CN108129850B - High-resilience high-strength silicone rubber and preparation method thereof - Google Patents
High-resilience high-strength silicone rubber and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- 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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- C—CHEMISTRY; METALLURGY
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- 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 discloses high-resilience high-strength silicone rubber and a preparation method thereof. The high-resilience high-strength silicone rubber comprises the following raw material components in parts by weight: 100 parts of methyl vinyl silicone rubber; 2-10 parts of ultra-high molecular weight dimethyl silicone rubber; 10-40 parts of precipitated white carbon black; 5-30 parts of superfine silicon powder; 3-15 parts of silicone powder; 1-3 parts of hydroxy vinyl silicone oil; 0.1 to 1 portion of hydrogen-containing silicone oil; 0.05 to 1 portion of internal release agent and 0.3 to 2 portions of vulcanizing agent. The high-resilience high-strength silicone rubber reduces the consumption of low-viscosity hydroxyl silicone oil, obviously improves the resilience of the vulcanized silicone rubber, and obviously improves the overall performance of the silicone rubber; the preparation method is simple and easy to operate.
Description
Technical Field
The invention relates to high-resilience high-strength silicone rubber and a preparation method thereof, belonging to the field of silicone rubber.
Background
Silicone rubber is a high molecular elastomer having both organic and inorganic material properties, has many excellent properties such as weather resistance, electrical properties, low compression set, heat resistance and cold resistance, and is widely used in the fields of electrical equipment, motor vehicles, construction, medicine, food industry and the like. For example, it can be used as rubber contacts in remote controllers, computer terminals, musical instruments, etc., building pads, fixing rollers, developing rollers, copying rollers, spotting rollers, and paper feeding rollers in commercial machines, vibration-proof rubbers for audio equipment, etc., packaging of high-density magnetic disks, and cable sheath materials.
The resilience performance is a key index for measuring the quality of the sealing material, the capability of the sealing material for filling sealing defects and compensating elasticity is embodied, and a good sealing material has good resilience. The silicon rubber has good rebound resilience and smaller compression deformability, can be used as a manufacturing raw material of kitchen supplies, shaft sealing rings, gaskets, nipples, sundry joints, office equipment and the like, and has wide application range. Along with the development of science and technology, higher requirements are provided for the resilience performance of the silicon rubber, the high-temperature vulcanized silicon rubber in the prior art can not meet the special requirements of certain products in the market due to lower resilience,
at present, the silicon rubber has higher resilience mainly through a matching technology and modification technologies such as adding a new auxiliary agent, changing a crosslinking mode, copolymerizing and blending and the like. For example, in patent publication No. CN106633910A, a high resilience and high tear resistance silicone rubber composition is prepared by using different terminal vinyl raw rubber and treated white carbon black; in patent publication No. CN104194352A, high-elasticity silicone rubber is prepared by using methyl vinyl silicone rubber, chlorinated butyl rubber, phenolic resin, etc. as raw materials and by blending. Although the above two methods can improve the rebound resilience of silicone rubber, the improvement is not obvious.
Disclosure of Invention
In order to overcome the defects of poor rebound resilience and the like of silicon rubber in the prior art, the invention provides high-resilience high-strength silicon rubber and a preparation method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the high-resilience high-strength silicone rubber comprises the following raw material components in parts by weight:
100 parts of methyl vinyl silicone rubber;
2-10 parts of ultra-high molecular weight dimethyl silicone rubber;
10-40 parts of precipitated white carbon black;
5-30 parts of superfine silicon powder;
3-15 parts of silicone powder
1-3 parts of hydroxy vinyl silicone oil;
0.1 to 1 portion of hydrogen-containing silicone oil;
0.05 to 1 portion of internal release agent;
0.3 to 2 portions of vulcanizing agent.
At present, in the silicone rubber industry, the dispersion of a reinforcing filler in silicone rubber is promoted by adding a large amount of hydroxyl silicone oil or vinyl silicone oil, but the rebound resilience of the silicone rubber is greatly reduced by adding low-viscosity silicone oil. The principle of the invention is that the method of adding lubricant silicone powder is used for promoting the dispersion of the reinforcing filler in the silicone rubber, improving the compatibility between the reinforcing filler and the silicone rubber, and reducing the addition amount of low-viscosity silicone oil to the maximum extent, thereby improving the resilience of the silicone rubber; meanwhile, methyl vinyl silicone rubber and dimethyl crude rubber with ultrahigh molecular weight are compounded to serve as basic crude rubber, and precipitated white carbon black and superfine silicon powder are mixed and matched to serve as reinforcing filler, so that the resilience of the silicone rubber is improved together; the applicant finds that the synergistic effect among the selected material components is obvious, so that the rebound resilience and the strength of the silicone rubber are remarkably improved.
