CN113088090A - High-resilience low-pressure-change silicone rubber material and preparation method thereof - Google Patents
High-resilience low-pressure-change silicone rubber material and preparation method thereof Download PDFInfo
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- CN113088090A CN113088090A CN202110248866.4A CN202110248866A CN113088090A CN 113088090 A CN113088090 A CN 113088090A CN 202110248866 A CN202110248866 A CN 202110248866A CN 113088090 A CN113088090 A CN 113088090A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 164
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 147
- 239000000463 material Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920001971 elastomer Polymers 0.000 claims abstract description 109
- 239000005060 rubber Substances 0.000 claims abstract description 107
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 100
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000006229 carbon black Substances 0.000 claims abstract description 46
- 229920002545 silicone oil Polymers 0.000 claims abstract description 46
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims abstract description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 230000006835 compression Effects 0.000 claims abstract description 10
- 238000007906 compression Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 52
- 238000004898 kneading Methods 0.000 claims description 45
- 239000003795 chemical substances by application Substances 0.000 claims description 37
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 28
- 229920002554 vinyl polymer Polymers 0.000 claims description 28
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 23
- YEECOJZAMZEUBB-UHFFFAOYSA-N 2,2,3,3,6,6,7,7-octamethyloctane Chemical compound CC(C)(C)C(C)(C)CCC(C)(C)C(C)(C)C YEECOJZAMZEUBB-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000004513 sizing Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 239000006082 mold release agent Substances 0.000 abstract description 5
- 230000032683 aging Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 13
- 238000001816 cooling Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000000806 elastomer Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention belongs to the field of silicon rubber, and particularly relates to a high-resilience low-pressure-change silicon rubber material and a preparation method thereof, wherein the mass ratio of the high-resilience low-pressure-change silicon rubber material is as follows: 100 portions of composite methyl vinyl silicone rubber crude rubber, 50 to 60 portions of precipitated white carbon black, 1 to 2 portions of dimethyl diethoxy silane, 0.3 to 0.5 portion of hydrogen-containing silicone oil, 0.1 to 0.3 portion of mold release agent and 2 to 4 portions of hydroxyl silicone oil, and provides a preparation method. The silicone rubber material provided by the invention has high rebound resilience, lower compression set rate, excellent tensile strength and aging resistance, can meet the requirements of products with the performance on the market, and widens the application range of the silicone rubber material.
Description
Technical Field
The invention belongs to the field of silicon rubber, and particularly relates to a high-resilience low-pressure-change silicon rubber material and a preparation method thereof.
Background
Silicone rubbers have a unique molecular structure, and unlike other organic rubbers, they have both inorganic and organic properties. Because of Si-O bond and inorganic property of silicon rubber, the silicon rubber is superior to common organic rubber in heat resistance, chemical stability, electric insulation, wear resistance, weather resistance and ozone resistance. The unique advantages of silicone rubber make it widely used in the aerospace, ammunition, automotive, construction, electrical and electronic, medical and food processing industries to replace petrochemicals.
With the demand of the market for reliable elastomers, the application range of the silicone rubber material with high resilience and low compression deformation rate is gradually expanded, but the rebound resilience, the mechanical property and the compression permanent deformation rate of the existing silicone rubber material cannot completely meet the demand of the market.
Disclosure of Invention
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a high-resilience low-pressure-change silicone rubber material comprises the following components in parts by mass: 100-110 parts of composite methyl vinyl silicone rubber crude rubber, 50-60 parts of precipitated white carbon black, 1-2 parts of dimethyl diethoxy silane, 0.3-0.5 part of hydrogen-containing silicone oil, 0.1-0.3 part of release agent and 2-4 parts of hydroxyl silicone oil.
