CN111363365B - Ultra-high pressure and high temperature resistant mixed silicone rubber and preparation method thereof - Google Patents
Ultra-high pressure and high temperature resistant mixed silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of silicone rubber, and particularly relates to ultra-high pressure and high temperature resistant mixed silicone rubber and a preparation method thereof. The invention provides an ultra-high pressure and high temperature resistant mixing silicone rubber which comprises the following components in parts by weight: 70-120 parts of methyl vinyl silicone rubber crude rubber, 20-30 parts of fumed silica, 3-6 parts of hexamethyldisilazane, 1-3 parts of dimethyl diethoxysilane, 0.1-1 part of zinc stearate, 5-30 parts of silica micropowder, 5-20 parts of nitrogen compound, 5-20 parts of ferric oxide, 1-5 parts of titanium dioxide, 0.1-1 part of vinyl triethoxysilane, 0.5-3 parts of distilled water, 1-5 parts of cerium oxide and 1-3 parts of flame retardant. The ultra-high pressure and high temperature resistant mixed silicon rubber provided by the invention obviously improves the flame retardance, the stability of the electrical property and the breakdown voltage of the silicon rubber material. The electric power product produced by using the silicon rubber has higher safety and more stable quality.
Description
Technical Field
The invention belongs to the technical field of silicone rubber, and particularly relates to ultra-high pressure and high temperature resistant mixed silicone rubber and a preparation method thereof.
Background
The silicon rubber forms a commodity group with various performances, purposes and product forms due to the difference of the structure and polymerization degree of the used basic polymers and the diversity of the rubber material and the formula composition and the forming and vulcanizing methods. According to the vulcanization temperature, silicone rubber can be classified into high-temperature vulcanized silicone rubber and room-temperature vulcanized silicone rubber. The high temperature silicone rubber HVR (Heat curing rubber) discussed in this patent is a rubber compound compounded by linear polyorganosiloxane (crude rubber) with high polymerization degree (5000-. When in use, a vulcanizing agent is added, and the vulcanizing agent is heated to form the elastomer. The process of processing the product is the same as that of common organic rubber, and the product is molded and vulcanized after being mixed on a rubber mixing mill, so the product is also called high-temperature mixed silicone rubber.
The silicon rubber has excellent heat resistance, cold resistance, dielectric property, ozone resistance, atmospheric aging resistance and other properties. The heat-vulcanized silicone rubber has ozone resistance and weather resistance superior to other organic rubbers, and the volume fraction of ozone is 2.0 multiplied by 10-8When the environment of the rubber is subjected to an accelerated aging test, the inner surface of the rubber is cracked within seconds to hours, and the mechanical strength of the silicone rubber is slightly reduced after 28 days, so that the surface of the silicone rubber is not cracked or sticky. Meanwhile, the heat vulcanized silicone rubber has excellent electrical property, the 1mm breakdown voltage strength of the conventional heat vulcanized silicone rubber is 18-24KV, and the volume resistivity is 1013-1015Omega/cm. The silicon rubber is not easy to burn, but can continue burning after being ignited. With the improvement of the performance and safety of electric products, the electrical property and flame retardant property of the silicon rubber are necessary to be further improved.
Chinese patent CN102850806B discloses a heat-vulcanized flame-retardant silicone rubber composite material and a preparation method thereof, wherein the composite material is prepared by mixing and vulcanizing hydrotalcite-like compound containing zinc, boron and iron and heat-vulcanized silicone rubber raw rubber. The material is prepared by mixing hot vulcanization type silicon rubber crude rubber and hydrotalcite-like compound containing zinc, boron and iron uniformly; then adding a vulcanizing agent, uniformly mixing and then discharging the mixture; and finally, vulcanizing. The heat-vulcanized flame-retardant silicone rubber composite material provided by the invention has remarkable flame-retardant and smoke-suppressing performances and excellent physical and mechanical properties. Although the flame retardant property of the silicone rubber is improved, the electrical properties such as breakdown voltage strength, volume resistivity and the like of the silicone rubber are not improved, and the silicone rubber cannot be used in a high-voltage environment. With the development of science and technology and the improvement of safety consciousness, higher requirements are put forward on the flame retardance of the silicone rubber. In addition, in the case of improving flame retardancy, other properties such as stability of electrical properties and breakdown voltage of silicone rubber are required to be further improved. Therefore, it is necessary to further improve the flame retardant property and the stability of the electrical property of the silicone rubber, and to ensure that the silicone rubber can be used at high temperature and high pressure for a long time without changing the quality of the silicone rubber, so as to enrich the application of the silicone rubber in the fields of life and scientific and technological research.