In order to further promote the synergistic effect among the components and further improve the rebound resilience and other mechanical properties of the silicone rubber, the methyl vinyl silicone rubber is prepared from the following components in percentage by mass (5-7): (5-3) compounding the first methyl vinyl silicone rubber and the second methyl vinyl silicone rubber, wherein the first methyl vinyl silicone rubber contains 0.03-0.09 mol% of vinyl and has a molecular weight of 65-75 ten thousand; the second vinyl silicone rubber has vinyl molar content of 0.25-1.5% and molecular weight of 50-65 ten thousand.
Preferably, the molecular weight of the ultra-high molecular weight dimethyl silicone rubber is 100-120 ten thousand, and the chain link of the ultra-high molecular weight dimethyl silicone rubber does not contain vinyl, and the structural formula is as follows:
wherein the value range of m is 13000-17000. This further ensures the resilience of the resulting product.
Preferably, the mass content of siloxane in the silicone powder is 40-60%, so that the dispersibility and compatibility of materials can be further improved, and the resilience of the silicone rubber is further improved.
The silicone powder is a powder formed by mixing siloxane, silicon dioxide and other auxiliary agents (such as a silane coupling agent).
The specific surface area of the precipitated white carbon black is not less than 150m2(ii) in terms of/g. Preferably, the precipitated silica has a specific surface area of 150m2(ii)/g or 200m2/g。
Preferably, the particle size of the superfine silicon powder is 0.3-2 μm, preferably 0.5-1 μm. Thus further improving the compatibility of the raw material components and the mechanical property of the silicon rubber.
Preferably, the hydroxyl vinyl silicone oil is hydroxyl-terminated vinyl silicone oil, and the structure of the hydroxyl-terminated vinyl silicone oil is as follows:
wherein the value range of m is 50-150, the value range of n is 5-20, the viscosity of the hydroxyl vinyl silicone oil is 100-250 cst, and the vinyl content is 3.5-10%. Thus further improving the compatibility of the raw material components and the mechanical property of the silicon rubber.
Preferably, the hydrogen content in the hydrogen-containing silicone oil is 1.5 wt% or more, so that the synergistic effect between the raw material components can be further promoted, and the rebound resilience of the silicone rubber can be further improved.
Preferably, the release agent is stearic acid or stearate, and the stearate is at least one of zinc stearate, magnesium stearate or calcium stearate; the vulcanizing agent is peroxide bis-tetra (2, 4-dichlorobenzoyl peroxide) or bis-penta (2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide). Thus, the synergistic effect among the raw material components can be further promoted, and the rebound resilience, the mechanical property and the like of the silicone rubber can be further improved.
The preparation method of the high-resilience high-strength silicone rubber comprises the following steps of sequentially connecting:
1) uniformly mixing methyl vinyl silicone rubber, ultra-high molecular weight dimethyl silicone rubber, silicone powder, hydroxyl vinyl silicone oil, hydrogen-containing silicone oil and an internal mold release agent in a kneading machine;
2) adding precipitated white carbon black and superfine silicon powder into the material obtained in the step 1), wherein the precipitated white carbon black and the superfine silicon powder are uniformly added for four times, the four-time adding amounts of the precipitated white carbon black and the superfine silicon powder are respectively 40 +/-3%, 25 +/-3%, 20 +/-3% and 15 +/-3%, stirring and kneading at the temperature of 60-80 ℃ under normal pressure after the feeding is finished, forming into clusters, and continuously kneading for 10-30 min after the clusters are formed;
3) heating the material obtained in the step 2) to 100-120 ℃, banburying for 1.5 +/-0.2 h under the vacuum degree of-0.8 MPa-0.9 MPa, and then cooling and placing for 24 +/-2 h to obtain rubber compound;
4) uniformly mixing the rubber compound obtained in the step 3) with a vulcanizing agent, vulcanizing at 175 +/-5 ℃ for 5 +/-1 min, and then vulcanizing at 200 +/-5 ℃ for 4 +/-1 h to obtain the high-resilience high-strength silicone rubber.
The prior art is referred to in the art for techniques not mentioned in the present invention.
The high-resilience high-strength silicone rubber reduces the consumption of low-viscosity hydroxyl silicone oil, obviously improves the resilience of the vulcanized silicone rubber, and obviously improves the overall performance of the silicone rubber; the preparation method is simple and easy to operate.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
The unit of measurement "part(s)" of each substance in each example described below means part(s) by weight.
