CN108129850A - A kind of high rebound high-strength silicone rubber and preparation method thereof - Google Patents
A kind of high rebound high-strength silicone rubber and preparation method thereof Download PDFInfo
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- 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
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses a kind of high rebound high-strength silicone rubbers and preparation method thereof.A kind of high rebound high-strength silicone rubber, raw material components include the component of following parts by weight:Methyl vinyl silicone rubber, 100 parts;Super high molecular weight dimethyl silicone rubber, 2~10 parts;Precipitated silica, 10 parts~40 parts;Super-fine silicon micro-powder, 5~30 parts;Silicone powder, 3~15 parts;Hydroxyvinyl silicone oil, 1~3 part;Containing hydrogen silicone oil, 0.1 part~1 part;Inner pattern releasing agent applicable, 0.05 part~1 part and vulcanizing agent, 0.3 part~2 parts.High rebound high-strength silicone rubber of the invention, reduces the dosage of low viscosity hydroxy silicon oil, significantly improves the resilience after silicon rubber vulcanization, and the overall performance of silicon rubber is improved significantly;Preparation method of the present invention is simple to operation.
Description
Technical field
The present invention relates to a kind of high rebound high-strength silicone rubbers and preparation method thereof, belong to silicone rubber art.
Background technology
Silicon rubber is the macromolecular elastomer for having both organic material and inorganic material performance, has many excellent properties, such as
Weatherability, electrical property, low compressive deformation, heat resistance and cold resistance, be widely used in electrical equipment, field of motor vehicles,
Building field, medical domain, field of food industry etc..It such as can be as the rubber in remote controler, terminal, musical instrument etc.
Contact, building pad, and the fixing roller, developer roll, photocopying roll, band point roller and feeding-in roll, audio frequency apparatus etc. in business machine are prevented
Shake rubber, the packaging of compact disk and wire covering material.
Resilience performance is a key index for weighing seal member material properties quality, and embodying sealing material, to fill up sealing scarce
It falls into and the ability of elastic compensating, good sealing material should have good resilience.Since resilience is good, compression becomes silicon rubber
Shape is smaller, can be used as the manufacture raw material of kitchen articles, axle envelope circle, washer, nipple, sundries connector and office equipment etc., application
It is in extensive range.With the development of science and technology, higher requirement is also proposed to the resilience performance of silicon rubber, it is of the prior art
High-temperature silicon disulfide rubber due to the relatively low particular/special requirement that cannot meet certain products in the market of rebound degree,
At present, mainly by compounding technique and addition new auxiliary, change the modification technologies such as crosslinking method and copolymerizing and blending,
Make silicon rubber that there is higher resilience performance.Such as different end ethylene are used in the patent document of Publication No. CN106633910A
Base raw rubber and the white carbon of processing prepare high rebound High tear resistance silicon rubber composition;The patent text of Publication No. CN104194352A
High resiliency is prepared by the way of blending for raw material with methyl vinyl silicone rubber, chlorinated scoline, phenolic resin etc. in offering
Silicon rubber.Though both the above method can improve the resilience of silicon rubber, that improves is not obvious.
Invention content
In order to solve the defects of silicon rubber resilience is poor in the prior art, the present invention provides a kind of high rebound high intensity silicon rubber
Glue and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
A kind of high rebound high-strength silicone rubber, raw material components include the component of following parts by weight:
Methyl vinyl silicone rubber, 100 parts;
Super high molecular weight dimethyl silicone rubber, 2~10 parts;
Precipitated silica, 10 parts~40 parts;
Super-fine silicon micro-powder, 5~30 parts;
Silicone powder, 3~15 parts
Hydroxyvinyl silicone oil, 1~3 part;
Containing hydrogen silicone oil, 0.1 part~1 part;
Inner pattern releasing agent applicable, 0.05 part~1 part;
Vulcanizing agent, 0.3 part~2 parts.
Reinforced filling is promoted to exist by way of adding great amount of hydroxy group silicone oil or vinyl silicone oil in silicon rubber industry at present
Dispersion in silicon rubber, but the addition of silicone oil with low viscosity can greatly reduce the resilience of silicon rubber.The principle of the present invention is
Dispersion of the reinforced filling in silicon rubber is promoted by the method for adding lubricant silicone powder, improves compatibility between the two,
The additive amount of silicone oil with low viscosity is reduced to the maximum extent, so as to improve the resilience of silicon rubber;Simultaneously with methyl ethylene silicon rubber
Glue and the dimethyl raw rubber of super high molecular weight compounding as basic raw rubber, using precipitated silica and super-fine silicon micro-powder it is mashed up as
Reinforced filling, the common resilience for improving silicon rubber;And applicant it has been investigated that, each material component selected by the application it
Between synergistic effect it is apparent, make the promotion highly significant of silicon rubber resilience and intensity.
