CN108659545B - Silicone rubber composite material and preparation method thereof - Google Patents
Silicone rubber composite material and preparation method thereof Download PDFInfo
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- CN108659545B CN108659545B CN201710212969.9A CN201710212969A CN108659545B CN 108659545 B CN108659545 B CN 108659545B CN 201710212969 A CN201710212969 A CN 201710212969A CN 108659545 B CN108659545 B CN 108659545B
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- isooctanoate
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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
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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
- 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
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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
- 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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- 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
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Abstract
The invention provides a silicone rubber composite material and a preparation method thereof, wherein the silicone rubber composite material comprises the following components in parts by mass: 100 parts of silicon rubber; 1-10 parts of silane modified polyisobutylene; 10-100 parts of white carbon black; 1-10 parts of silazane; 1-10 parts of phenyl silicone oil; 1-10 parts of isooctoate; 0.5-2.0 parts of vulcanizing agent; discloses a preparation method of a silicone rubber composite material, and the prepared silicone rubber has excellent mechanical properties.
Description
Technical Field
The invention relates to rubber, in particular to a silicone rubber composite material and a preparation method thereof.
Background
The silicon rubber has excellent high and low temperature resistance, weather resistance, electric insulation and the like, and is widely applied to the fields of machinery, electronic and electric appliances, chemical industry, aerospace and the like.
Ordinary silicone rubber has various excellent properties, but has poor mechanical properties. Particularly, the tearing strength of the silicon rubber is lower in the tearing resistance and can only reach 5-10kN/m, and the product is easy to tear when used in a harsher environment, so that the service performance of the product is influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the silicone rubber which has the advantages of simple process, low production cost, higher tensile strength, elongation at break and tearing strength and the preparation method thereof.
In order to achieve the above object, the present invention provides a silicone rubber composite material comprising, in mass fraction:
wherein, the silicon rubber is methyl vinyl silicon rubber, the vinyl content is 0.07 percent to 1.2 percent, and the molecular weight range is 45 to 70 ten thousand;
the silane modified polyisobutylene is a reactant of vinyl methyl dimethoxysilane and isobutylene homopolymer and copolymer, an end group and/or a side group contain an alkoxy silicon group, and the viscosity is 800000-1200000 cSt;
wherein the white carbon black is non-treatment white carbon black, the specific surface area is 100m 2/g-300 m2/g, the PH value is 3.7-4.3, and the density is 5lbs/ft 2;
the silazane is one or more of hexamethyldisilazane, hexamethylcyclotrisilazane and hexaphenylcyclotrisilazane;
wherein the hydroxyl silicone oil is one or more of vinyl methyl phenyl hydroxyl silicone oil, methyl hydroxyl silicone oil and methyl phenyl hydroxyl silicone oil, and the content of hydroxyl is 3-10%;
wherein the iso-octoate is one or more of manganese iso-octoate, zinc iso-octoate, cerium iso-octoate, zirconium iso-octoate, lead iso-octoate, cobalt iso-octoate, calcium iso-octoate, potassium iso-octoate, nickel iso-octoate, copper iso-octoate and vanadium iso-octoate.
Wherein, the vulcanizing agent is a peroxide vulcanizing agent, and the peroxide is one or a mixture of two of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, 2, 4-dichlorobenzoyl peroxide, dicumyl peroxide, benzoyl peroxide, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane and 1, 3-bis (tert-butylperoxyisopropyl) benzene;
the invention also relates to a preparation method of the silicon rubber composite material, which comprises the following steps:
(1) banburying silane modified polyisobutylene and white carbon black in a close-mixing machine to obtain a silane modified polyisobutylene white carbon black mixture, wherein the mixing density is controlled to be 30-60 ℃; (ii) a
(2) Mixing silicon rubber, white carbon black, silazane, hydroxyl silicone oil and isooctoate in an internal mixer to obtain a silicon rubber mixture, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(3) mixing the silane modified polyisobutylene white carbon black mixture and the silicon rubber mixture in an internal mixer to obtain silicon rubber silane modified polyisobutylene rubber compound, wherein the mixing temperature of the internal mixer is controlled at 30-60 DEG C
(4) Standing the silicone rubber silane modified polyisobutylene rubber compound for 24 hours;
(5) the parked silicone rubber silane modified polyisobutylene rubber compound is milled on an open mill to a wrapping roller, and 0.5 to 2.0 parts of vulcanizing agent is added and mixed to be uniform;
(6) vulcanizing the rubber compound added with the vulcanizing agent on a flat vulcanizing machine, wherein the vulcanizing temperature is controlled at 130 ℃ and 170 ℃, and the pressure is controlled at 5-10 MPa;
(7) and (3) carrying out secondary vulcanization on the vulcanized silicone rubber in an oven, wherein the secondary vulcanization temperature is controlled at 200 ℃ and the time is 4 h.
