CN107964247B - Preparation method of conductive high-temperature vulcanized silicone rubber with excellent mechanical properties - Google Patents
Preparation method of conductive high-temperature vulcanized silicone rubber with excellent mechanical properties Download PDFInfo
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- 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
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- 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
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
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- 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
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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
Abstract
The invention discloses a preparation method of conductive high-temperature vulcanized silicone rubber, which consists of polysiloxane, fumed silica, a carbon nano tube mixture, polydimethylsiloxane, a silane coupling agent, a mold release agent and a vulcanizing agent. The conductive silicone rubber has the characteristics that the novel material carbon nanotube mixture is added, so that the conductive silicone rubber has good conductivity and excellent mechanical properties, and the production process is simple and the operation is convenient.
Description
Technical Field
The invention relates to a preparation method of conductive high-temperature vulcanized silicone rubber with excellent mechanical properties, belonging to the field of silicone rubber materials.
Background
The conductive high-temperature vulcanized silicone rubber is a homogeneous rubber material prepared by mixing raw polyorganosiloxane rubber with high molecular weight, reinforcing filler, a structure control agent, a vulcanizing agent and other additives in a mixing machine. Because of the characteristics of excellent high and low temperature resistance, weather aging resistance, fatigue resistance, insulativity, high air permeability, resistance to certain solvents, physiological inertia and the like, the coating is widely applied to various fields of national economy and people's life, such as aerospace, aviation, electronics, electricity, machinery, automobiles, daily seals, medical sanitation and the like, and also plays an important role in national defense and military industry and high technology industry.
The conductive silicone rubber has good conductivity, and has good electromagnetic sealing and water vapor sealing capabilities, so that the conductive silicone rubber is widely applied to the fields of electronics, electric power, telecommunication, war industry, aviation, aerospace, ships and the like. Most of the conductive silicone rubber sold in the market at present is prepared from acetylene black serving as a raw material, and the defects are that the preparation process is complex for environmental protection and health of operators, the addition amount of the acetylene black in the conventional conductive silicone rubber is large, and the mechanical property of the conductive silicone rubber is poor.
Chinese patent CN 103937258B selects modified multi-wall carbon nano-tubes and conductive carbon black as filling materials, the prepared conductive silicone rubber has low elongation and poor tearing, and the powdered addition mode is not beneficial to environmental protection and body health. The conductive fillers used in patents CN 104327509 a and CN 103665875 are acetylene black or other fillers, and all have the disadvantages of large addition amount of acetylene black, poor mechanical properties of conductive silicone rubber, complex process, and the like. The conductive filler of the invention adopts pre-dispersed single-walled carbon nanotube paste mixture, the dispersibility of the conductive filler in the silicone rubber compound is good, and the conductive performance of the conductive filler is superior to that of multi-walled carbon nanotubes and other conductive carbon black. The conductive silicone rubber uses the single-walled carbon nanotube as the conductive filler, and has the main advantages that the addition amount of the conductive filler is less, and the conductive silicone rubber has excellent mechanical properties, particularly elongation and tear resistance under the condition of the same volume resistivity.
Disclosure of Invention
The invention aims to provide a preparation method of conductive high-temperature vulcanized silicone rubber with excellent mechanical properties, which is prepared by a method of adding carbon nanotubes.
A preparation method of conductive high-temperature vulcanized silicone rubber with excellent mechanical properties comprises the following steps: kneading 100 parts by weight of polysiloxane, 20-70 parts by weight of fumed silica, 1-10 parts by weight of carbon nanotube mixture, 0.5-10 parts by weight of polydimethylsiloxane, 0.05-1 part by weight of silane coupling agent and 0.05-1 part by weight of release agent into homogeneous high-temperature vulcanized conductive silicone rubber material by using a kneader, then performing heat treatment, vacuumizing, cooling the rubber material, adding 0.4-8 parts by weight of curing agent, and uniformly mixing to obtain the product.
The kneading temperature of the kneader is 30-85 ℃, the heat treatment time is 30-60 min, the heat treatment temperature is 90-130 ℃, and the vacuumizing time is 60-90 min.