The raw materials in the following examples are all commercially available products.
Example 1
In parts by mass, 70 parts of a dimethylvinyl terminated methyl vinyl silicone rubber (Dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 65 ten thousand and a vinyl molar content of 0.05%, 30 parts of a dimethylvinyl terminated end, methyl vinyl silicone rubber (dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 55 ten thousand and a vinyl molar content of 0.25%, dimethyl silicone gum (dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 100 ten thousand, 5 parts of silicone powder (KJ-B01, Kanji plastics toughening Material Co., Ltd., Jiande), 1.0 part of hydroxy vinyl silicone oil (Stannless all-dimensional chemical Co., Ltd., vinyl content of 6%) having a kinematic viscosity of 155cst, 0.5 part of hydrogen-containing silicone oil (Stannless all-dimensional chemical Co., Ltd.) having a hydrogen content of 1.53%, and 0.2 part of calcium stearate were mixed uniformly in a kneader.
2) In step 1) 15 parts of a mixture having a specific surface area of 150m are added2The silica gel rubber is prepared by the steps of mixing precipitated silica gel (Fujian Yuanhong chemical Co., Ltd.) and 5 parts of superfine silica powder (Guangdong south China sea Xinchuan mineral Co., Ltd., particle size of 1 μm), wherein the silica gel and the superfine silica powder are uniformly added for four times, the adding amount of the precipitated silica gel and the superfine silica powder for four times is 40%, 25%, 20% and 15% in sequence, stirring and kneading at normal pressure and 70 ℃ after the materials are added, agglomerating, and continuously kneading for 20min after agglomerating to obtain the rubber material.
3) Heating the rubber material obtained in the step 2) to 110 ℃, carrying out vacuum high-temperature banburying for 1.5h under the vacuum degree of-0.8 MPa to-0.9 MPa, and cooling and standing for 24h to obtain the rubber compound.
4) Uniformly mixing 100 parts of the rubber compound obtained in the step 3) and 0.65 part of peroxide vulcanizing agent bis-penta (2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane) in an open mill, vulcanizing at 175 ℃ for 5 minutes, and then vulcanizing at 200 ℃ for 4 hours to obtain the high-elasticity high-strength silicone rubber composition.
The obtained high-elasticity high-strength silicone rubber composition was subjected to a performance test, and the results are shown in table 1.
Example 2
In parts by mass, 80 parts of a dimethylvinyl terminated methyl vinyl silicone rubber (Dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 70 ten thousand and a vinyl molar content of 0.06%, 20 parts of a dimethylvinyl terminated rubber, methyl vinyl silicone rubber (Dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 55 ten thousand and a vinyl molar content of 0.3%, dimethyl raw rubber (Dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 100 ten thousand, silicone powder (KJ-B01, Kanji plastics toughening Material Co., Ltd., Jiande), hydroxy vinyl silicone oil (Stannless all-dimensional chemical Co., Ltd.) having a kinematic viscosity of 155cst (a vinyl content of 6%), hydrogen silicone oil (Stannless all-dimensional chemical Co., Ltd.) having a hydrogen content of 1.50%, and zinc stearate (0.3%) were mixed uniformly in a kneader.
2) In step 1) 25 parts of a mixture having a specific surface area of 150m are added2The silica gel rubber is prepared by uniformly adding four times of silica gel and 10 parts of superfine silica powder (particle size is 1 mu m, manufactured by Fujian Yuanhong chemical Co., Ltd.) in a precipitation method per gram, wherein the silica gel and the superfine silica powder are uniformly added for four times, the adding amounts of the four times of the silica gel and the superfine silica powder are respectively 40%, 25%, 20% and 15% in sequence, after the materials are completely added, stirring and kneading are carried out at normal pressure and 60 ℃, agglomeration is carried out, and after agglomeration, the kneading is continuously carried out for 30min, so that the rubber material is obtained.
3) Heating the rubber material obtained in the step 2) to 100 ℃, carrying out vacuum high-temperature banburying for 1.5h under the vacuum degree of-0.8 MPa to-0.9 MPa, and cooling and standing for 24h to obtain the rubber compound.
4) Uniformly mixing 100 parts of the rubber compound obtained in the step 3) and 0.65 part of peroxide vulcanizing agent bis-di-penta in an open mill, vulcanizing at 175 ℃ for 5 minutes, and then vulcanizing at 200 ℃ for 4 hours to obtain the high-elasticity high-strength silicone rubber composition. The obtained high-elasticity high-strength silicone rubber composition was subjected to a performance test, and the results are shown in table 1.
