CN109021583A - Three component tear-proof silicon rubber of one kind and preparation method - Google Patents
Three component tear-proof silicon rubber of one kind and preparation method Download PDFInfo
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- CN109021583A CN109021583A CN201810926089.2A CN201810926089A CN109021583A CN 109021583 A CN109021583 A CN 109021583A CN 201810926089 A CN201810926089 A CN 201810926089A CN 109021583 A CN109021583 A CN 109021583A
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- silicon rubber
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/06—Polyurethanes from polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/08—Polyurethanes from polyethers
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/08—Crosslinking by silane
Abstract
The present invention relates to a kind of anti-tear split silicone of three components and preparation methods.Three component specifically includes that silicon rubber, polyurethane and ethylene-vinyl acetate copolymer.Preparation method includes: that silicon rubber, ethylene-vinyl acetate copolymer, crosslinking agent, radical initiator are kneaded 5-10 minutes by (1) at 150 DEG C -200 DEG C, obtains silicon rubber and is kneaded glue 1；(2) above-mentioned silicon rubber is kneaded glue 1 and filler, polyurethane under the conditions of 30-50 DEG C, be kneaded 10-20 minutes, obtained silicon rubber and be kneaded glue 2；(3) dynamic vulcanization: silicon rubber is kneaded glue 2 and vulcanizing agent is placed in double screw extruder, is arranged 130-170 DEG C of extruder temperature, dynamic vulcanization obtains three component tear-proof silicon rubber under revolving speed 200-600rpm.The three components tear-proof silicon rubber, has excellent mechanical performance, and tear resistance is especially prominent.
Description
Technical field
The present invention relates to a kind of three component tear-proof silicon rubber and preparation methods, belong to technical field of polymer materials.
Background technique
Silicon rubber is one of most important product in organosilicon material.Silicon rubber is mainly by linear polysiloxanes (or base
Glue, raw rubber), reinforced filling, crosslinking agent, catalyst and other additives composition.All components mixing uniformly can be processed into mixed
Refining glue, rubber compound is crosslinked under certain condition (or vulcanization, solidification), is just transformed into elasticity by initial high viscous plastic state
State has the vulcanizate of three-dimensional netted cross-linked structure to get arriving.
It is well known that silicon rubber has many unique and excellent performance, as heat resistance, cold resistance, resistance to ag(e)ing are (resistance to smelly
Oxygen aging, heat oxygen aging resistance, light aging resisting and weather-resistant etc.), electric insulating quality and special surface property etc..Exactly
As silicon rubber have General Purpose Rubber not available for excellent properties, successfully synthesized as a kind of special synthetic rubber from 1945
Since, development at full speed is all obtained in basic research and application field, in aerospace, traffic, automobile, chemical industry, electronics electricity
The national economy such as gas, building, medical treatment field is widely used, and becomes a kind of irreplaceable advanced material.However,
Compared with most of General Purpose Rubber, the physical mechanical property of silicon rubber general at present is poor, and intensity is lower, this is to a certain degree
On limit the application range of silicon rubber.So how effectively to improve the physical mechanical property of silicon rubber, can satisfy
The silicon rubber of application request is always an important subject in silicone rubber art.
Patent CN107868477 discloses a kind of dual-component polyurethane modified liquid silicon rubber and preparation method thereof, described
Dual-component polyurethane modified liquid silicon rubber includes component A and B component, and the component A is by amido silicon oil and filler according to certain
Ratio is prepared, and the B component is prepared according to a certain percentage by urethane oligomer, catalyst, the polyurethane
Oligomer is to be obtained by polyalcohol, prepolymerization catalyst and isocyanates by polymerization reaction, in use, the component A and institute
B component is stated to mix according to a certain percentage.Although dual-component polyurethane modified liquid silicon rubber is due to polyurethane made from the method
Presence, increase the mechanical performance of silicon rubber, but the two is that two kinds of high polymers lean on merely that end group is crosslinked or physical entanglement is handed over
Connection, crosslink density is lower, and mechanical performance is mutually chemically crosslinked solid netted relative to three components by cross-linking agents
Structured product is poor.