Disclosure of Invention
The invention aims to provide the ultra-high pressure and high temperature resistant mixed silicone rubber and the preparation method thereof, and the ultra-high pressure and high temperature resistant mixed silicone rubber provided by the invention obviously improves the flame retardance, the stability of the electrical property and the breakdown voltage of the silicone rubber material, and can ensure that the silicone rubber can be used for a long time under high temperature and high pressure without changing the quality, and the obtained silicone rubber material has more excellent insulating property.
The technical scheme of the invention is as follows:
the ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight:
70-120 parts of methyl vinyl silicone rubber crude rubber, 20-30 parts of fumed silica, 3-6 parts of hexamethyldisilazane, 1-3 parts of dimethyl diethoxysilane, 0.1-1 part of zinc stearate, 5-30 parts of silica micropowder, 5-20 parts of nitrogen compound, 5-20 parts of ferric oxide, 1-5 parts of titanium dioxide, 0.1-1 part of vinyl triethoxysilane, 0.5-3 parts of distilled water, 1-5 parts of cerium oxide and 1-3 parts of flame retardant.
Further, the ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 25 parts of fumed silica, 5 parts of hexamethyldisilazane, 2 parts of dimethyl diethoxy silane, 0.6 part of zinc stearate, 18 parts of silica powder, 12 parts of nitrogen compound, 13 parts of ferric oxide, 3 parts of titanium dioxide, 0.8 part of vinyl triethoxysilane, 2 parts of distilled water, 2 parts of cerium oxide and 2 parts of flame retardant.
Further, the raw methyl vinyl silicone rubber is prepared from raw methyl vinyl silicone rubber with a vinyl-terminated vinyl molar content of 0.03-0.09% and raw methyl vinyl silicone rubber with a vinyl-terminated vinyl molar content of 0.05-0.30% in a weight ratio of 5-8: 2-4.
Further, the raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with 0.06% of vinyl-terminated vinyl molar content and raw methyl vinyl silicone rubber with 0.24% of vinyl-terminated vinyl molar content according to the weight ratio of 7: 3, and (3).
Further, the nitrogen compound is one or more of aluminum nitride, silicon nitride, 5-amino tetrazole, 2-phenyl-5-amino tetrazole and triazole.
Further, the specific surface area of the fumed silica is 150-250 m2/g。
Further, the flame retardant comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
The invention also provides a preparation method of the ultra-high pressure and high temperature resistant mixed silicone rubber, which comprises the following steps:
s1, putting methyl vinyl raw rubber, fumed silica, dimethyl diethoxysilane, hexamethyldisilazane and distilled water with different vinyl contents into an internal mixer, uniformly mixing at a low temperature, stirring for 60min, standing for 3-5 hours, vacuumizing, heating to 170 ℃, treating for 3 hours, cooling to obtain a base primer;
s2, adding zinc stearate, silicon micropowder, nitrogen compound, ferric oxide, titanium dioxide, vinyl triethoxysilane, cerium oxide and flame retardant, and cerium oxide and flame retardant into the base primer obtained in the step S1, and uniformly mixing at low temperature for 40-80min to obtain the product.
Further, in the step S1, vacuum pumping is carried out until the pressure is between-0.060 MPa and-0.080 MPa.
According to the ultra-high pressure and high temperature resistant mixing silicone rubber prepared by the invention, methyl vinyl raw rubber and fumed silica are mixed at a low temperature, hexamethyldisilazane and dimethyldiethoxysilane are added to treat fumed silica, and then a high-temperature reaction is carried out, so that the base primer with good hydrophobicity and breakdown voltage stabilized between 20 MV/m and 24MV/m is obtained. The added fumed silica can improve the strength, wear resistance, ageing resistance and other properties of the product.
Meanwhile, the added raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with the vinyl terminated vinyl molar content of 0.03-0.09% and raw methyl vinyl silicone rubber with the vinyl terminated vinyl molar content of 0.05-0.30% in a weight ratio of 5-8: 2-4. The base rubber with good mechanical property is obtained by matching and using two kinds of methyl vinyl silicone rubber crude rubber with different molar contents.
