides a solution for the problems.
In order to achieve the purpose, the invention provides the following technical scheme: a silicone rubber material with good hydrophobicity and flame retardance comprises the following raw materials: methyl vinyl crude rubber, hydrophobic fumed silica, vulcanizing agent (DCP), zinc stearate, hydroxyl silicone oil, titanium dioxide or tungsten trioxide or nickel oxide, magnesium hydroxide, aluminum hydroxide and silane coupling agent (KH 550).
The method comprises the following steps: modifying the filler: absolute ethyl alcohol, deionized water and a silane coupling agent are mixed according to a certain proportion to prepare a modified mixed solution. Taking absolute ethyl alcohol as a dispersing agent, respectively taking a proper amount of magnesium hydroxide powder, aluminum hydroxide powder, titanium dioxide or tungsten trioxide or nickel oxide powder, respectively dissolving the magnesium hydroxide powder, the aluminum hydroxide powder, the titanium dioxide or the tungsten trioxide or the nickel oxide powder in a proper amount of absolute ethyl alcohol, and preparing a suspension by ultrasonic oscillation. And placing the suspension in a condensing reflux device, slowly adding the modified mixed solution, and reacting for 7 hours at the constant temperature of 70 ℃ under magnetic stirring to prepare the suspension of modified particles. Washing the modified particle suspension with absolute ethyl alcohol for many times, filtering, and drying in an oven for later use;
step two: mixing filler, auxiliary materials and raw rubber: setting the temperature of a double roller of a double-roller mixing mill to be 80-100 ℃, taking a proper amount of methyl vinyl raw rubber, placing the methyl vinyl raw rubber into the double-roller mixing mill, wrapping the raw rubber with a roller, adding hydrophobic fumed silica, zinc stearate, hydroxyl silicone oil, magnesium hydroxide, aluminum hydroxide, titanium dioxide or tungsten trioxide or nickel oxide and a crosslinking agent (DCP) one by one according to a certain proportion, and preparing a mixed silicon rubber material through repeated remixing;
step three: vulcanizing and forming a flat plate: placing the mixed silicon rubber material prepared in the step two into a corresponding flat vulcanizing machine for a mold to be vulcanized at high temperature and high pressure;
step four: and (3) performance testing: including hydrophobicity testing, flame retardancy testing, and breakdown field strength testing.
Preferably, according to the parts by weight, 90-110 parts of methyl vinyl raw rubber, 20-35 parts of aluminum hydroxide, 7-15 parts of magnesium hydroxide, 1-3 parts of titanium dioxide, 45-60 parts of hydrophobic fumed silica, 0.4-0.6 part of hydroxyl silicone oil, 1-2 parts of vulcanizing agent and 0.3-1 part of zinc stearate.
Preferably, 90-110 parts of methyl vinyl raw rubber, 18-32 parts of aluminum hydroxide, 7-10 parts of magnesium hydroxide, 2-5 parts of tungsten trioxide, 45-60 parts of hydrophobic fumed silica, 0.3-0.5 part of hydroxyl silicone oil, 1-2 parts of vulcanizing agent and 0.3-1 part of zinc stearate by weight.
Preferably, 90-110 parts of methyl vinyl raw rubber, 15-28 parts of aluminum hydroxide, 8-12 parts of magnesium hydroxide, 2-6 parts of nickel oxide, 45-60 parts of hydrophobic fumed silica, 0.3-0.5 part of hydroxyl silicone oil, 1-2 parts of vulcanizing agent and 0.3-1 part of zinc stearate by weight.
Preferably, the ratio of the silane coupling agent KH550 to the modified powder in the first step is 3: 1 and 4: 1.
Preferably, in the process of filling one by one in the step two, the filler is added again after each step of mixing uniformly (5-10 minutes).
Preferably, the vulcanization temperature in the fourth step is 180-220 ℃, the pressure is 10-20MPa, and the time is 50-70 minutes.
Compared with the prior art, the invention has the beneficial effects that: according to the silicone rubber material with good hydrophobicity and flame retardance and the preparation method thereof, the silicone rubber is prepared by selecting methyl vinyl raw rubber, hydrophobic fumed silica, a vulcanizing agent (DCP), zinc stearate, hydroxyl silicone oil, titanium dioxide or tungsten trioxide or nickel oxide, magnesium hydroxide, aluminum hydroxide and a silane coupling agent (KH550), and the formed silicone rubber has good elasticity, hydrophobicity and flame retardance, is stable in structure and excellent in performance, and can meet the use requirements in various environments.