Example 3
In parts by mass, 50 parts of a dimethylvinyl terminated methyl vinyl silicone rubber (Dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 75 ten thousand and a vinyl molar content of 0.05%, 50 parts of a dimethylvinyl terminated rubber, methyl vinyl silicone rubber (Dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 50 ten thousand and a vinyl molar content of 0.5%, 3 parts of dimethyl raw rubber (Dongjue silicone (Nanjing) Co., Ltd.) having a molecular weight of 100 ten thousand, 4 parts of silicone powder (KJ-B01, Qianji plastics toughening material Co., Ltd., Jiand), 2.5 parts of hydroxy vinyl silicone oil having a kinematic viscosity of 100cst (Stannless all-dimensional chemical Co., Ltd., vinyl content of 6%), 1 part of hydrogen-containing silicone oil having a hydrogen content of 1.53% (Stannless all-dimensional chemical Co., Ltd.), and 0.5 part of calcium stearate were mixed uniformly in a kneader.
2) In step 1) 35 parts of a mixture having a specific surface area of 200m were added2Precipitated silica/g (Fujian Yuanhong chemical Co., Ltd.) and 10 parts of ultrafine silica powder (Guangdong south China sea Xinchuan mining Co., Ltd.)The grain diameter is 1 mu m), wherein the white carbon black and the superfine silicon powder are uniformly added for four times, the adding amounts of the white carbon black and the superfine silicon powder by the four-time gas phase method are respectively 40%, 25%, 20% and 15% in sequence, after the materials are added, the materials are stirred, kneaded and agglomerated at the normal pressure and the temperature of 80 ℃, and then the materials are continuously kneaded for 10min to obtain the rubber material.
3) Heating the rubber material obtained in the step 2) to 120 ℃, carrying out vacuum high-temperature banburying for 1.5h under the vacuum degree of-0.8 MPa to-0.9 MPa, and cooling and standing for 24h to obtain the rubber compound.
4) Mixing 100 parts of the rubber compound obtained in the step 3) and 0.65 part of peroxide vulcanizing agent bis-di-five uniformly in an open mill, vulcanizing at 175 ℃ for 5 minutes, and then vulcanizing at 200 ℃ for 4 hours to obtain the high-elasticity high-strength silicone rubber composition.
The obtained high-elasticity high-strength silicone rubber composition was subjected to a performance test, and the results are shown in table 1.
Performance testing
The silicone rubber compositions prepared in the examples were tested for mechanical properties by the test methods: testing the tensile strength and the elongation at break of the obtained high-elasticity high-strength silicone rubber composition according to the national standard with the standard number GB/T528-2009; the tear strength of the obtained high-elasticity high-strength silicone rubber composition is tested according to the national standard with the standard number GB/T529-2008; testing the Shore hardness of the obtained high-elasticity high-strength silicone rubber composition according to the national standard with the standard number GB/T531.1-2008; the rebound resilience of the obtained high-elasticity high-strength silicone rubber composition is tested according to the national standard with the standard number GB/T1681-2009.
The test results are shown in table 1:
TABLE 1 determination of the Properties of the high-elasticity, high-strength Silicone rubber compositions
| Item | Example 1 | Example 2 | Example 3 |
| Shore hardness (A) | 45 | 52 | 65 |
| Tensile Strength (MPa) | 9.6 | 10 | 9.8 |
| Elongation (%) | 923 | 956 | 946 |
| Tear Strength (kN/m) | 38.9 | 39.2 | 38.2 |
| Rebound resilience (%) | 75 | 72 | 70 |
As shown in Table 1, the invention provides a high-elasticity high-strength silicone rubber composition, which has rebound resilience of more than 70% and tensile strength of 10 MPa.
Claims (9)
1. The high-resilience high-strength silicone rubber is characterized in that: the raw material components comprise the following components in parts by weight:
100 parts of methyl vinyl silicone rubber;
2-10 parts of ultra-high molecular weight dimethyl silicone rubber;
10-40 parts of precipitated white carbon black;
5-30 parts of superfine silicon powder;
3-15 parts of silicone powder;
1-3 parts of hydroxy vinyl silicone oil;
0.1 to 1 portion of hydrogen-containing silicone oil;
0.05 to 1 portion of internal release agent;
0.3-2 parts of vulcanizing agent;
the molecular weight of the ultra-high molecular weight dimethyl silicone rubber is 95-120 ten thousand, the chain link of the ultra-high molecular weight dimethyl silicone rubber does not contain vinyl, and the structural formula is as follows:
wherein the value range of m is 13000-17000.