The nitrogen compound, the titanium dioxide, the iron oxide and the cerium oxide added in the ultra-high pressure and high temperature resistant mixing silicone rubber prepared by the invention are inorganic powder, and the inorganic powder and the fire retardant are added into the cooled base rubber, so that the volume resistivity, the breakdown voltage strength and the flame retardant property of the rubber material are improved. Among them, titanium dioxide has excellent anti-ultraviolet ability, can scatter ultraviolet rays in a long wave region, can absorb ultraviolet rays in a medium wave region, has characteristics of sensitivity to light, heat and magnetism and surface stability different from those of conventional particles, and thus has excellent weather resistance and aging resistance. Meanwhile, the vinyltriethoxysilane is added to treat the inorganic powder, so that the powder is uniformly dispersed in the rubber material, the stability of the electrical property of the rubber material is ensured, and the physical and mechanical properties of the silicone rubber compound are improved. Moreover, after the self-made flame retardant is added, the flame retardance of the rubber material can reach UL94V-0 level, and the application range of the ultra-high pressure and high temperature resistant mixed silicone rubber is widened.
Compared with the prior art, the ultra-high pressure and high temperature resistant mixing silicone rubber provided by the invention has the following advantages:
(1) according to the ultra-high pressure and high temperature resistant mixing silicone rubber provided by the invention, methyl vinyl silicone rubber raw rubber and hexamethyldisilazane with different molar contents are added, so that the silicone rubber has good heat resistance, long service life, good hydrophobicity and stable breakdown voltage.
(2) According to the ultra-high pressure and high temperature resistant mixing silicone rubber provided by the invention, the added nitrogen compound, titanium dioxide and iron oxide are inorganic powder, so that the breakdown voltage strength of the rubber can be effectively improved, and the flame retardant property of the rubber can be assisted to be improved.
(3) The ultra-high pressure and high temperature resistant mixing silicon rubber provided by the invention can maintain excellent mechanical properties and flame retardant properties, and simultaneously, the breakdown voltage and the volume resistivity of the silicon rubber are also obviously improved, so that the obtained silicon rubber material has better insulating property, more stable electrical property and higher safety.
Detailed Description
The present invention is further illustrated by the following description of specific embodiments, which are not intended to limit the invention, and various modifications and improvements can be made by those skilled in the art based on the basic idea of the invention, but the invention is within the protection scope of the invention.
Wherein, the reagents used in the invention are all common reagents and can be purchased from common reagent production and sale companies.
Example 1 an ultra-high pressure and high temperature resistant compounded silicone rubber
The ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight:
70 parts of methyl vinyl silicone rubber crude rubber, 20 parts of fumed silica, 3 parts of hexamethyldisilazane, 1 part of dimethyl diethoxy silane, 0.1 part of zinc stearate, 5 parts of silica micropowder, 5 parts of nitrogen compound, 5 parts of ferric oxide, 1 part of titanium dioxide, 0.1 part of vinyl triethoxysilane, 0.5 part of distilled water, 1 part of cerium oxide and 1 part of flame retardant.
The raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with 0.03 percent of vinyl molar content of vinyl end capping and raw methyl vinyl silicone rubber with 0.05 percent of vinyl molar content of vinyl end capping according to the weight ratio of 5: 4.
The nitrogen compound is aluminum nitride.
The specific surface area of the fumed silica is 150m2/g。
The flame retardant consists of the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
The preparation method of the ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following steps:
s1, putting methyl vinyl raw rubber, fumed silica, dimethyl diethoxysilane, hexamethyldisilazane and distilled water with different vinyl contents into an internal mixer, uniformly mixing at a low temperature, stirring for 60min, standing for 3 hours, vacuumizing to-0.080 MPa, heating to 170 ℃, treating for 3 hours, cooling to obtain a base rubber;
s2, adding zinc stearate, silicon micropowder, nitrogen compound, ferric oxide, titanium dioxide, vinyl triethoxysilane, cerium oxide and flame retardant into the base primer obtained in the step S1, and mixing uniformly for 40min at low temperature to obtain the coating.