The invention has the following excellent effects: the process is simple and the production cost is low; the vulcanized rubber has excellent mechanical properties, the tensile strength can reach 13MPa, the elongation at break can reach about 800%, and the tear strength can reach 55 KN/m.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples, which are not intended to limit the scope of the present invention.
Example 1
The formula comprises the following components in parts by mass:
the preparation method comprises the following steps:
(1) banburying 1 part of silane modified polyisobutylene and 2 parts of white carbon black in a close-mixing machine to obtain a silane modified polyisobutylene white carbon black mixture, wherein the mixing density is controlled to be 30-60 ℃; (ii) a
(2) Mixing 100 parts of silicon rubber, 8 parts of white carbon black, 1 part of hexamethyldisilazane, 1 part of phenyl hydroxyl silicone oil and 1 part of cerium isooctanoate in an internal mixer to obtain a silicon rubber mixture, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(3) mixing the silane modified polyisobutylene white carbon black mixture and the silicon rubber mixture in an internal mixer to obtain silicon rubber silane modified polyisobutylene rubber compound, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(4) standing the silicone rubber silane modified polyisobutylene rubber compound for 24 hours;
(5) the parked silicone rubber silane modified polyisobutylene rubber compound is milled on a mill until a roll is wrapped, 0.5 part of 2, 5-dimethyl-2, 5-bis (tert-butyl peroxy) hexane vulcanizing agent is added and mixed evenly;
(6) vulcanizing the rubber compound added with the vulcanizing agent on a flat vulcanizing machine, wherein the vulcanizing temperature is controlled at 170 ℃, and the pressure is controlled at 8 MPa;
(7) and (3) carrying out secondary vulcanization on the vulcanized silicone rubber in an oven, wherein the secondary vulcanization temperature is controlled at 200 ℃ and the time is 4 h. And cooling the obtained high-temperature vulcanized rubber sheet.
Example 2
The formula comprises the following components in parts by mass:
the preparation method comprises the following steps:
(1) banburying 10 parts of silane modified polyisobutylene and 20 parts of white carbon black in a close-mixing machine to obtain a silane modified polyisobutylene white carbon black mixture, wherein the mixing density is controlled to be 30-60 ℃; (ii) a
(2) Mixing 100 parts of silicon rubber, 80 parts of white carbon black, 10 parts of hexamethylcyclotrisilazane, 5 parts of vinyl methyl phenyl hydroxy silicone oil, 5 parts of methyl hydroxy silicone oil, 5 parts of cerium isooctanoate and 5 parts of calcium isooctanoate in an internal mixer to obtain a silicon rubber mixture, wherein the mixing temperature of the internal mixer is controlled to be 30-60 ℃;
(3) mixing the silane modified polyisobutylene white carbon black mixture and the silicon rubber mixture in an internal mixer to obtain silicon rubber silane modified polyisobutylene rubber compound, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(4) standing the silicone rubber silane modified polyisobutylene rubber compound for 24 hours;
(5) the parked silicone rubber silane modified polyisobutylene rubber compound is milled on a mill until a roll is wrapped, 1 part of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane and 1 part of 2, 4-dichlorobenzoyl peroxide vulcanizing agent are added, and the mixture is milled uniformly;
(6) vulcanizing the rubber compound added with the vulcanizing agent on a flat vulcanizing machine, wherein the vulcanizing temperature is controlled at 130 ℃, and the pressure is controlled at 10 MPa;
(7) and (3) carrying out secondary vulcanization on the vulcanized silicone rubber in an oven, wherein the secondary vulcanization temperature is controlled at 200 ℃ and the time is 4 h. And cooling the obtained high-temperature vulcanized rubber sheet.