Patent CN105924972A discloses a kind of silicon rubber/polyurethane thermoplastic vulcanizate and preparation method thereof, specifically
The preparation method is as follows: 1. draw methyl vinyl silicone rubber, ethylene vinyl acetate copolymer or maleic anhydride, free radical
It sends out agent melting mixing at 150-200 DEG C to react 3-20 minutes, obtains the silicon rubber of graft modification；2. silicon rubber and filler are existed
Under room temperature, it is sufficiently mixed uniformly, obtains silicon rubber and be kneaded glue.3. rubber premixes: the grafting that polyurethane and step 1 are obtained
Modified silicon rubber mixes at 160-200 DEG C, and the silicon rubber gross rubber and antioxidant of step 2 is then added, to be mixed equal
It is cooled to room temperature after even；Then it is uniformly mixed to obtain rubber and plastic pre-composition with vulcanizing agent and polymerization inhibitor at room temperature again；4. dynamic sulphur
Change: the obtained rubber and plastic pre-composition of step 3 is placed in double screw extruder, be arranged 170-200 DEG C of extruder temperature, revolving speed is
300-700rpm, dynamic vulcanization obtain silicon rubber/polyurethane thermoplastic vulcanizate.This method is improved by homemade solubilizer
The problem of silicon rubber and polyurethane poor compatibility, but its obtained silicon rubber/polyurethane thermoplastic vulcanizate is simple silicon
The physical blending of rubber and polyurethane, mechanical performance are mutually chemically crosslinked the rubber compound for forming space network compared with three components
It is poor.
Summary of the invention
The object of the present invention is to provide a kind of anti-tear split silicone of three components and preparation methods.Using cumyl peroxide or
One of dibenzoyl peroxide or it is a variety of be used as radical initiator, by silicon rubber, ethylene-vinyl acetate polymer,
Vinyltriacetoxy silane carries out chemical bond by free radical polymerization and is connected, then passes through vinyltriacetoxy silane
Active group and polyurethane carry out chemical reaction crosslinking, so that obtaining each macromolecule all passes through three components that chemical bond is cross-linked with each other
Anti-tear split silicone, mechanical performance caused by solving the problems, such as physical crosslinking or the degree of cross linking not enough are poor.Three groups be prepared
Point anti-tear split silicone has brilliant tear resistance, can be widely applied to sky space flight, traffic, automobile, chemical industry, it is electric,
The fields such as building, medical treatment.
The present invention provides a kind of three component tear-proof silicon rubber, it is characterised in that: has silicon rubber, polyurethane, ethyl vinyl acetate
Vinyl ester copolymers, filler, radical initiator, vulcanizing agent, crosslinking agent composition, the composition of the three components tear-proof silicon rubber are pressed
Mass parts ratio is as shown in the table.
The silicon rubber is one of methyl vinyl silicone rubber, methyl vinyl phenyl silicon rubber or a variety of.
The polyurethane is polyester polyurethane or polyether polyurethane.
The vinyl acetate content of the ethylene-vinyl acetate copolymer is 28%-70%.
The filler are as follows: carboxy-modified carbon nanotube, silane-modified white carbon black, gas-phase silica, precipitated silica or
One of activated Calcium carbonate is a variety of.
The radical initiator are as follows: one of cumyl peroxide or dibenzoyl peroxide are a variety of.
The vulcanizing agent are as follows: bis- (tert-butyl peroxide) hexanes of cumyl peroxide, 2,5- dimethyl -2,5- or 2,5-
Dimethyl -2,5- bis- (tert-butyl peroxides) one of alkynes or a variety of.
The crosslinking agent are as follows: vinyltriacetoxy silane.
The present invention also provides the preparation method of above-mentioned three components tear-proof silicon rubber, specific steps are as follows:
(1) silicon rubber, ethylene-vinyl acetate copolymer, crosslinking agent, radical initiator are kneaded at 150 DEG C -200 DEG C
It 5-10 minutes, obtains silicon rubber and is kneaded glue 1；
(2) above-mentioned silicon rubber is kneaded glue 1 and filler, polyurethane under the conditions of 30-50 DEG C, is kneaded 10-20 minutes, obtains silicon rubber
Glue is kneaded glue 2；
(3) dynamic vulcanization: silicon rubber is kneaded glue 2 and vulcanizing agent is placed in double screw extruder, extruder temperature 130-170 is set
DEG C, revolving speed 200-600rpm, dynamic vulcanization obtains three component tear-proof silicon rubber.