Example 2 ultra-high pressure and high temperature resistant mixed silicone rubber
The ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 25 parts of fumed silica, 5 parts of hexamethyldisilazane, 2 parts of dimethyl diethoxy silane, 0.6 part of zinc stearate, 18 parts of silica powder, 12 parts of nitrogen compound, 13 parts of ferric oxide, 3 parts of titanium dioxide, 0.8 part of vinyl triethoxysilane, 2 parts of distilled water, 2 parts of cerium oxide and 2 parts of flame retardant.
The raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with 0.08 percent of vinyl molar content of vinyl end capping and raw methyl vinyl silicone rubber with 0.16 percent of vinyl molar content of vinyl end capping according to the weight ratio of 7: 3, and (3).
The nitrogen compound is silicon nitride.
The specific surface area of the fumed silica is 200m2/g。
The flame retardant consists of the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
The preparation method of the ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following steps:
s1, putting methyl vinyl raw rubber, fumed silica, dimethyl diethoxysilane, hexamethyldisilazane and distilled water with different vinyl contents into an internal mixer, uniformly mixing at a low temperature, stirring for 60min, standing for 4 hours, vacuumizing to-0.070 MPa, heating to 170 ℃, treating for 3 hours, and cooling to obtain the base rubber;
s2, adding zinc stearate, silicon micropowder, nitrogen compound, ferric oxide, titanium dioxide, vinyl triethoxysilane, cerium oxide and flame retardant into the base primer obtained in the step S1, and mixing uniformly for 60min at low temperature to obtain the coating.
Example 3 an ultra high pressure and high temperature resistant compounded silicone rubber
The ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight:
120 parts of methyl vinyl silicone rubber crude rubber, 30 parts of fumed silica, 6 parts of hexamethyldisilazane, 3 parts of dimethyl diethoxysilane, 1 part of zinc stearate, 30 parts of silica micropowder, 20 parts of nitrogen compound, 20 parts of ferric oxide, 5 parts of titanium dioxide, 1 part of vinyl triethoxysilane, 3 parts of distilled water, 5 parts of cerium oxide and 3 parts of flame retardant.
The raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with vinyl terminated vinyl molar content of 0.09 percent and raw methyl vinyl silicone rubber with vinyl terminated vinyl molar content of 0.30 percent according to the weight ratio of 8: 2.
The nitrogen compound is composed of silicon nitride and triazole according to the weight ratio of 1: 1.
The specific surface area of the fumed silica is 250m2/g。
The flame retardant consists of the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
The preparation method of the ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following steps:
s1, putting methyl vinyl crude rubber, fumed silica, dimethyl diethoxysilane, hexamethyldisilazane and distilled water with different vinyl contents into an internal mixer, uniformly mixing at a low temperature, stirring for 60min, standing for 5 hours, vacuumizing to-0.060 MPa, heating to 170 ℃, treating for 3 hours, and cooling to obtain the base rubber;
s2, adding zinc stearate, silicon micropowder, nitrogen compound, ferric oxide, titanium dioxide, vinyl triethoxysilane, cerium oxide and flame retardant into the base primer obtained in the step S1, and mixing uniformly for 80min at low temperature to obtain the coating.
Comparative example 1 ultra-high pressure and high temperature resistant mixed silicone rubber
The ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 25 parts of fumed silica, 5 parts of hexamethyldisilazane, 2 parts of dimethyl diethoxy silane, 0.6 part of zinc stearate, 18 parts of silica micropowder, 12 parts of nitrogen compound, 13 parts of ferric oxide, 3 parts of titanium dioxide, 0.8 part of vinyl triethoxysilane, 2 parts of distilled water and 2 parts of cerium oxide.
The raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with 0.06 percent of vinyl molar content of vinyl end capping and raw methyl vinyl silicone rubber with 0.24 percent of vinyl molar content of vinyl end capping according to the weight ratio of 7: 3, and (3).
The nitrogen compound is silicon nitride.
The specific surface area of the fumed silica is 200m2/g。
The preparation method of the ultra-high pressure and high temperature resistant mixed silicone rubber is similar to that of the example 2.
The difference from example 2 is that no flame retardant was added.