Further, the composite methyl vinyl silicone rubber raw rubber is formed by combining any three of methyl vinyl silicone rubber raw rubber A, methyl vinyl silicone rubber raw rubber B, methyl vinyl silicone rubber raw rubber C, methyl vinyl silicone rubber raw rubber D and methyl vinyl silicone rubber raw rubber E; the vinyl content of the raw methyl vinyl silicone rubber A is 0.050-0.053%, and the molecular weight is 61-63 ten thousand; the vinyl content of the raw methyl vinyl silicone rubber B is 0.08-0.083%, and the molecular weight is 62-64 ten thousand; the vinyl content of the raw methyl vinyl silicone rubber C is 0.160-0.162%, and the molecular weight is 62-64 ten thousand; the vinyl content of the raw methyl vinyl silicone rubber D is 0.230 to 0.233 percent, and the molecular weight is 63 to 66 million; the vinyl content of the raw methyl vinyl silicone rubber E is 3.00-3.10%, and the molecular weight is 50-55 ten thousand. The composite crude rubber is composed of three types of silicon rubber crude rubbers with different vinyl contents and different molecular weights, vulcanized rubbers with different crosslinking densities can be debugged by the different vinyl contents and the different molecular weights, and the rubber material can achieve an excellent dispersion crosslinking mode while mechanical property reduction caused by concentrated crosslinking is avoided, so that the elasticity and the mechanical property are synergistically improved.
Further, the specific surface area of the precipitated silica white is 150-180m2(ii) in terms of/g. The white carbon black prepared by the precipitation method has the advantages that the rebound resilience of vulcanized rubber is improved, the reinforcing agent is played, the specific surface can be directly limited to the particle size of the white carbon black, the dispersibility of the white carbon black is more uniform based on the small particle size, and the silicon rubber material can be ensured to have better and excellent mechanical properties.
The release agent is zinc stearate or a mixture of zinc stearate and methyl vinyl silicone rubber crude rubber; further, the mass ratio of zinc stearate to raw methyl vinyl silicone rubber in the mixture is 1:1, the vinyl content of the raw methyl vinyl silicone rubber is 0.030-0.033%, and the molecular weight is 60-62 ten thousand.
A preparation method of a high-resilience low-pressure-change silicone rubber material comprises the following steps:
step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber raw rubber, a release agent, dimethyl diethoxy silane and 26-30% of precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 26-30% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
step 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain a high-resilience low-pressure-change silicone rubber product; the dipenta-penta-vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and ordinary methyl vinyl silicone rubber crude rubber in a weight ratio of 1: 1; the adding amount of the bis-dipentamethylenebisulphide is 1.2-1.5% of the silicon rubber material.
Further, the dipenta-penta-vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and methyl vinyl silicone rubber raw rubber with the vinyl content of 0.030-0.033% and the molecular weight of 60-62 ten thousand, and the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the methyl vinyl silicone rubber raw rubber is 1: 1.
From the above description, it can be seen that the present invention has the following advantages:
the silicone rubber material provided by the invention has high rebound resilience, lower compression set rate, excellent tensile strength and aging resistance, can meet the requirements of products with the performance on the market, and widens the application range of the silicone rubber material.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber B, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 2.50 parts of hydroxyl silicone oil, 1.25 parts of dimethyl diethoxy silane, 0.31 part of hydrogen-containing silicone oil and 0.30 part of zinc stearate;
the preparation method comprises the following steps: the components are added into an internal mixer in a certain sequence to be kneaded into a mass, and then the temperature is increased, and the temperature is controlled between 165 ℃ and 175 ℃. Closing the cover, kneading for 1h, and vacuumizing and kneading for 1 h. After cooling, a bis-penta vulcanizing agent is mixed and added in an open mill, and finally, the mixture is vulcanized and molded on a vulcanizing instrument.
Example 2
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber A, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 2.50 parts of hydroxyl silicone oil, 1.25 parts of dimethyl diethoxy silane, 0.31 part of hydrogen-containing silicone oil and 0.30 part of zinc stearate;
the preparation method comprises the following steps: the components are added into an internal mixer in a certain sequence to be kneaded into a mass, and then the temperature is increased and controlled between 165 ℃ and 175 ℃. Closing the cover, kneading for 1h, and vacuumizing and kneading for 1 h. After cooling, a bis-penta vulcanizing agent is mixed and added in an open mill, and finally, the mixture is vulcanized and molded on a vulcanizing instrument.
Example 3
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber B, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 2.50 parts of hydroxyl silicone oil, 0.05 part of vinyl silazane, 1.25 parts of dimethyl diethoxysilane, 0.31 part of hydrogen-containing silicone oil and 0.30 part of zinc stearate;
the preparation method comprises the following steps: the components are added into an internal mixer in a certain sequence to be kneaded into a mass, and then the temperature is increased, and the temperature is controlled between 165 ℃ and 175 ℃. Closing the cover, kneading for 1h, and vacuumizing and kneading for 1 h. After cooling, a bis-penta vulcanizing agent is mixed and added in an open mill, and finally, the mixture is vulcanized and molded on a vulcanizing instrument.
