CN111019355A - High-temperature-resistant silicon rubber - Google Patents
High-temperature-resistant silicon rubber Download PDFInfo
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- CN111019355A CN111019355A CN201911327770.6A CN201911327770A CN111019355A CN 111019355 A CN111019355 A CN 111019355A CN 201911327770 A CN201911327770 A CN 201911327770A CN 111019355 A CN111019355 A CN 111019355A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 91
- 239000004945 silicone rubber Substances 0.000 claims abstract description 56
- 239000000654 additive Substances 0.000 claims abstract description 20
- 230000000996 additive effect Effects 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 16
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 10
- 229920002554 vinyl polymer Polymers 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 description 20
- 229920001971 elastomer Polymers 0.000 description 14
- 239000005060 rubber Substances 0.000 description 14
- 229920002050 silicone resin Polymers 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N methyl pentane Natural products CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- XJWOWXZSFTXJEX-UHFFFAOYSA-N phenylsilicon Chemical compound [Si]C1=CC=CC=C1 XJWOWXZSFTXJEX-UHFFFAOYSA-N 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides high-temperature-resistant silicon rubber which is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 20-50 parts of white carbon black, 1-10 parts of hydroxyl silicone oil, 1-15 parts of heat-resistant additive and 1-6 parts of dicumyl peroxide. The heat-resistant additive in the high-temperature-resistant silicon rubber raw material can obviously improve the residual quality of the silicon rubber at high temperature, improve the initial degradation temperature, overcome the defect of poor compatibility of the common heat-resistant additive and the silicon rubber, and improve the mechanical properties of the silicon rubber, so that the silicon rubber not only has good heat resistance, but also has excellent mechanical properties.
Description
Technical Field
The disclosure relates to the field of silicone rubber, and particularly relates to high-temperature-resistant silicone rubber.
Background
The silicone rubber is a special rubber which is formed by alternately bonding Si atoms and O atoms to form a molecular main chain skeleton and taking various organic groups as side groups. Because the carbon chain structure of the silicon rubber is different from that of common rubber, the silicon rubber has excellent high and low temperature resistance, weather resistance, electric insulation, mildew resistance, physiological inertia and the like. The common silicon rubber can be used for a long time at the temperature of-50-260 ℃ and keeps elasticity, and the heat-resistant temperature of the phenyl silicon rubber reaches 300-350 ℃. However, with the development of science and technology, especially in the field of aerospace, the heat resistance of the current silicone rubber cannot meet the use requirements of some special fields. Therefore, the heat resistance of the silicone rubber is to be further improved.
At present, the heat resistance of the silicone rubber is mainly improved by adding inorganic heat-resistant additives or silicone resin and the like. The common inorganic heat-resistant additive is iron oxide, cerium oxide, nickel oxide, cobalt oxide, white carbon black and the like, or the heat-resistant additive is prepared by modifying the metal oxides and mixing the metal oxides in different proportions. Adopting nano CeO in Song Yuan Wen2Nano Fe2O3And Al treated with a silane coupling agent2O3The heat-resistant silicon rubber prepared by using the heat-resistant filler obviously improves the heat resistance of the silicon rubber. The silicone resin can be crosslinked with the silicone rubber, so that the crosslinking degree of the silicone rubber is improved, the reinforcing effect is achieved, the spiral structure of the silicone rubber is damaged to a certain extent, the main chain is more difficult to be subjected to unbuckled degradation, and the high-temperature resistance of the silicone rubber is improved. Kang Min-Joo and the like increase the diffusivity of nano-silica in silicone resin by carrying out ozone treatment on the nano-silica, and add the silicone resin mixed with the nano-silica into silicone rubber by a melt blending method to prepare a novel silicone rubber/silicone resin composite material, and along with the increase of the content of the silicone resin in the composite material, the thermal stability of the composite material is obviously improved.
In summary, the current research on the preparation of the high temperature resistant silicone rubber has a certain progress, but the existing high temperature resistant silicone rubber has the following defects: the metal oxide has larger polarity, has poorer compatibility with the silicon rubber, is difficult to disperse, and can cause serious reduction of the elasticity and the mechanical property of the silicon rubber when being added too much; the compatibility of the silicone resin and the silicone rubber is better, but the improvement on the high-temperature resistance of the silicone rubber is limited, and the mechanical properties such as the hardness of the silicone rubber are also influenced to a certain extent. Therefore, the research on the silicone rubber with good high temperature resistance and mechanical property is of great significance.
Disclosure of Invention
The purpose of the disclosure is to provide a high-temperature resistant silicone rubber so as to achieve the purpose of improving the heat resistance and mechanical properties of the silicone rubber.