Example 3
The formula comprises the following components in parts by mass:
the preparation method comprises the following steps:
(1) banburying 5 parts of silane modified polyisobutylene and 10 parts of white carbon black in a close-mixing machine to obtain a silane modified polyisobutylene white carbon black mixture, wherein the mixing density is controlled to be 30-60 ℃; (ii) a
(2) Mixing 100 parts of silicon rubber, 40 parts of white carbon black, 5 parts of hexaphenylcyclotrisilazane, 5 parts of methylphenyl hydroxy silicone oil, 2 parts of manganese isooctoate and 5 parts of nickel isooctoate in an internal mixer to obtain a silicon rubber mixture, wherein the mixing temperature of the internal mixer is controlled to be 30-60 ℃;
(3) mixing the silane modified polyisobutylene white carbon black mixture and the silicon rubber mixture in an internal mixer to obtain silicon rubber silane modified polyisobutylene rubber compound, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(4) standing the silicone rubber silane modified polyisobutylene rubber compound for 24 hours;
(5) the parked silicone rubber silane modified polyisobutylene rubber compound is milled on an open mill to a wrapping roller, 0.4 part of 1, 1-di-tert-butyl peroxy-3, 3, 5-trimethylcyclohexane and 0.6 part of 1, 3-bis (tert-butyl peroxy isopropyl) benzene are added, and the mixture is milled uniformly;
(6) vulcanizing the rubber compound added with the vulcanizing agent on a flat vulcanizing machine, wherein the vulcanizing temperature is controlled at 150 ℃, and the pressure is controlled at 9 MPa;
(7) and (3) carrying out secondary vulcanization on the vulcanized silicone rubber in an oven, wherein the secondary vulcanization temperature is controlled at 200 ℃ and the time is 4 h. And cooling the obtained high-temperature vulcanized rubber sheet.
Example 4
The formula comprises the following components in parts by mass:
the preparation method comprises the following steps:
(1) banburying 8.79 parts of silane modified polyisobutylene and 20 parts of white carbon black in a close-mixing machine to obtain a silane modified polyisobutylene white carbon black mixture, wherein the mixing density is controlled to be 30-60 ℃; (ii) a
(2) Mixing 100 parts of silicon rubber, 50 parts of white carbon black, 3 parts of hexamethyldisilazane, 3 parts of hexamethylcyclotrisilazane, 3 parts of phenyl hydroxyl silicone oil, 4 parts of methyl phenyl hydroxyl silicone oil, 2 parts of zinc isooctanoate and 4 parts of vanadium isooctanoate in an internal mixer to obtain a silicon rubber mixture, wherein the mixing temperature of the internal mixer is controlled to be 30-60 ℃;
(3) mixing the silane modified polyisobutylene white carbon black mixture and the silicon rubber mixture in an internal mixer to obtain silicon rubber silane modified polyisobutylene rubber compound, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(4) standing the silicone rubber silane modified polyisobutylene rubber compound for 24 hours;
(5) the parked silicone rubber silane modified polyisobutylene rubber compound is milled on an open mill to a wrapping roller, 0.8 part of dicumyl peroxide and 0.4 part of benzoyl peroxide are added, and the mixture is milled uniformly;
(6) vulcanizing the rubber compound added with the vulcanizing agent on a flat vulcanizing machine, wherein the vulcanizing temperature is controlled at 140 ℃, and the pressure is controlled at 10 MPa;
(7) and (3) carrying out secondary vulcanization on the vulcanized silicone rubber in an oven, wherein the secondary vulcanization temperature is controlled at 200 ℃ and the time is 4 h. And cooling the obtained high-temperature vulcanized rubber sheet.
The mechanical properties of the vulcanizates obtained in examples 1 to 4 were measured and the results are shown in Table 1:
TABLE 1 mechanical Property test results
| Tensile strength/MPa | Elongation at break/% | Tear Strength/KN/m | |
| Example 1 | 11 | 800 | 40 |
| Example 2 | 12.7 | 700 | 48 |
| Example 3 | 13 | 780 | 45 |
| Example 4 | 12.5 | 800 | 55 |
The present invention is not limited to the above-described embodiments, and various changes may be made by those skilled in the art, which changes are equivalent or similar to the present invention and are intended to be included within the scope of the appended claims.