The invention has the advantages that freely using one of cumyl peroxide or dibenzoyl peroxide or a variety of conducts
Base initiator, by silicon rubber, ethylene-vinyl acetate polymer, vinyltriacetoxy silane by free radical polymerization into
Row chemical bond is connected, then carries out chemical reaction with polyurethane by the active group of vinyltriacetoxy silane and be crosslinked, from
And obtain each macromolecule and all pass through the anti-tear split silicone of three components that chemical bond is cross-linked with each other, solve physical crosslinking mechanical performance compared with
The problem of difference.
Specific embodiment:
The present invention is specifically described and is further illustrated below by embodiment, is not to be construed as limiting model of the invention
It encloses.The person skilled in the art in the field can make some non-intrinsically safe modifications and adaptations according to the content of aforementioned present invention.
Testing standard used by embodiment:
Tearing strength GB/T529-2008 room temperature electron puller system rate of extension: 500mm/min.
Embodiment 1-5 is shown in steps are as follows:
(1) Brabender is heated to 175 DEG C from note vulcameter temperature, by silicon rubber, the ethyl vinyl acetate in formula listed by table 1
Vinyl ester copolymers, crosslinking agent, radical initiator are added to Brabender from note vulcameter, are kneaded 7.5 minutes；
(2) by the resulting rubber compound of step (1), filler, polyurethane on double Kun kneading machines, be kneaded temperature be 40 DEG C under the conditions of
It is kneaded 15 minutes；
(3) dynamic vulcanization: rubber compound obtained by step (2) and vulcanizing agent are placed in double screw extruder, and extruder temperature 150 is arranged
DEG C, under revolving speed 400rpm, dynamic vulcanization obtains three component tear-proof silicon rubber.
Three component tear-proof silicon rubber tear strength properties are listed in table 3.
Comparative example 1 is prepared according to embodiment 1-5 preparation process, but does not add crosslinking agent；Comparative example 2 is according to embodiment 1-
5 preparation processes preparation, but do not add radical initiator and vulcanizing agent.The tearing strength of Comparative Examples 1 and 2 is listed in table 3.
The preparation formula of embodiment 6-9 and comparative example 3,4 is according to the preparation formula of embodiment 1, and preparation process is according to implementation
Example 1-5 preparation process preparation, corresponding preparation condition are changed to condition shown in table 2.The tearing of embodiment 6-9 and comparative example 3,4 is strong
Degree is listed in table 3.
In the comparison of above-mentioned table 1, for comparative example 1,2 compared with embodiment 1-5, comparative example 1 does not add crosslinking agent, although
Silicon rubber and ethylene-vinyl acetate copolymer form copolymer by free radical polymerization in sulfidation, but do not have
It is formed and is chemically crosslinked with polyurethane, from without being formed between silicon rubber, ethylene-vinyl acetate copolymer and polyurethane mutually
The structure of chemical crosslinking, therefore by table 3 it is found that the tearing strength of comparative example 1 only has 40.4 KN/m, comparative example 2 is not added certainly
By base initiator and vulcanizing agent, silicon rubber, ethylene-vinyl acetate copolymer and crosslinking agent are not over certainly in vulcanization engineering
It is polymerize by base and forms chemical crosslinking, so that each component and polyurethane can not also generate chemical crosslinking, each component is simple object
Reason crosslinking, so its tearing strength only has 27.0KN/m.
Above-mentioned table 2 comparison in, comparative example 3,4 compared with embodiment 1,6-9,3 step of comparative example (1) be kneaded temperature compared with
Low, the time is shorter, affect silicon rubber in first step sulfidation, ethylene-vinyl acetate copolymer and crosslinking agent from
By base polymerization reaction, but step (3) has reinforcing effect to step (1), thus pass through table 3 it is found that the tearing strength of comparative example 3 still
46.9 KN/m are so reached；4 dynamic vulcanization temperature of comparative example is lower, revolving speed is slower, affects silicon rubber, ethene-vinyl acetate
The cross-linking reaction of ester copolymer and polyurethane, therefore by table 3 it is found that the tearing strength of comparative example 4 only has 37.8 KN/m.