Drawings
FIG. 1 is a schematic view of the structure of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
taking methyl vinyl crude rubber, hydrophobic fumed silica, magnesium hydroxide, aluminum hydroxide and titanium dioxide as main raw materials, taking zinc stearate, hydroxyl silicone oil and a vulcanizing agent as auxiliary materials, taking a silane coupling agent KH550 as an interface modifier, respectively modifying the aluminum hydroxide, the magnesium hydroxide and the titanium dioxide by using the silane coupling agent KH550 in the step one, taking 90-110 parts of the methyl vinyl crude rubber, 45-60 parts of the hydrophobic fumed silica, 0.3-1 part of zinc stearate and 0.4-0.6 part of hydroxyl silicone oil, mixing uniformly on a double-roll mixing mill, sequentially adding 20-35 parts of modified aluminum hydroxide, 7-15 parts of magnesium hydroxide and 1-3 parts of titanium dioxide, mixing uniformly, then adding 1-2 parts of the vulcanizing agent, and continuously mixing to prepare the uniformly mixed composite silicone rubber. Putting the mixture into a mould and vulcanizing the mixture by a flat vulcanizing machine, and operating according to the conditions in the step three. And carrying out hydrophobicity test, flame retardance test, volume resistivity test and breakdown field strength test on the vulcanized composite silicone rubber.
Example two:
taking methyl vinyl raw rubber, hydrophobic fumed silica, magnesium hydroxide, aluminum hydroxide and titanium dioxide as main raw materials, taking zinc stearate, hydroxyl silicone oil and a vulcanizing agent as auxiliary materials, taking a silane coupling agent KH550 as an interface modifier, respectively modifying the aluminum hydroxide, the magnesium hydroxide and the tungsten trioxide by using the silane coupling agent KH550 in the step one, taking 90-110 parts of the methyl vinyl raw rubber, 45-60 parts of the hydrophobic fumed silica, 0.3-1 part of the zinc stearate and 0.3-0.5 part of the hydroxyl silicone oil, mixing uniformly on a double-roll mixing mill, sequentially adding 18-32 parts of the modified aluminum hydroxide, 7-10 parts of the magnesium hydroxide and 2-5 parts of the tungsten trioxide, mixing uniformly, then adding 1-2 parts of the vulcanizing agent, and continuously mixing to prepare the uniformly mixed composite silicone rubber. Putting the mixture into a mould and vulcanizing the mixture by a flat vulcanizing machine, and operating according to the conditions in the step three. And carrying out hydrophobicity test, flame retardance test, volume resistivity test and breakdown field strength test on the vulcanized composite silicone rubber.
Example two:
taking methyl vinyl raw rubber, hydrophobic fumed silica, magnesium hydroxide, aluminum hydroxide and titanium dioxide as main raw materials, taking zinc stearate, hydroxyl silicone oil and a vulcanizing agent as auxiliary materials, taking a silane coupling agent KH550 as an interface modifier, respectively modifying the aluminum hydroxide, the magnesium hydroxide and the nickel oxide by using the silane coupling agent KH550 in the step one, taking 90-110 parts of the methyl vinyl raw rubber, 45-60 parts of the hydrophobic fumed silica, 0.3-1 part of the zinc stearate and 0.3-0.5 part of the hydroxyl silicone oil, mixing uniformly on a double-roll mixing mill, sequentially adding 15-28 parts of modified aluminum hydroxide, 8-12 parts of magnesium hydroxide and 2-6 parts of nickel oxide, mixing uniformly, then adding 1-2 parts of the vulcanizing agent, and continuously mixing to prepare the uniformly mixed composite silicone rubber. Putting the mixture into a mould and vulcanizing the mixture by a flat vulcanizing machine, and operating according to the conditions in the step three. And carrying out hydrophobicity test, flame retardance test, volume resistivity test and breakdown field strength test on the vulcanized composite silicone rubber.
The results of the tests of the above examples are shown in Table 1.
Table 1 results of performance testing of examples
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A silicone rubber material with good hydrophobicity and flame retardance comprises the following raw materials: methyl vinyl crude rubber, hydrophobic fumed silica, vulcanizing agent (DCP), zinc stearate, hydroxyl silicone oil, titanium dioxide or tungsten trioxide or nickel oxide, magnesium hydroxide, aluminum hydroxide and silane coupling agent (KH 550).