Claims (6)
1. A silicone rubber composite characterized by: the formula comprises the following components in parts by mass:
the silicon rubber is methyl vinyl silicon rubber, the vinyl content is 0.07-1.2%, and the molecular weight range is 45-70 ten thousand; the silane modified polyisobutylene is a reactant of vinyl methyl dimethoxysilane and isobutylene homopolymer and copolymer, an end group and/or a side group contain an alkoxy silicon group, and the viscosity is 800000-1200000 cSt;
the preparation method of the silicone rubber composite material comprises the following steps:
(1) banburying silane modified polyisobutylene and white carbon black in a close-mixing machine to obtain a silane modified polyisobutylene white carbon black mixture, wherein the mixing density is controlled to be 30-60 ℃;
(2) mixing silicon rubber, white carbon black, silazane, hydroxyl silicone oil and isooctoate in an internal mixer to obtain a silicon rubber mixture, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(3) mixing the silane modified polyisobutylene white carbon black mixture and the silicon rubber mixture in an internal mixer to obtain silicon rubber silane modified polyisobutylene rubber compound, wherein the mixing temperature of the internal mixer is controlled at 30-60 ℃;
(4) standing the silicone rubber silane modified polyisobutylene rubber compound for 24 hours;
(5) the parked silicone rubber silane modified polyisobutylene rubber compound is milled on an open mill to a wrapping roller, and 0.5 to 2.0 parts of vulcanizing agent is added and mixed to be uniform;
(6) vulcanizing the rubber compound added with the vulcanizing agent on a flat vulcanizing machine, wherein the vulcanizing temperature is controlled at 130 ℃ and 170 ℃, and the pressure is controlled at 5-10 MPa;
(7) and (3) carrying out secondary vulcanization on the vulcanized silicone rubber in an oven, wherein the secondary vulcanization temperature is controlled at 200 ℃ for 4 hours, and obtaining the vulcanized rubber.
2. The silicone rubber composite material according to claim 1, wherein: the white carbon black is non-processed white carbon black with the specific surface area of 100m2/g～300m2(iv) g, pH 3.7-4.3, density 5lbs/ft2。
3. The silicone rubber composite material according to claim 1, wherein: the silazane is one or more of hexamethyldisilazane, hexamethylcyclotrisilazane and hexaphenylcyclotrisilazane.
4. The silicone rubber composite material according to claim 1, wherein: the hydroxyl silicone oil is one or more of vinyl methyl phenyl hydroxyl silicone oil, methyl hydroxyl silicone oil and methyl phenyl hydroxyl silicone oil, and the content of hydroxyl is 3-10%.
5. The silicone rubber composite material according to claim 1, wherein: the isooctoate is one or a mixture of manganese isooctanoate, zinc isooctanoate, cerium isooctanoate, zirconium isooctanoate, lead isooctanoate, cobalt isooctanoate, calcium isooctanoate, potassium isooctanoate, nickel isooctanoate, copper isooctanoate and vanadium isooctanoate.
6. The silicone rubber composite material according to claim 1, wherein: the vulcanizing agent is a peroxide vulcanizing agent, and the peroxide is one or a mixture of two of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, 2, 4-dichlorobenzoyl peroxide, dicumyl peroxide, benzoyl peroxide, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane and 1, 3-bis (tert-butylperoxyisopropyl) benzene.
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| CN109370234A (en) * | 2018-10-26 | 2019-02-22 | 常州大学怀德学院 | A kind of bubble-tight transparent silica gel of baking-curing and preparation method thereof |
| CN109679353A (en) * | 2019-01-21 | 2019-04-26 | 广德鸣生新材料有限公司 | A kind of ice machine silicon rubber connector and preparation method thereof |
| CN112011186A (en) * | 2020-09-04 | 2020-12-01 | 陕西省石油化工研究设计院 | Efficient mould-resistant silicon rubber material and preparation method thereof |
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| JP2002047419A (en) * | 2000-08-02 | 2002-02-12 | Ge Toshiba Silicones Co Ltd | Composition for silicone rubber sheet |
| US6750279B1 (en) * | 2000-08-11 | 2004-06-15 | General Electric Company | High tear strength low compression set heat curable silicone elastomer and additive |
| CN104004360A (en) * | 2014-05-07 | 2014-08-27 | 天长市荣盛有机硅科技有限公司 | High-strength tear-resistant methyl vinyl silicone rubber material |
| CN104559202A (en) * | 2015-01-21 | 2015-04-29 | 宜昌兴之新塑胶电子科技有限公司 | Preparation method of high-tear-resistance silicon compounded rubber |
| CN105482466A (en) * | 2015-12-24 | 2016-04-13 | 佛山市华联有机硅有限公司 | Low-hardness high-strength silicon rubber and preparation method thereof |
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