The polymerization degree of the polyorganosiloxane is 5000 to 20000;
the polyorganosiloxane has at least two silicon-bonded vinyl groups, and has an average composition formula: r2aSiO (4-a)/2, wherein a is a positive number of 1.95-2.05;
wherein R2 may be the same or different and each represents an unsubstituted or substituted monovalent hydrocarbon group, such hydrocarbon groups preferably having 1 to 12 carbon atoms, including alkyl groups, cycloalkyl groups, alkenyl groups, aryl groups, aralkyl groups, groups in which part or all of the hydrogen atoms of the group are substituted with halogen atoms, cyano groups or the like;
wherein alkyl includes ethyl, propyl, butyl, hexyl and octyl; cycloalkyl includes cyclopentyl and cyclohexyl; alkenyl groups include vinyl, allyl, propenyl, and cycloalkenyl; aryl groups include phenyl and tolyl; aralkyl groups include benzyl and 2-phenylethyl; the group formed by substituting a part or all of hydrogen atoms of the group with a halogen atom, a cyano group or the like is a trifluoropropyl group.
The polyorganosiloxane, wherein R2 is preferably a methyl group and a vinyl group, wherein the methyl group is 90 mol%.
The specific surface area of the fumed silica is 120m2/g-300m 2/g.
The carbon nanotube mixture is a mixture of carbon nanotubes and polyorganosiloxane; wherein the ratio of the carbon nanotubes to the polyorganosiloxane is 1: (0.05-0.20).
The polydimethylsiloxane is a polydimethylsiloxane with a molecular chain end being hydroxyl or methoxyl end capping or a hydrogen-containing group, or a polydimethylsiloxane with a molecular chain end being hydroxyl or methoxyl end capping or a hydrogen-containing group and a side group containing phenyl or vinyl or hydroxyl or a hydrogen-containing group, and can be one or a mixture of more than one of the polydimethylsiloxanes.
The silane coupling agent is an organosilicon compound containing two groups with different chemical properties in a molecule, and can be represented by a general formula YSiX3, wherein Y is a non-hydrolytic group and comprises an alkenyl group which is mainly a vinyl group and a hydrocarbon group with Cl, NH2, SH, epoxy, N3, acryloyloxy, methacryloyloxy and isocyanate functional groups at the tail end, namely a carbon functional group; x is a hydrolyzable group including Cl, OMe, OEt, OC2H4OCH3, OSiMe3, and OAc.
The release agent is one or more of higher fatty acid, metal salt of higher fatty acid and ester synthesized by higher fatty acid and alcohol; wherein the higher fatty acid comprises stearic acid, palmitic acid, oleic acid, and lauric acid; metal salts of higher fatty acids including zinc stearate, zinc oleate, calcium oleate; the ester synthesized from higher fatty acid and alcohol comprises ethyl stearate, stearyl stearate, ethyl oleate, and butyl oleate.
The curing agent is one of benzoyl peroxide, 2, 4-dichlorobenzoyl peroxide, p-methylbenzoyl peroxide, o-methylbenzoyl peroxide, dicumyl peroxide, 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and di-tert-butyl peroxide, or a mixture of any combination.
The invention has the advantages that: the conductive high-temperature vulcanized silicone rubber is prepared by adding the single-walled carbon nanotube premix, and has the characteristics of excellent electrical property, stronger tensile strength, elongation at break and tearing strength, simpler production process and convenient operation.
The specific implementation mode is as follows:
example 1
A mixture of 75 parts of a polyorganosiloxane having 90.0mol% of dimethylsiloxane units, 10.0mol% of methylvinylsiloxane units and an average degree of polymerization of 7000 and 25 parts of a polyorganosiloxane having 99.78mol% of dimethylsiloxane units, 0.22mol% of methylvinylsiloxane units and an average degree of polymerization of 7000 was mixed with 30 parts of a polyorganosiloxane having a specific surface area of 230m using a kneader2Fumed silica MS-35 (manufactured by CABOT corporation) in a ratio of 10 parts, a single-walled carbon nanotube mixture in a ratio of 4 parts, polydimethylsiloxane containing hydroxyl groups at each molecular chain end and having a viscosity of 25cSt (25 ℃), and a mold release agent in a ratio of 0.2 part, were mixed at 50 ℃ to form a homogeneous high-temperature vulcanized silicone rubber compound, the heat treatment temperature was 120 ℃, the heat treatment was carried out for 45 minutes, and the mixture was evacuated for 1.5 hours and then cooled.