Example 4
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber B, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 2.50 parts of hydroxyl silicone oil, 5 parts of dimethyl diethoxy silane and 1.50 parts of hydrolysate with the pH value of 3.6, 0.31 part of hydrogen-containing silicone oil and 0.30 part of zinc stearate;
the preparation method comprises the following steps: step 1, adding 30 parts of dimethyldiethoxysilane and 9 parts of dilute hydrochloric acid with the pH value of 3.6 into a 100ml beaker, and stirring and hydrolyzing the mixture by using a magnetic stirrer until the solution is clear to obtain a dimethyldiethoxysilane hydrolysate;
step 2, adding the components into an internal mixer in a certain order, kneading into a mass, and then heating, wherein the temperature is controlled between 165 and 175 ℃. Closing the cover, kneading for 1h, and vacuumizing and kneading for 1 h. After cooling, a bis-penta vulcanizing agent is mixed and added in an open mill, and finally, the mixture is vulcanized and molded on a vulcanizing instrument.
Example 5
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber D, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 1.25 parts of dimethyl diethoxysilane, 0.4 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate and 2.5 parts of hydroxyl silicone oil;
the preparation method comprises the following steps: step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber raw rubber, a release agent, dimethyl diethoxy silane and 28% precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 28% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
and 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain the high-resilience low-pressure-change silicone rubber product.
The vulcanized rubber products prepared by the five groups of examples are respectively numbered and tested for performance, and the results are shown in the following table:
the silicone rubber material has the advantages of low cost, simple process and strong industrial large-scale production feasibility. Furthermore, from the above data it can be seen that: through comparative analysis of five groups of examples, the silicone rubber product prepared in example 5 has high rebound rate, and has good tensile strength and tear strength, and in addition, the excellent compression set rate proves that the silicone rubber product has excellent anti-aging performance, so that the silicone rubber product can meet the performance requirements of most elastomer industries.
In addition, the comparative tests of examples 1, 2 and 5 confirm that: in the conventional precipitation method silicone rubber, along with the increase of vinyl content in raw methyl vinyl silicone rubber, rebound resilience, tensile strength and elongation at break are continuously increased, but the elongation at break is continuously reduced to a certain extent. Furthermore, the compression set can only be significantly reduced when the vinyl content reaches a certain level;
the comparative tests of examples 1 and 3 confirm that: the effect of improving the mechanical property of the silicone rubber can be achieved by adding the vinyl silazane to treat the white carbon black, but the compression permanent deformation rate is not obviously improved. In addition, the gum is yellow and ammoniacal;
comparative experiments of examples 1 and 4 confirmed that: the precipitated silica white is treated by hydrolysate of dimethyl diethoxysilane, so that the effect of improving the mechanical property of the silicone rubber can not be achieved, and the compression permanent deformation rate of the precipitated silica white is obviously increased.
Example 6
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber A, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 51 parts of precipitated white carbon black, 1.25 parts of dimethyl diethoxysilane, 0.1 part of hydrogen-containing silicone oil, 0.3 part of zinc stearate and 2.5 parts of hydroxyl silicone oil;
the preparation method comprises the following steps: step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber crude rubber, zinc stearate, dimethyl diethoxy silane and 26% precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 26% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
step 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain a high-resilience low-pressure-change silicone rubber product; the adding amount of the bis-dipentamethylenebisulphide is 1.5 percent of that of the silicon rubber material.
Example 7
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber A, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 60 parts of precipitated white carbon black, 2 parts of dimethyl diethoxysilane, 0.5 part of hydrogen-containing silicone oil, 0.3 part of zinc stearate and 4 parts of hydroxyl silicone oil;
the preparation method comprises the following steps: step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber crude rubber, zinc stearate, dimethyl diethoxy silane and 30% precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 30% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
and 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain the high-resilience low-pressure-change silicone rubber product, wherein the adding amount of the bis-di-pentavulcanizing agent is 1.2% of that of the silicone rubber material.