Comparative example 2 ultra-high pressure and high temperature resistant mixed silicone rubber
The ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 25 parts of fumed silica, 5 parts of hexamethyldisilazane, 2 parts of dimethyl diethoxy silane, 0.6 part of zinc stearate, 18 parts of silica micropowder, 12 parts of nitrogen compound, 3 parts of titanium dioxide, 0.8 part of vinyl triethoxysilane, 2 parts of distilled water, 2 parts of cerium oxide and 2 parts of flame retardant.
The raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with 0.06 percent of vinyl molar content of vinyl end capping and raw methyl vinyl silicone rubber with 0.24 percent of vinyl molar content of vinyl end capping according to the weight ratio of 7: 3, and (3).
The nitrogen compound is silicon nitride.
The specific surface area of the fumed silica is 200m2/g。
The flame retardant consists of the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
The preparation method of the ultra-high pressure and high temperature resistant mixed silicone rubber is similar to that of the example 2.
The difference from example 2 is that no iron oxide is added.
Comparative example 3 ultra-high pressure and high temperature resistant mixed silicone rubber
The ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 25 parts of fumed silica, 5 parts of hexamethyldisilazane, 2 parts of dimethyl diethoxy silane, 0.6 part of zinc stearate, 18 parts of silica micropowder, 12 parts of nitrogen compound, 13 parts of ferric oxide, 0.8 part of vinyl triethoxysilane, 2 parts of distilled water, 2 parts of cerium oxide and 2 parts of flame retardant.
The raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with 0.06 percent of vinyl molar content of vinyl end capping and raw methyl vinyl silicone rubber with 0.24 percent of vinyl molar content of vinyl end capping according to the weight ratio of 7: 3, and (3).
The nitrogen compound is silicon nitride.
The specific surface area of the fumed silica is 200m2/g。
The flame retardant consists of the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
The preparation method of the ultra-high pressure and high temperature resistant mixed silicone rubber is similar to that of the example 2.
The difference from example 2 is that no titanium dioxide is added.
Comparative example 4 an ultra-high pressure and high temperature resistant mixed silicone rubber
The ultra-high pressure and high temperature resistant mixing silicone rubber comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 25 parts of fumed silica, 5 parts of hexamethyldisilazane, 2 parts of dimethyl diethoxysilane, 0.6 part of zinc stearate, 18 parts of silicon micropowder, 13 parts of ferric oxide, 3 parts of titanium dioxide, 0.8 part of vinyl triethoxysilane, 2 parts of distilled water, 2 parts of cerium oxide and 2 parts of flame retardant.
The raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with 0.06 percent of vinyl molar content of vinyl end capping and raw methyl vinyl silicone rubber with 0.24 percent of vinyl molar content of vinyl end capping according to the weight ratio of 7: 3, and (3).
The specific surface area of the fumed silica is 200m2/g。
The flame retardant consists of the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
The preparation method of the ultra-high pressure and high temperature resistant mixed silicone rubber is similar to that of the example 2.
The difference from example 2 is that no nitrogen compound is added.
Test example I, Performance test
1. Testing materials: the ultra-high pressure and high temperature resistant compounded silicone rubbers obtained in examples 1 to 3 and comparative examples 1 to 4.
2. The test method comprises the following steps: the ultra-high pressure and high temperature resistant mixed silicone rubber prepared in the examples 1 to 3 and the comparative examples 1 to 4 is detected, and the performance indexes and the corresponding test methods are shown in the following table 1:
table 1: detected performance index and corresponding test method
| Performance index | Unit of | Test method |
| Degree of plasticity | -- | GB/T 12828-2006 |
| Density of | g/cm3 | ISO 2781:2018 |
| Hardness Shore A | -- | ISO 48-4:2018 |
| Tensile strength | MPa | JIS K6251:2017 |
| Elongation percentage | ％ | JIS K6251:2017 |
| Tear strength | N/mm | JIS K 6252-1:2015 |
| Volume resistivity | Ω.cm | GB/T 1410-2006 |
| Breakdown voltage | MV/m | GB/T 1695-2005 |
| Flame retardancy | UL94V-0 | GB/T 10707-2008 |
3. And (3) testing results: the test results are shown in table 2.
Table 2: results of performance testing
As can be seen from Table 2, the volume resistivity and breakdown voltage of the ultra-high pressure and high temperature resistant mixed silicone rubber prepared in the embodiments 2 and 3 of the invention are obviously improved compared with those of common silicone rubber, and the ultra-high pressure and high temperature resistant mixed silicone rubber has excellent physical properties and flame retardant properties; compared with comparative examples 1-4, the ultra-high pressure and high temperature resistant mixed silicone rubber prepared in example 2 of the invention has more excellent flame retardant property and electrical property on the premise of maintaining excellent physical properties, and especially the breakdown voltage and volume resistivity of the silicone rubber are remarkably improved, so that the obtained silicone rubber material has better insulating property and more stable electrical property.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. The ultra-high pressure and high temperature resistant mixing silicone rubber is characterized by comprising the following components in parts by weight: 70-120 parts of methyl vinyl silicone rubber crude rubber, 20-30 parts of fumed silica, 3-6 parts of hexamethyldisilazane, 1-3 parts of dimethyl diethoxysilane, 0.1-1 part of zinc stearate, 5-30 parts of silica micropowder, 5-20 parts of nitrogen compound, 5-20 parts of ferric oxide, 1-5 parts of titanium dioxide, 0.1-1 part of vinyl triethoxysilane, 0.5-3 parts of distilled water, 1-5 parts of cerium oxide and 1-3 parts of flame retardant;
the raw methyl vinyl silicone rubber is raw methyl vinyl silicone rubber with vinyl terminated vinyl molar content of 0.03-0.09% and raw methyl vinyl silicone rubber with vinyl terminated vinyl molar content of 0.05-0.30% according to the weight ratio of 5-8: 2-4;
the nitrogen compound is one or more of aluminum nitride, silicon nitride, 5-amino tetrazole, 2-phenyl-5-amino tetrazole and triazole.
2. The ultra-high pressure and high temperature resistant mixing silicone rubber of claim 1, which comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber, 25 parts of fumed silica, 5 parts of hexamethyldisilazane, 2 parts of dimethyl diethoxy silane, 0.6 part of zinc stearate, 18 parts of silica powder, 12 parts of nitrogen compound, 13 parts of ferric oxide, 3 parts of titanium dioxide, 0.8 part of vinyl triethoxysilane, 2 parts of distilled water, 2 parts of cerium oxide and 2 parts of flame retardant.
3. The ultra-high pressure and high temperature resistant compounded silicone rubber according to claim 1, wherein the raw methyl vinyl silicone rubber is a raw methyl vinyl silicone rubber with a vinyl terminated vinyl molar content of 0.06% and a raw methyl vinyl silicone rubber with a vinyl terminated vinyl molar content of 0.24% in a weight ratio of 7: 3, and (3).
4. The ultra-high pressure and high temperature resistant mixed silicone rubber according to claim 1 or 2, wherein the fumed silica has a specific surface area of 150-250 m2/g。
5. The ultra-high pressure and high temperature resistant mixing silicone rubber according to claim 1 or 2, wherein the flame retardant comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber crude rubber with vinyl terminated vinyl molar content of 0.04 percent, 5 parts of platinum catalyst and 1.5 parts of 1-methyl triazole.
6. A method for preparing the ultra-high pressure and high temperature resistant mixed silicone rubber according to any one of claims 1 to 5, comprising the steps of:
s1, putting methyl vinyl raw rubber, fumed silica, dimethyl diethoxysilane, hexamethyldisilazane and distilled water with different vinyl contents into an internal mixer, uniformly mixing at a low temperature, stirring for 60min, standing for 3-5 hours, vacuumizing, heating to 170 ℃, treating for 3 hours, cooling to obtain a base primer;
s2, adding zinc stearate, silicon micropowder, nitrogen compound, ferric oxide, titanium dioxide, vinyl triethoxysilane, cerium oxide and flame retardant into the base primer obtained in the step S1, and uniformly mixing at low temperature for 40-80min to obtain the coating.
7. The method of preparing the ultra-high pressure and high temperature resistant compounded silicone rubber according to claim 6, wherein the step S1 is performed by evacuating to-0.060 MPa to-0.080 MPa.
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| CN113088091B (en) * | 2021-03-23 | 2023-01-03 | 新安天玉有机硅有限公司 | High-temperature mixed silicone rubber for rail transit vehicle cables and preparation method thereof |
| CN113913017B (en) * | 2021-10-21 | 2023-04-28 | 北京天山新材料技术有限公司 | Rubber composition, single-component dealcoholized silicone rubber and preparation method thereof |
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