To 100 parts of the resulting high-temperature vulcanized silicone rubber compound, 1 part of 2, 5-dimethyl-2, 5-di-t-butylperoxyhexane was added and mixed uniformly. The resulting homogeneous mixture was cured at 170 ℃ for 10min to prepare a sheet for property detection, and then secondarily cured at 200 ℃ for 4 h. The physical and mechanical properties and conductivity properties were evaluated, and the results are shown in Table 1.
Example 2
A mixture of 50 parts of a polyorganosiloxane having 99.97mol% of dimethylsiloxane units, 0.03mol% of methylvinylsiloxane units and an average degree of polymerization of 5000 and 50 parts of a polyorganosiloxane having 99.78mol% of dimethylsiloxane units, 0.22mol% of methylvinylsiloxane units and an average degree of polymerization of 5000 was mixed with 20 parts of a polyorganosiloxane having a specific surface area of 120m using a kneader2Fumed silica MS-35 (manufactured by CABOT corporation) of per gram, 1 part of a single-walled carbon nanotube mixture, 0.5 part of polydimethylsiloxane containing hydroxyl groups at each molecular chain end and having a viscosity of 25cSt (25 ℃), 0.05 part of a silane coupling agent and 0.05 part of a mold release agent are mixed to form a homogeneous high-temperature vulcanized silicone rubber compound at a temperature of 30 ℃, the heat treatment temperature is 90 ℃, the heat treatment is carried out for 30 minutes, and the mixture is cooled after being vacuumized for 1 hour.
To 100 parts of the resulting high temperature vulcanized silicone rubber compound, 0.4 part of 2, 5-dimethyl-2, 5-di-t-butylperoxy hexane was added and mixed well. The resulting homogeneous mixture was cured at 170 ℃ for 10min to prepare a sheet for property detection, and then secondarily cured at 200 ℃ for 4 h. The physical and mechanical properties and conductivity properties were evaluated, and the results are shown in Table 1.
Example 3
A mixture of 50 parts of a polyorganosiloxane having 99.96mol% of dimethylsiloxane units, 0.04mol% of methylvinylsiloxane units and an average degree of polymerization of 20000 and 50 parts of a polyorganosiloxane having 99.79mol% of dimethylsiloxane units, 0.21mol% of methylvinylsiloxane units and an average degree of polymerization of 20000 was mixed with 70 parts of a mixture having a specific surface area of 300m2The preparation method comprises the following steps of mixing 10 parts of single-walled carbon nanotube mixture, 10 parts of polydimethylsiloxane containing hydroxyl groups at the tail ends of molecular chains and having the viscosity of 25cSt (25 ℃), 1 part of silane coupling agent and 1 part of release agent into homogeneous high-temperature vulcanized silicone rubber material at 85 ℃, wherein the heat treatment temperature is 130 ℃, the heat treatment is carried out for 60 minutes, and the material is cooled after being vacuumized for 90 minutes.
To 100 parts of the resulting high-temperature vulcanized silicone rubber compound, 8 parts of 2, 5-dimethyl-2, 5-di-t-butylperoxyhexane was added and mixed uniformly. The resulting homogeneous mixture was cured at 170 ℃ for 10min to prepare a sheet for property detection, and then secondarily cured at 200 ℃ for 4 h. The physical and mechanical properties and conductivity properties were evaluated, and the results are shown in Table 1.
Example 4
Sheets for property testing were prepared in the same manner as in example 1 except that 4 parts of the single-walled carbon nanotube mixture was used, and their physical mechanical properties and electrical conductivity properties were evaluated, and the results are shown in table 1.