In order to realize the purpose, the technical scheme is as follows:
the high-temperature-resistant silicon rubber comprises the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 20-50 parts of white carbon black, 1-10 parts of hydroxyl silicone oil, 1-15 parts of heat-resistant additive and 1-6 parts of dicumyl peroxide.
The molecular weight of the methyl vinyl silicone rubber is 40-55 ten thousand, wherein the content of vinyl is 0.05-4 mol%.
The specific surface area of the white carbon black is 200-450m2/g。
The hydroxyl content in the hydroxyl silicone oil is 4-10 wt%.
The heat-resistant additive has the structure that:
wherein m is an integer greater than or equal to 1; p is an integer of 1 or more; r is
n is an integer of 0 to 10.
The beneficial effects of this disclosure are: the heat-resistant additive in the high-temperature-resistant silicon rubber raw material can obviously improve the residual quality of the silicon rubber at high temperature, improve the initial degradation temperature, overcome the defect of poor compatibility of the common heat-resistant additive and the silicon rubber, and improve the mechanical property of the silicon rubber, so that the silicon rubber not only has good heat resistance, but also has excellent mechanical property.
Detailed Description
The following steps are only used for illustrating the technical scheme of the disclosure and are not limited; although the present disclosure has been described in detail with reference to the foregoing steps, those of ordinary skill in the art will understand that: the technical solutions recorded in the foregoing steps may still be modified, or some or all of the technical features may be equivalently replaced; and such modifications or substitutions do not depart from the scope of the respective technical solutions of the steps of the present disclosure.
Example 1
The high-temperature-resistant silicon rubber comprises the following raw materials in parts by weight: 80 parts of methyl vinyl silicone rubber (molecular weight: 45 ten thousand) having a vinyl content of 0.08 mol%, 20 parts of methyl vinyl silicone rubber (molecular weight: 55 ten thousand) having a vinyl content of 4 mol%, and 25 parts of white carbon black (specific surface area: 200 m)2/g) and 1 part of hydroxy silicone oil (hydroxyl content 4 wt%), 15 parts of heat-resistant additive and 1 part of dicumyl peroxide.
A preparation method of high-temperature-resistant silicon rubber comprises the following specific operation steps:
(1) mixing the methyl vinyl silicone rubber, the white carbon black and the hydroxyl silicone oil in a kneading machine according to the mass parts, mixing for 4 hours at room temperature, heating to 150 ℃, continuing to mix for 2 hours, then vacuumizing and mixing for 1 hour, and cooling to room temperature to obtain the silicone rubber base rubber;
(2) and adding the heat-resistant additive and dicumyl peroxide into the base rubber on an open mill, uniformly mixing, taking out the base rubber, vulcanizing at 155 ℃ for 15min, and then vulcanizing at 190 ℃ for two times for 4h to obtain the high-temperature-resistant silicon rubber.
Example 2 preparation of a high temperature resistant Silicone rubber
The high-temperature-resistant silicon rubber comprises the following raw materials in parts by weight: 82 parts of methyl vinyl silicone rubber (molecular weight: 50 ten thousand) having a vinyl content of 0.45 mol%, 18 parts of methyl vinyl silicone rubber (molecular weight: 55 ten thousand) having a vinyl content of 3 mol%, and 35 parts of white carbon black (specific surface area: 400 m)2Per g) and 10 parts of hydroxylSilicone oil (hydroxyl content 10 wt%), 15 parts of heat-resistant additive and 6 parts of dicumyl peroxide.
A preparation method of high-temperature-resistant silicon rubber comprises the following specific operation steps:
(1) mixing the methyl vinyl silicone rubber, the white carbon black and the hydroxyl silicone oil in a kneading machine according to the mass parts, mixing for 4 hours at room temperature, heating to 170 ℃, continuing mixing for 1 hour, then vacuumizing and mixing for 1 hour, and cooling to room temperature to obtain the silicone rubber base rubber;
(2) and adding the heat-resistant additive and dicumyl peroxide into the base rubber on an open mill, uniformly mixing, taking out the base rubber, vulcanizing at 160 ℃ for 6min, and then vulcanizing at 210 ℃ for two times for 1h to obtain the high-temperature-resistant silicon rubber.
Example 3
The high-temperature-resistant silicon rubber comprises the following raw materials in parts by weight: 75 parts of methyl vinyl silicone rubber (molecular weight: 55 ten thousand) having a vinyl content of 0.09 mol%, 25 parts of methyl vinyl silicone rubber (molecular weight: 50 ten thousand) having a vinyl content of 2 mol%, and 30 parts of white carbon black (specific surface area: 200 m)2/g) and 7 parts of hydroxysilicone oil (hydroxyl content 6 wt%), 9 parts of heat-resistant additive and 5 parts of dicumyl peroxide.