Example 8
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber B, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 50 parts of precipitated white carbon black, 1 part of dimethyl diethoxysilane, 0.3 part of hydrogen-containing silicone oil, 0.1g of mold release agent and 2 parts of hydroxyl silicone oil;
the release agent is a mixture of zinc stearate and raw methyl vinyl silicone rubber; the mass ratio of zinc stearate to raw methyl vinyl silicone rubber in the mixture is 1:1, the vinyl content of the raw methyl vinyl silicone rubber is 0.030%, and the molecular weight is 60-62 ten thousand.
The preparation method comprises the following steps: step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber raw rubber, a release agent, dimethyl diethoxy silane and 26% precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 26% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
step 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain a high-resilience low-pressure-change silicone rubber product; the dipenta-penta vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and methyl vinyl silicone rubber raw rubber with the vinyl content of 0.033% and the molecular weight of 60-62 ten thousand, and the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the methyl vinyl silicone rubber raw rubber is 1: 1; the adding amount of the bis-dipentamethylenebisulphide is 1.2 percent of that of the silicon rubber material.
Example 9
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber D, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 1.0 part of dimethyl diethoxysilane, 0.31 part of hydrogen-containing silicone oil, 0.3 part of mold release agent and 2.5g of hydroxyl silicone oil;
the release agent is a mixture of zinc stearate and raw methyl vinyl silicone rubber; the mass ratio of zinc stearate to raw methyl vinyl silicone rubber in the mixture is 1:1, the vinyl content of the raw methyl vinyl silicone rubber is 0.033%, and the molecular weight is 60-62 ten thousand.
The preparation method comprises the following steps: step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber raw rubber, a release agent, dimethyl diethoxy silane and 30% precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 30% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
step 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain a high-resilience low-pressure-change silicone rubber product; the dipenta-penta vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and methyl vinyl silicone rubber raw rubber with the vinyl content of 0.030% and the molecular weight of 60-62 ten thousand, and the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the methyl vinyl silicone rubber raw rubber is 1: 1; the adding amount of the bis-dipentamethylenebisulphide is 1.5 percent of that of the silicon rubber material.
Example 10
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber D, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 2.50 parts of hydroxyl silicone oil, 1.25 parts of dimethyl diethoxy silane, 0.36 part of hydrogen-containing silicone oil and 0.3 part of mold release agent;
the release agent is a mixture of zinc stearate and raw methyl vinyl silicone rubber; the mass ratio of the zinc stearate to the raw methyl vinyl silicone rubber in the mixture is 1:1, the vinyl content of the raw methyl vinyl silicone rubber is 0.031%, and the molecular weight is 60-62 ten thousand.
The preparation method comprises the following steps: step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber raw rubber, a release agent, dimethyl diethoxy silane and 28% precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 28% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
step 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain a high-resilience low-pressure-change silicone rubber product; the dipenta-penta vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and methyl vinyl silicone rubber raw rubber with the vinyl content of 0.032% and the molecular weight of 60-62 ten thousand, and the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the methyl vinyl silicone rubber raw rubber is 1: 1; the adding amount of the bis-dipentamethylenebisulphide is 1.5 percent of that of the silicon rubber material.
Example 11
A high-resilience and low-pressure-change silicone rubber material,
the mass ratio is as follows: 37 parts of methyl vinyl silicone rubber crude rubber D, 60 parts of methyl vinyl silicone rubber crude rubber C, 3 parts of methyl vinyl silicone rubber crude rubber E, 56 parts of precipitated white carbon black, 4.0 parts of hydroxyl silicone oil, 1.5 parts of dimethyl diethoxy silane, 0.36 part of hydrogen-containing silicone oil and 0.3 part of mold release agent;
the release agent is a mixture of zinc stearate and raw methyl vinyl silicone rubber; the mass ratio of the zinc stearate to the raw methyl vinyl silicone rubber in the mixture is 1:1, the vinyl content of the raw methyl vinyl silicone rubber is 0.0312%, and the molecular weight is 60-62 ten thousand.
The preparation method comprises the following steps: step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber raw rubber, a release agent, dimethyl diethoxy silane and 26% precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 26% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
step 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain a high-resilience low-pressure-change silicone rubber product; the dipenta-penta vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and methyl vinyl silicone rubber raw rubber with the vinyl content of 0.032% and the molecular weight of 60-62 ten thousand, and the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the methyl vinyl silicone rubber raw rubber is 1: 1; the adding amount of the bis-dipentamethylenebisulphide is 1.4 percent of that of the silicon rubber material.