Example 5
Sheets for property testing were prepared in the same manner as in example 1 except that 1 part of the single-walled carbon nanotube mixture was used, and their physical mechanical properties and electrical conductivity properties were evaluated, and the results are shown in table 1.
Example 6
Sheets for performance testing were prepared in the same manner as in example 1 except that 0.5 parts of the single-walled carbon nanotube mixture was used, and their physical mechanical properties and electrical conductivity properties were evaluated, and the results are shown in table 1.
Example 7
Sheets for property testing were prepared in the same manner as in example 1 except that the single-walled carbon nanotube mixture was not used, and their physical mechanical properties and electrical conductivity properties were evaluated, and the results are shown in table 1.
Example 8
The single-walled carbon nanotube mixture of example 1 was replaced with the same amount of multi-walled carbon nanotubes, and sheets were prepared according to example 1 and evaluated for physical and mechanical properties and electrical conductivity, and the results are shown in Table 1.
Example 9
The single-walled carbon nanotube mixture of example 1 was replaced with acetylene black in the same amount, and sheets were prepared according to example 1, and their physical and mechanical properties and electrical conductivity were evaluated, and the results are shown in table 1.
TABLE 1 results of physical and electrical properties of the electrically conductive silicone rubber prepared in each example
As can be seen from the data results in Table 1, the high-temperature vulcanized conductive silicone rubber prepared by the invention has excellent electrical properties and stronger tensile strength, elongation at break and tear strength.
Claims (8)
1. A preparation method of conductive high-temperature vulcanized silicone rubber with excellent mechanical properties is characterized by comprising the following steps: kneading 100 parts by weight of polysiloxane, 20-70 parts by weight of fumed silica, 1-10 parts by weight of carbon nanotube mixture, 0.5-10 parts by weight of polydimethylsiloxane, 0.05-1 part by weight of silane coupling agent and 0.05-1 part by weight of release agent into homogeneous high-temperature vulcanized conductive silicone rubber material by using a kneader, then performing heat treatment and vacuumizing, cooling the rubber material, adding 0.4-8 parts by weight of curing agent, and uniformly mixing to obtain the conductive silicone rubber material; the carbon nanotube mixture is a pre-dispersed single-walled carbon nanotube paste mixture, namely a mixture of carbon nanotubes and polyorganosiloxane, and the ratio of the carbon nanotubes to the polyorganosiloxane is 1: (0.05-0.20); the kneading temperature of the kneader is 30-85 ℃, the heat treatment time is 30-60 min, the heat treatment temperature is 90-130 ℃, and the vacuumizing time is 60-90 min.
2. The method of claim 1 for preparing an electrically conductive high temperature vulcanized silicone rubber with excellent mechanical properties, wherein: the polymerization degree of the polyorganosiloxane is 5000 to 20000; the polyorganosiloxane has at least two silicon-bonded vinyl groups, and has an average composition formula: r2aSiO(4-a)/2Wherein a is a positive number from 1.95 to 2.05; wherein R2 may be the same or different and each represents an unsubstituted or substituted monovalent hydrocarbon group having 1 to 12 carbon atoms, including an alkyl group, a cycloalkyl group, an alkenyl group, an aryl group, an aralkyl group, a group in which part or all of the hydrogen atoms of the group are substituted with a halogen atom or a cyano group; wherein alkyl includes ethyl, propyl, butyl, hexyl and octyl; cycloalkyl includes cyclopentyl and cyclohexyl; alkenyl groups include vinyl, allyl, propenyl, and cycloalkenyl; aryl groups include phenyl and tolueneA group; aralkyl groups include benzyl and 2-phenylethyl; a group in which a part or all of hydrogen atoms of the group are substituted with a halogen atom or a cyano group.
3. The method for preparing an electrically conductive high temperature vulcanized silicone rubber with excellent mechanical properties according to claim 2, wherein: the polyorganosiloxane, wherein R2 is methyl and vinyl, wherein the methyl is 90 mol%.