A preparation method of high-temperature-resistant silicon rubber comprises the following specific operation steps:
(1) mixing the methyl vinyl silicone rubber, the white carbon black and the hydroxyl silicone oil in a kneading machine according to the mass parts, mixing for 4 hours at room temperature, heating to 140 ℃, continuing to mix for 4 hours, then vacuumizing and mixing for 1 hour, and cooling to room temperature to obtain the silicone rubber base rubber;
(2) and adding the heat-resistant additive and dicumyl peroxide into the base rubber on an open mill, uniformly mixing, taking out the base rubber, vulcanizing at 150 ℃ for 30min, and then vulcanizing at 170 ℃ for 5h for two times to obtain the high-temperature-resistant silicon rubber.
Example 4 high temperature resistant Silicone rubber Performance testing
Comparative example 1
90 parts of methyl vinyl silicone rubber (molecular weight: 56 ten thousand) having a vinyl content of 0.03 mol%, 10 parts of methyl vinyl silicone rubber (molecular weight: 60 ten thousand) having a vinyl content of 5 mol%, and 15 parts of fumed silica (1Specific surface area of 180m2Mixing the raw materials in parts by weight of/g) and 12 parts of hydroxyl silicone oil (the hydroxyl content is 3 wt%) in a kneader, mixing for 4 hours at room temperature, heating to 150 ℃, continuing mixing for 2 hours, vacuumizing and mixing for 1 hour, and cooling to room temperature to obtain the silicone rubber base rubber;
adding 2 parts by mass of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane into the base rubber on an open mill, uniformly mixing, taking out the base rubber, vulcanizing at 155 ℃ for 15min, and vulcanizing at 190 ℃ for two times for 4h to obtain a sample for testing high temperature resistance and mechanical properties.
The performance of the silicone rubbers prepared in example 1, example 2, example 3 and comparative example 1 are respectively tested, and the tensile strength and the elongation at break of the silicone rubber are firstly measured according to GB/T528-one 2009; then, the tearing strength of the silicone rubber is determined according to GB/T529-; determining the Shore A hardness of the silicone rubber according to GB/T531-2008; the thermal stability parameters of the silicone rubber were tested by thermogravimetric analysis.
As shown in Table 1, it can be seen from Table 1 that comparative example 1 has a residual mass of only 25% by weight in an air atmosphere at 700 ℃ and a residual mass of only 18% in an air atmosphere at 700 ℃. The residual mass of the silicon rubber of the examples 1, 2 and 3 in the 700 ℃ air atmosphere is up to 45-59 wt%, and the residual mass in the 700 ℃ nitrogen atmosphere is 37-49 wt%; the heat-resistant additive used in the method can effectively improve the heat stability of the silicone rubber; meanwhile, the mechanical properties of the silicone rubbers of examples 1, 2 and 3 are higher than those of the silicone rubber of comparative example 1, which shows that the heat-resistant additive not only can not damage the mechanical properties of the silicone rubber, but also can improve the mechanical properties of the silicone rubber. Therefore, the high-temperature-resistant silicone rubber disclosed by the disclosure has excellent thermal stability and mechanical properties.
TABLE 1 mechanical and high temperature resistance of Silicone rubber
Claims (5)
1. The high-temperature-resistant silicon rubber is characterized by comprising the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 20-50 parts of white carbon black, 1-10 parts of hydroxyl silicone oil, 1-15 parts of heat-resistant additive and 1-6 parts of dicumyl peroxide.
2. The high temperature resistant silicone rubber according to claim 1, wherein the methyl vinyl silicone rubber has a molecular weight of 40 to 55 ten thousand, and the vinyl content is 0.05 to 4 mol%.
3. The high temperature resistant silicone rubber as recited in claim 1, wherein the silica white has a specific surface area of 200-450m2/g。
4. The high temperature resistant silicone rubber of claim 1, wherein the hydroxyl silicone oil has a hydroxyl content of 4 to 10 wt%.
5. The high temperature resistant silicone rubber of claim 1, wherein the heat resistant additive is of the structure:
wherein m is an integer greater than or equal to 1; p is an integer of 1 or more; r is
n is an integer of 0 to 10.
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| CN201911327770.6A CN111019355A (en) | 2019-12-20 | 2019-12-20 | High-temperature-resistant silicon rubber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114058188A (en) * | 2021-12-10 | 2022-02-18 | 浙江恒业成有机硅有限公司 | High-temperature-resistant medium-temperature vulcanized silicone rubber and preparation method thereof |
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-
2019
- 2019-12-20 CN CN201911327770.6A patent/CN111019355A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114058188A (en) * | 2021-12-10 | 2022-02-18 | 浙江恒业成有机硅有限公司 | High-temperature-resistant medium-temperature vulcanized silicone rubber and preparation method thereof |
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