In order to further promote the synergistic effect between each component, the resilience of silicon rubber and other mechanics are further improved
Performance, methyl vinyl silicone rubber are (5-7) by mass ratio:First methyl vinyl silicone rubber of (5-3) and the second methyl second
Alkenyl silicon rubber compounds, wherein, the first methyl vinyl silicone rubber medium vinyl molar content is 0.03%~0.09%,
Molecular weight is 650,000~750,000;Second methyl vinyl silicone rubber medium vinyl molar content is 0.25%~1.5%, molecular weight
It is 500,000~650,000.
It is preferred that the molecular weight of super high molecular weight dimethyl silicone rubber is 100~1,200,000, super high molecular weight dimethyl-silicon rubber
Vinyl is not contained on the chain link of glue, structural formula is:
Wherein the value range of m is 13000~17000.It can be further ensured that the resilience of products obtained therefrom in this way.
It is preferred that the mass content of siloxanes is 40~60% in silicone powder, the dispersibility of material can further improve in this way
And compatibility, while further improve the resilience of silicon rubber.
Silicone powder is a kind of powder formed by the mixing of siloxanes, silica and other auxiliary agents (such as silane coupling agent).
The specific surface area of precipitated silica is not less than 150m2/g.It is preferred that the specific surface area of precipitated silica is
150m2/ g or 200m2/g。
It is preferred that the grain size of super-fine silicon micro-powder is 0.3~2 μm, preferably 0.5~1 μm.Which further increases each raw materials
The compatibility of component and the mechanical property of silicon rubber.
It is preferred that hydroxyvinyl silicone oil is hydroxy-end capped vinyl silicone oil, structure is as follows:
It is 5~20 that wherein m value ranges, which are 50~150, n value ranges, the viscosity of hydroxyvinyl silicone oil for 100~
250cst, contents of ethylene are 3.5~10%.Which further increases the compatibility of each raw material components and the mechanics of silicon rubber
Performance.
It is preferred that hydrogen content is more than 1.5%wt in containing hydrogen silicone oil, it can further promote the association between each raw material components in this way
Same effect, and then further improve the resilience of silicon rubber.
It is preferred that releasing agent is stearic acid or stearate, stearate is in zinc stearate, magnesium stearate or calcium stearate
At least one;Vulcanizing agent for double two or four (the 2,4- dichlorobenzoperoxides) of peroxide or it is double two or five (2,5- dimethyl -2,
5- di-t-butyl hexane peroxides).The synergistic effect between each raw material components can further be promoted in this way, and then further improved
Resilience and mechanical property of silicon rubber etc..
The preparation method of above-mentioned high rebound high-strength silicone rubber, including following steps connected in order:
1) by methyl vinyl silicone rubber, super high molecular weight dimethyl silicone rubber, silicone powder, hydroxyvinyl silicone oil, contain
Hydrogen silicone oil and inner pattern releasing agent applicable are uniformly mixed in kneader;
2) precipitated silica and super-fine silicon micro-powder are added in step 1) resulting material, wherein, precipitated silica and
Super-fine silicon micro-powder adds in four times, four additions of precipitated silica and super-fine silicon micro-powder respectively are 40 ± 3%,
25 ± 3%, 20 ± 3%, 15 ± 3%, after charging, at normal pressure, temperature 60 C~80 DEG C, stirring is mediated, agglomerating, agglomerating
After continue 10~30min of kneading;
3) step 2) resulting material is warming up to 100 DEG C~120 DEG C, it is close in the case where vacuum degree is -0.8MPa~-0.9MPa
1.5 ± 0.2h is refined, 24 ± 2h is parked in then cooling, obtains rubber compound;
4) by rubber compound obtained by step 3) and vulcanizing agent mixing, first vulcanize 5 ± 1 minutes at 175 ± 5 DEG C, then 200 ±
5 DEG C vulcanize 4 ± 1 hours, obtain high rebound high-strength silicone rubber.
The unmentioned technology of the present invention is with reference to the prior art.