2. A preparation method of a silicone rubber material with good hydrophobicity and flame retardance is characterized in that: comprises the following steps;
the method comprises the following steps: modifying the filler: mixing absolute ethyl alcohol, deionized water and a silane coupling agent according to a certain proportion to prepare a modified mixed solution; taking absolute ethyl alcohol as a dispersing agent, respectively taking a proper amount of magnesium hydroxide powder, aluminum hydroxide powder, titanium dioxide or tungsten trioxide or nickel oxide powder, respectively dissolving the magnesium hydroxide powder, the aluminum hydroxide powder, the titanium dioxide or the tungsten trioxide or the nickel oxide powder in a proper amount of absolute ethyl alcohol, and preparing a suspension by ultrasonic oscillation. And placing the suspension in a condensing reflux device, slowly adding the modified mixed solution, and reacting for 7 hours at the constant temperature of 70 ℃ under magnetic stirring to obtain the suspension of modified particles. Washing the modified particle suspension with absolute ethyl alcohol for many times, filtering, and drying in an oven for later use;
step two: mixing filler, auxiliary materials and raw rubber: setting the temperature of a double roller of a double-roller mixing mill to be 80-100 ℃, taking a proper amount of methyl vinyl raw rubber, placing the methyl vinyl raw rubber into the double-roller mixing mill, wrapping the raw rubber with a roller, adding hydrophobic fumed silica, zinc stearate, hydroxyl silicone oil, magnesium hydroxide, aluminum hydroxide, titanium dioxide or tungsten trioxide or nickel oxide and a crosslinking agent (DCP) one by one according to a certain proportion, and preparing a mixed silicon rubber material through repeated remixing;
step three: vulcanizing and forming a flat plate: placing the mixed silicon rubber material prepared in the step two into a corresponding flat vulcanizing machine for a mold to be vulcanized at high temperature and high pressure;
step four: and (3) performance testing: the method comprises a hydrophobicity test, a flame retardance test, a volume resistivity test and a breakdown field strength test.
3. The raw material of silicone rubber material with good hydrophobicity and flame retardancy as claimed in claim 1, wherein: 90-110 parts of methyl vinyl raw rubber, 20-35 parts of aluminum hydroxide, 7-15 parts of magnesium hydroxide, 1-3 parts of titanium dioxide, 45-60 parts of hydrophobic fumed silica, 0.4-0.6 part of hydroxyl silicone oil, 1-2 parts of vulcanizing agent and 0.3-1 part of zinc stearate.
4. The method for preparing a silicone rubber material with good hydrophobicity and flame retardancy as claimed in claim 1, wherein: 90-110 parts of methyl vinyl raw rubber, 18-32 parts of aluminum hydroxide, 7-10 parts of magnesium hydroxide, 2-5 parts of tungsten trioxide, 45-60 parts of hydrophobic fumed silica, 0.3-0.5 part of hydroxyl silicone oil, 1-2 parts of vulcanizing agent and 0.3-1 part of zinc stearate.
5. The method for preparing a silicone rubber material with good hydrophobicity and flame retardancy as claimed in claim 1, wherein: 90-110 parts of methyl vinyl raw rubber, 15-28 parts of aluminum hydroxide, 8-12 parts of magnesium hydroxide, 2-6 parts of nickel oxide, 45-60 parts of hydrophobic fumed silica, 0.3-0.5 part of hydroxyl silicone oil, 1-2 parts of vulcanizing agent and 0.3-1 part of zinc stearate.
6. The method for preparing a silicone rubber material with good hydrophobicity and flame retardancy as claimed in claim 2, wherein: in the first step, the ratio of the silane coupling agent KH550 to the modified powder is 3: 1 and 4: 1.
7. The method for preparing a silicone rubber material with good hydrophobicity and flame retardancy as claimed in claim 2, wherein: in the process of filling one by one in the step two, the addition is continued after the uniform mixing (7-10 minutes) of each step is ensured.
8. The method for preparing a silicone rubber material with good hydrophobicity and flame retardancy as claimed in claim 2, wherein: the vulcanization temperature in the third step is 180-220 ℃, the pressure is 10-20MPa, and the time is 50-70 minutes.
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Cited By (2)
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| CN114806183A (en) * | 2022-03-17 | 2022-07-29 | 哈尔滨理工大学 | Silicon rubber material with electrochromic property and preparation method thereof |
| CN116041962A (en) * | 2023-01-31 | 2023-05-02 | 安徽迈腾新材料有限公司 | Low-compressibility flame-retardant silicone rubber material |
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Application publication date: 20220211 |