By table 3 it is found that the tearing strength of embodiment 1-9 has all reached 50 KN/m or more, therefore three groups that the present invention obtains
Divide tear-proof silicon rubber that there is stronger tear resistance.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of specification record.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (9)
1. a kind of three component tear-proof silicon rubber, it is characterised in that: be copolymerized by silicon rubber, polyurethane, ethylene-vinyl acetate
Object, filler, radical initiator, vulcanizing agent, crosslinking agent composition, the composition of the three components tear-proof silicon rubber press mass parts ratio
As shown in the table.
2. three components tear-proof silicon rubber according to claim 1, it is characterised in that: the silicon rubber is ethylene methacrylic
One of base silicon rubber, methyl vinyl phenyl silicon rubber are a variety of.
3. three components tear-proof silicon rubber according to claim 1, it is characterised in that: the polyurethane is the poly- ammonia of polyester-type
Ester or polyether polyurethane.
4. three components tear-proof silicon rubber according to claim 1, it is characterised in that: the ethylene-vinyl acetate is total
The vinyl acetate content of polymers is 28%-70%.
5. three components tear-proof silicon rubber according to claim 1, it is characterised in that: the filler are as follows: carboxy-modified carbon
One of nanotube, silane-modified white carbon black, gas-phase silica, precipitated silica or activated Calcium carbonate are a variety of.
6. three components tear-proof silicon rubber according to claim 1, it is characterised in that: the radical initiator are as follows: mistake
Aoxidize one of diisopropylbenzene (DIPB) or dibenzoyl peroxide or a variety of.
7. three components tear-proof silicon rubber according to claim 1, it is characterised in that: the vulcanizing agent are as follows: peroxidating two
Bis- (tert-butyl peroxide) hexanes of isopropylbenzene, 2,5- dimethyl -2,5- or 2,5- dimethyl -2,5- bis- (tert-butyl peroxides) are
One of alkynes is a variety of.
8. three components tear-proof silicon rubber according to claim 1, it is characterised in that: the crosslinking agent are as follows: vinyl three
Acetoxylsilane.
9. the preparation method of claim 1 to 8 any three components tear-proof silicon rubber, specific steps are as follows:
(1) silicon rubber, ethylene-vinyl acetate copolymer, crosslinking agent, radical initiator are kneaded at 150 DEG C -200 DEG C
It 5-10 minutes, obtains silicon rubber and is kneaded glue 1；
(2) above-mentioned silicon rubber is kneaded glue 1 and filler, polyurethane under the conditions of 30-50 DEG C, is kneaded 10-20 minutes, obtains silicon rubber
Glue is kneaded glue 2；
(3) dynamic vulcanization: silicon rubber is kneaded glue 2 and vulcanizing agent is placed in double screw extruder, extruder temperature 130-170 is set
DEG C, revolving speed 200-600rpm, dynamic vulcanization obtains three component tear-proof silicon rubber.
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| CN201810926089.2A CN109021583B (en) | 2018-08-15 | 2018-08-15 | Three-component anti-tear silicone rubber and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109627749A (en) * | 2018-12-27 | 2019-04-16 | 山东百多安医疗器械有限公司 | A kind of platinum vulcanization blending-type polyurethane and preparation method thereof |
| CN109651822A (en) * | 2018-12-29 | 2019-04-19 | 山东百多安医疗器械有限公司 | A kind of high-mechanical property medical grade silicon rubber and preparation method thereof |
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| CN105924972A (en) * | 2016-05-24 | 2016-09-07 | 北京化工大学 | Silicone rubber/polyurethane thermoplastic vulcanized rubber and preparing method thereof |
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2018
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| CN101962515A (en) * | 2009-07-22 | 2011-02-02 | 东莞市贝特利新材料有限公司 | Ultraviolet curing adhesive for bonding silicon rubber with plastics |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109627749A (en) * | 2018-12-27 | 2019-04-16 | 山东百多安医疗器械有限公司 | A kind of platinum vulcanization blending-type polyurethane and preparation method thereof |
| CN109627749B (en) * | 2018-12-27 | 2020-12-18 | 山东百多安医疗器械股份有限公司 | Platinum vulcanization mixing type polyurethane and preparation method thereof |
| CN109651822A (en) * | 2018-12-29 | 2019-04-19 | 山东百多安医疗器械有限公司 | A kind of high-mechanical property medical grade silicon rubber and preparation method thereof |
| CN109651822B (en) * | 2018-12-29 | 2021-01-12 | 山东百多安医疗器械股份有限公司 | Medical silicone rubber with high mechanical property and preparation method thereof |
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