High rebound high-strength silicone rubber of the invention, reduces the dosage of low viscosity hydroxy silicon oil, significantly improves silicon rubber
Resilience after vulcanization, and the overall performance of silicon rubber is improved significantly;Preparation method of the present invention is simple to operation.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
The measurement unit " part " of each substance refers to parts by weight in following each embodiments.
Raw material in following embodiments is commercial goods.
Embodiment 1
In terms of mass fraction, in vacuum mixer, 70 parts of dimethyl ethenyl sealing ends are added in, molecular weight is 650,000, second
Alkenyl molar content be 0.05% methyl vinyl silicone rubber (Dongjue Silicone Group Company Limited), 30 parts of dimethyl second
Alkenyl sealing end, methyl vinyl silicone rubber (the eastern rank of nobility organosilicon that molecular weight is 550,000, the molar content of vinyl is 0.25%
(Nanjing) Co., Ltd), the dimethyl-silicon raw rubber (Dongjue Silicone Group Company Limited) that 2.0 parts of molecular weight are 1,000,000,5
Part silicone powder (KJ-B01, Kai Jie plastic toughenings Materials Co., Ltd of Jiande City), the hydroxyl second that 1.0 parts of dynamic viscosities are 155cst
Alkenyl silicone oil (Wuxi Quan Li Chemical Co., Ltd.s, contents of ethylene 6%), the containing hydrogen silicone oil (nothing of 0.5 part of hydrogen content 1.53%
Xi Quanli Chemical Co., Ltd.s), 0.2 part of calcium stearate is uniformly mixed in kneader.
2) it is 150m that 15 parts of specific surface areas are added in step 1)2(Fujian Far Glory chemical industry is limited for the precipitated silica of/g
Company) and 5 parts of super-fine silicon micro-powders (Xin Chuan mining industry Co., Ltd of Guangdong Nanhai, grain size are 1 μm), wherein white carbon and ultra-fine silicon is micro-
Powder adds in four times, and four precipitated silicas and super-fine silicon micro-powder addition are followed successively by 40%, 25%, 20%, 15%,
After material adds in, under normal pressure, temperature 70 C, stirring mediates, is agglomerating, continues to mediate 20min after agglomerating, obtains sizing material.
3) sizing material obtained by step 2) is warming up to 110 DEG C, in the case where vacuum degree is -0.8MPa~-0.9MPa, vacuum high-temperature
Mixing 1.5h, cooling are parked for 24 hours, obtain rubber compound.
4) by 100 parts of rubber compounds obtained by step 3) and 0.65 portion of peroxide vulcanizing agent double 25 (2,5- dimethyl -2,
5- bis(t-butylperoxy)s hexane) it is refined in open mill uniformly, first vulcanize at 175 DEG C 5 minutes, it is then small in 200 DEG C of vulcanizations 4
When, obtain high elastic and strength silicone rubber compound.
The present invention is tested for the property obtained high elastic and strength silicone rubber compound, and the results are shown in Table 1.
Embodiment 2
In terms of mass fraction, in vacuum mixer, 80 parts of dimethyl ethenyl sealing ends are added in, molecular weight is 700,000, second
Alkenyl molar content be 0.06% methyl vinyl silicone rubber (Dongjue Silicone Group Company Limited), 20 parts of dimethyl second
Alkenyl sealing end, methyl vinyl silicone rubber (the eastern rank of nobility organosilicon (south that molecular weight is 550,000, vinyl molar content is 0.3%
Capital) Co., Ltd), the dimethyl raw rubber (Dongjue Silicone Group Company Limited) that 3.0 parts of molecular weight are 1,000,000,8 parts of silicone
Powder (KJ-B01, Kai Jie plastic toughenings Materials Co., Ltd of Jiande City), the hydroxyvinyl silicon that 1.0 parts of dynamic viscosities are 155cst
Oily (Wuxi Quan Li Chemical Co., Ltd.s, contents of ethylene 6%), containing hydrogen silicone oil (Wuxi verticalization entirely of 1 part of hydrogen content 1.50%
Work Co., Ltd), 0.3 part of zinc stearate is uniformly mixed in kneader.
2) it is 150m that 25 parts of specific surface areas are added in step 1)2(Fujian Far Glory chemical industry is limited for the precipitated silica of/g
Company) and 10 parts of super-fine silicon micro-powders (Xin Chuan mining industry Co., Ltd of Guangdong Nanhai, grain size are 1 μm), wherein white carbon and ultra-fine silicon
Micro mist adds in four times, four precipitated silicas and super-fine silicon micro-powder addition are followed successively by 40%, 25%, 20%,
15%, after material adds in, under normal pressure, temperature 60 C, stirring mediates, is agglomerating, continues to mediate 30min after agglomerating, obtains glue
Material.