2. The high-resilience high-strength silicone rubber according to claim 1, wherein: the methyl vinyl silicone rubber is prepared from (5-7) by mass: (5-3) compounding the first methyl vinyl silicone rubber and the second methyl vinyl silicone rubber, wherein the first methyl vinyl silicone rubber contains 0.03-0.09 mol% of vinyl and has a molecular weight of 65-75 ten thousand; the second vinyl silicone rubber has vinyl molar content of 0.25-1.5% and molecular weight of 50-65 ten thousand.
3. The high-resilience high-strength silicone rubber according to claim 1 or 2, wherein: the mass content of siloxane in the silicone powder is 40-60%.
4. The high-resilience high-strength silicone rubber according to claim 1 or 2, wherein: sink with a metal plateThe specific surface area of precipitated white carbon black is not less than 150m2/g。
5. The high-resilience high-strength silicone rubber according to claim 1 or 2, wherein: the particle size of the superfine silicon powder is 0.3-2 μm.
6. The high-resilience high-strength silicone rubber according to claim 1 or 2, wherein: the hydroxyl vinyl silicone oil is hydroxyl-terminated vinyl silicone oil, and has the following structure:
wherein the value range of m is 50-150, the value range of n is 5-20, the viscosity of the hydroxyl vinyl silicone oil is 100-250 cst, and the vinyl content is 3.5-10%.
7. The high-resilience high-strength silicone rubber according to claim 1 or 2, wherein: the hydrogen content in the hydrogen-containing silicone oil is more than 1.5 percent by weight.
8. The high-resilience high-strength silicone rubber according to claim 1 or 2, wherein: the internal mold release agent is stearic acid or stearate, and the stearate is at least one of zinc stearate, magnesium stearate or calcium stearate; the vulcanizing agent is peroxide bis-tetra (2, 4-dichlorobenzoyl peroxide) or bis-penta (2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide).
9. The method for producing a high-resilience high-strength silicone rubber according to any one of claims 1 to 8, wherein: comprises the following steps that:
1) uniformly mixing methyl vinyl silicone rubber, ultra-high molecular weight dimethyl silicone rubber, silicone powder, hydroxyl vinyl silicone oil, hydrogen-containing silicone oil and an internal mold release agent in a kneading machine;
2) adding precipitated white carbon black and superfine silicon powder into the material obtained in the step 1), wherein the precipitated white carbon black and the superfine silicon powder are uniformly added for four times, the four-time adding amounts of the precipitated white carbon black and the superfine silicon powder are respectively 40 +/-3%, 25 +/-3%, 20 +/-3% and 15 +/-3%, stirring and kneading at the temperature of 60-80 ℃ under normal pressure after the feeding is finished, forming into clusters, and continuously kneading for 10-30 min after the clusters are formed;
3) heating the material obtained in the step 2) to 100-120 ℃, banburying for 1.5 +/-0.2 h under the vacuum degree of-0.8 MPa-0.9 MPa, and then cooling and placing for 24 +/-2 h to obtain rubber compound;
4) uniformly mixing the rubber compound obtained in the step 3) with a vulcanizing agent, vulcanizing at 175 +/-5 ℃ for 5 +/-1 min, and then vulcanizing at 200 +/-5 ℃ for 4 +/-1 h to obtain the high-resilience high-strength silicone rubber.
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| CN111825987A (en) * | 2020-06-23 | 2020-10-27 | 凤阳加松新型材料科技有限公司 | High-elasticity mirror silica gel pad and preparation method thereof |
| CN112679958A (en) * | 2020-12-18 | 2021-04-20 | 厦门赛尔特电子有限公司 | Silicon rubber and preparation method thereof, and piezoresistor and preparation method thereof |
| CN113088090A (en) * | 2021-03-08 | 2021-07-09 | 浙江恒业成有机硅有限公司 | High-resilience low-pressure-change silicone rubber material and preparation method thereof |
| CN114479466A (en) * | 2021-12-17 | 2022-05-13 | 江阴市鸿萌橡塑制品有限公司 | High-resilience high-wear-resistance peristaltic pump tube and manufacturing method thereof |
| CN114524964A (en) * | 2021-12-28 | 2022-05-24 | 卢玉华 | Manufacturing process of silica gel slow-resilience sponge |
| CN115521624A (en) * | 2022-09-14 | 2022-12-27 | 安徽东爵有机硅有限公司 | High-resilience high-strength silicone rubber composition and preparation method thereof |
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