4. The method of claim 1 for preparing an electrically conductive high temperature vulcanized silicone rubber with excellent mechanical properties, wherein: the specific surface area of the fumed silica is 120m2/g-300m2/g。
5. The method of claim 1 for preparing an electrically conductive high temperature vulcanized silicone rubber with excellent mechanical properties, wherein: the polydimethylsiloxane is one or a mixture of more of polydimethylsiloxane with the molecular chain end being hydroxyl or methoxyl end-capping or hydrogen-containing group.
6. The method of claim 1 for preparing an electrically conductive high temperature vulcanized silicone rubber with excellent mechanical properties, wherein: the silane coupling agent is an organosilicon compound containing two groups with different chemical properties in a molecule, and can be represented by a general formula YSiX3Wherein Y is a non-hydrolyzable group including alkenyl; the alkenyl group is vinyl and has Cl and NH at the terminal 2SH, epoxy, N 3 Acryloxy, methacryloxy, hydrocarbyl of isocyanate functional groups, i.e. carbon functional groups; x is a hydrolyzable group, including Cl, OMe, OEt, OC2H4OCH3, OSiMe3And OAc.
7. The method of claim 1 for preparing an electrically conductive high temperature vulcanized silicone rubber with excellent mechanical properties, wherein: the release agent is one or more of higher fatty acid, metal salt of higher fatty acid and ester synthesized by higher fatty acid and alcohol; wherein the higher fatty acid comprises stearic acid, palmitic acid, oleic acid, and lauric acid; metal salts of higher fatty acids including zinc stearate, zinc oleate, calcium oleate; the ester synthesized from higher fatty acid and alcohol comprises ethyl stearate, stearyl stearate, ethyl oleate, and butyl oleate.
8. The method of claim 1 for preparing an electrically conductive high temperature vulcanized silicone rubber with excellent mechanical properties, wherein: the curing agent is one or a mixture of any combination of benzoyl peroxide, 2, 4-dichlorobenzoyl peroxide, p-methylbenzoyl peroxide, o-methylbenzoyl peroxide, dicumyl peroxide, 2, 5-dimethyl-2, 5-di-tert-butyl-hexane peroxide and di-tert-butyl peroxide.
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| CN110791103B (en) * | 2018-08-01 | 2022-09-06 | 江西蓝星星火有机硅有限公司 | Novel conductive liquid silicone rubber and preparation method and application thereof |
| WO2020025025A1 (en) | 2018-08-01 | 2020-02-06 | 江西蓝星星火有机硅有限公司 | Conductive liquid silicone rubber and preparation method and use thereof |
| WO2020061988A1 (en) * | 2018-09-28 | 2020-04-02 | Dow Silicones Corporation | Liquid silicone rubber composition |
| CN109486193B (en) * | 2018-09-29 | 2021-10-01 | 航天材料及工艺研究所 | Extrusion type silicone rubber system and preparation method and application thereof |
| CN109385094A (en) * | 2018-10-29 | 2019-02-26 | 镇江亿维硅材料科技有限公司 | A kind of silicon rubber conducting masterbatch and its preparation method and application |
| EP4101897A4 (en) * | 2020-02-07 | 2024-03-06 | Zeon Corp | Rubber composition and electrode |
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| CN104327512A (en) * | 2014-08-18 | 2015-02-04 | 杭州师范大学 | Preparation method of silicone rubber composite material containing carbon nanotubes |
| CN105400209A (en) * | 2015-12-18 | 2016-03-16 | 江西蓝星星火有机硅有限公司 | Preparation method for high-temperature vulcanized silicone rubber enhanced by precipitation-process white carbon black for extrusion molding |
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| CN104327512A (en) * | 2014-08-18 | 2015-02-04 | 杭州师范大学 | Preparation method of silicone rubber composite material containing carbon nanotubes |
| CN105400209A (en) * | 2015-12-18 | 2016-03-16 | 江西蓝星星火有机硅有限公司 | Preparation method for high-temperature vulcanized silicone rubber enhanced by precipitation-process white carbon black for extrusion molding |
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