3) sizing material of step 2) is warming up to 100 DEG C, in the case where vacuum degree is -0.8MPa~-0.9MPa, vacuum high-temperature mixing
1.5h, cooling are parked for 24 hours, obtain rubber compound.
4) 100 parts of rubber compounds obtained by step 3) and 0.65 portion of peroxide vulcanizing agent double 25 are refined in open mill equal
It is even, first vulcanize at 175 DEG C 5 minutes, then vulcanize 4 hours at 200 DEG C, obtain high elastic and strength silicone rubber compound.This hair
Bright that obtained high elastic and strength silicone rubber compound is tested for the property, the results are shown in Table 1.
Embodiment 3
In terms of mass fraction, in vacuum mixer, 50 parts of dimethyl ethenyl sealing ends are added in, molecular weight is 750,000, second
Alkenyl molar content be 0.05% methyl vinyl silicone rubber (Dongjue Silicone Group Company Limited), 50 parts of dimethyl second
Alkenyl sealing end, methyl vinyl silicone rubber (the eastern rank of nobility organosilicon (south that molecular weight is 500,000, vinyl molar content is 0.5%
Capital) Co., Ltd), the dimethyl raw rubber (Dongjue Silicone Group Company Limited) that 3 parts of molecular weight are 1,000,000,4 parts of silicone powders
(KJ-B01, Kai Jie plastic toughenings Materials Co., Ltd of Jiande City), the hydroxyvinyl silicone oil that 2.5 parts of dynamic viscosities are 100cst
(Wuxi Quan Li Chemical Co., Ltd.s, contents of ethylene 6%), the containing hydrogen silicone oil of 1 part of hydrogen content 1.53% (found chemical industry in Wuxi entirely
Co., Ltd), 0.5 part of calcium stearate is uniformly mixed in kneader.
2) it is 200m that 35 parts of specific surface areas are added in step 1)2(Fujian Far Glory chemical industry is limited for the precipitated silica of/g
Company), 10 parts of super-fine silicon micro-powders (Xin Chuan mining industry Co., Ltd of Guangdong Nanhai, grain size are 1 μm), wherein white carbon and ultra-fine silicon is micro-
Powder adds in four times, and four fume colloidal silicas and super-fine silicon micro-powder addition are followed successively by 40%, 25%, 20%, 15%,
After material adds in, at normal pressure, 80 DEG C of temperature, stirring mediates, is agglomerating, continues to mediate 10min after agglomerating, obtains sizing material.
3) sizing material of step 2) is warming up to 120 DEG C, in the case where vacuum degree is -0.8MPa~-0.9MPa, vacuum high-temperature mixing
1.5h, cooling are parked for 24 hours, obtain rubber compound.
4) it by 100 parts of rubber compounds obtained by step 3) and 0.65 portion of peroxide vulcanizing agent double 25, is refined in open mill
Uniformly, first vulcanize 5 minutes at 175 DEG C, then vulcanize 4 hours at 200 DEG C, obtain high elastic and strength silicone rubber compound.
The present invention is tested for the property obtained high elastic and strength silicone rubber compound, and the results are shown in Table 1.
Performance test
Silicone rubber compound made from embodiment is carried out to the test of mechanical performance, test method:It is GB/ according to standard No.
The national standard of T528-2009 is to the obtained tensile strength of high elastic and strength silicone rubber compound and elongation at break progress
Test;According to the tear of high elastic and strength silicone rubber compound of the national standard that standard No. is GB/T529-2008 to obtaining
Intensity is tested;By the national standard that standard No. is GB/T531.1-2008 to obtained high elastic and strength rubber composition
The shore hardness of object is tested;By the national standard that standard No. is GB/T 1681-2009 to obtained high elastic and strength silicon
The resilience of rubber composition is tested.
Test result is shown in Table 1:
1 high elastic and strength silicone rubber compound performance measurement of table
Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
Shore hardness (A) | 45 | 52 | 65 |
Tensile strength (MPa) | 9.6 | 10 | 9.8 |
Elongation (%) | 923 | 956 | 946 |
Tearing strength (kN/m) | 38.9 | 39.2 | 38.2 |
Resilience (%) | 75 | 72 | 70 |
As shown in Table 1, the present invention provides a kind of high elastic and strength silicone rubber compound, the resiliences of this composition
Reach more than 70%, while tensile strength can reach 10MPa.