The rubbers of examples 6 to 11 all exhibited effects not inferior to those of example 5.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (8)
1. A high-resilience low-pressure-change silicone rubber material is characterized in that: the mass ratio is as follows: 100-110 parts of composite methyl vinyl silicone rubber crude rubber, 50-60 parts of precipitated white carbon black, 1-2 parts of dimethyl diethoxy silane, 0.3-0.5 part of hydrogen-containing silicone oil, 0.1-0.3 part of release agent and 2-4 parts of hydroxyl silicone oil.
2. The high resilience, low pressure change silicone rubber material of claim 1, wherein: the composite methyl vinyl silicone rubber raw rubber is formed by combining any three of methyl vinyl silicone rubber raw rubber A, methyl vinyl silicone rubber raw rubber B, methyl vinyl silicone rubber raw rubber C, methyl vinyl silicone rubber raw rubber D and methyl vinyl silicone rubber raw rubber E; the vinyl content of the raw methyl vinyl silicone rubber A is 0.050-0.053%, and the molecular weight is 61-63 ten thousand; the vinyl content of the raw methyl vinyl silicone rubber B is 0.08-0.083%, and the molecular weight is 62-64 ten thousand; the vinyl content of the raw methyl vinyl silicone rubber C is 0.160-0.162%, and the molecular weight is 62-64 ten thousand; the vinyl content of the raw methyl vinyl silicone rubber D is 0.230 to 0.233 percent, and the molecular weight is 63 to 66 million; the vinyl content of the raw methyl vinyl silicone rubber E is 3.00-3.10%, and the molecular weight is 50-55 ten thousand.
3. The high resilience, low pressure change silicone rubber material of claim 1, wherein: the specific surface area of the precipitated white carbon black is 150-180m2/g。
4. The high resilience, low pressure change silicone rubber material of claim 1, wherein: the release agent adopts zinc stearate or a mixture of the zinc stearate and methyl vinyl silicone rubber crude rubber.
5. The high resilience, low pressure change silicone rubber material of claim 4, wherein: the mass ratio of zinc stearate to raw methyl vinyl silicone rubber in the mixture is 1:1, the vinyl content of the raw methyl vinyl silicone rubber is 0.030-0.033%, and the molecular weight is 60-62 ten thousand.
6. A preparation method of a high-resilience low-pressure-change silicone rubber material is characterized by comprising the following steps: the method comprises the following steps:
step 1, weighing raw materials according to a mass ratio, and adding the composite methyl vinyl silicone rubber raw rubber, a release agent, dimethyl diethoxy silane and 26-30% of precipitated white carbon black into a kneading machine to knead into a dough;
step 2, adding 26-30% of precipitated white carbon black and hydroxyl silicone oil into the mixture obtained in the step 1, and kneading the mixture into a dough;
step 3, dividing the rest precipitated white carbon black into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, and kneading the mixture into a dough;
step 4, heating the rubber material obtained in the step 3 to 165-175 ℃, continuing kneading, closing the cover for 1h, vacuumizing for 1h, standing for 2-3h, and filtering to obtain a finished rubber material; the cover closing time is counted from the temperature rise of the sizing material to 150 ℃, and the vacuum degree of the vacuumizing is-0.08 MPa to-0.06 MPa;
step 5, adding a bis-di-penta vulcanizing agent into the rubber material obtained in the step 4, and vulcanizing and forming to obtain a high-resilience low-pressure-change silicone rubber product; the adding amount of the bis-dipentamethylenebisulphide is 1.2-1.5% of the silicon rubber material.
7. The method for preparing a high resilience, low compression set silicone rubber according to claim 6, wherein: the dipenta-penta-vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and ordinary methyl vinyl silicone rubber crude rubber in a weight ratio of 1: 1.
8. The method for preparing a high resilience, low compression set silicone rubber according to claim 7, wherein: the dipenta-penta vulcanizing agent is a paste mixture consisting of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and methyl vinyl silicone rubber raw rubber with the vinyl content of 0.030-0.033% and the molecular weight of 60-62 ten thousand, and the mass ratio of the 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide to the methyl vinyl silicone rubber raw rubber is 1: 1.
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