Claims (10)
1. a kind of high rebound high-strength silicone rubber, it is characterised in that:Its raw material components includes the component of following parts by weight:
Methyl vinyl silicone rubber, 100 parts;
Super high molecular weight dimethyl silicone rubber, 2~10 parts;
Precipitated silica, 10 parts~40 parts;
Super-fine silicon micro-powder, 5~30 parts;
Silicone powder, 3~15 parts;
Hydroxyvinyl silicone oil, 1~3 part;
Containing hydrogen silicone oil, 0.1 part~1 part;
Inner pattern releasing agent applicable, 0.05 part~1 part;
Vulcanizing agent, 0.3 part~2 parts.
2. high rebound high-strength silicone rubber according to claim 1, it is characterised in that:Methyl vinyl silicone rubber is by quality
Than for (5-7):First methyl vinyl silicone rubber and the second methyl vinyl silicone rubber of (5-3) compound, wherein, first
Methyl vinyl silicone rubber medium vinyl molar content is 0.03%~0.09%, and molecular weight is 650,000~750,000;Second methyl
Vinylsiloxane rubber medium vinyl molar content is 0.25%~1.5%, and molecular weight is 500,000~650,000.
3. high rebound high-strength silicone rubber according to claim 1 or 2, it is characterised in that:Super high molecular weight dimethyl-silicon
The molecular weight of rubber is 95~1,200,000, and vinyl, structural formula are not contained on the chain link of super high molecular weight dimethyl silicone rubber
For:
Wherein the value range of m is 13000~17000.
4. high rebound high-strength silicone rubber according to claim 1 or 2, it is characterised in that:The matter of siloxanes in silicone powder
It is 40~60% to measure content.
5. high rebound high-strength silicone rubber according to claim 1 or 2, it is characterised in that:The ratio table of precipitated silica
Area is not less than 150m2/g。
6. high rebound high-strength silicone rubber according to claim 1 or 2, it is characterised in that:The grain size of super-fine silicon micro-powder is
0.3~2 μm.
7. high rebound high-strength silicone rubber according to claim 1 or 2, it is characterised in that:Hydroxyvinyl silicone oil is hydroxyl
The vinyl silicone oil of base sealing end, structure are as follows:
It is 5~20 that wherein m value ranges, which are 50~150, n value ranges, the viscosity of hydroxyvinyl silicone oil for 100~
250cst, contents of ethylene are 3.5~10%.
8. high rebound high-strength silicone rubber according to claim 1 or 2, it is characterised in that:Hydrogen content is in containing hydrogen silicone oil
More than 1.5%wt.
9. high rebound high-strength silicone rubber according to claim 1 or 2, it is characterised in that:Inner pattern releasing agent applicable for stearic acid or
Stearate, stearate are at least one of zinc stearate, magnesium stearate or calcium stearate;Vulcanizing agent is double for peroxide
Two or four (2,4- dichlorobenzoperoxides) or double two or five (2,5- dimethyl -2,5- di-t-butyl hexane peroxides).
10. the preparation method of high rebound high-strength silicone rubber described in any one of claim 1-9, it is characterised in that:Including
Following steps connected in order:
1) by methyl vinyl silicone rubber, super high molecular weight dimethyl silicone rubber, silicone powder, hydroxyvinyl silicone oil, Silicon Containing Hydrogen
Oil and inner pattern releasing agent applicable are uniformly mixed in kneader;
2) precipitated silica and super-fine silicon micro-powder are added in step 1) resulting material, wherein, precipitated silica and ultra-fine
Silicon powder adds in four times, and four additions of precipitated silica and super-fine silicon micro-powder respectively are 40 ± 3%, 25 ±
3%th, 20 ± 3%, 15 ± 3%, after charging, at normal pressure, temperature 60 C~80 DEG C, stirring is mediated, agglomerating, agglomerating subsequent
It is continuous to mediate 10~30min;
3) step 2) resulting material is warming up to 100 DEG C~120 DEG C, in the case where vacuum degree is -0.8MPa~-0.9MPa, mixing 1.5
± 0.2h, then cooling park 24 ± 2h, obtain rubber compound;
4) by rubber compound obtained by step 3) and vulcanizing agent mixing, first vulcanize 5 ± 1 minutes at 175 ± 5 DEG C, then at 200 ± 5 DEG C
Vulcanization 4 ± 1 hours obtains high rebound high-strength silicone rubber.
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