CN109867965A - A kind of high-temperature-resisting silicon rubber material and the preparation method and application thereof - Google Patents
A kind of high-temperature-resisting silicon rubber material and the preparation method and application thereof Download PDFInfo
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Abstract
The present invention relates to a kind of high-temperature-resisting silicon rubber materials and the preparation method and application thereof, are obtained by the component of following components and parts by weight is blend sulfurized: 100 parts of organic silicon rubber raw rubber, 10-50 parts of white carbon black, 0.1-10 parts of antistructurizing agent, 0.1~20 part of boron system heat-resistant agent, 0.1~5 part of vulcanizing agent.Its heat resistance greatly improved on the basis of keeping original performance in the high-temperature-resisting organic silicon rubber that the present invention obtains, especially suitable for 200 DEG C -350 DEG C of hot environment, such as engine of spacecraft, aircraft and automobile, fuel pipe, O-ring, electronic component etc..
Description
Technical field
The invention belongs to technique for modifying rubbers field, it is related to a kind of high-temperature-resisting silicon rubber material and preparation method thereof and answers
With.
Background technique
Organic silicon rubber, including methyl silicone rubber, methyl vinyl silicone rubber, phenyl siloxane rubber, methyl vinyl phenyl
Silicon rubber, fluorine silicone rubber, nitrile silicone rubber, the copolymerization materials such as fluorine silicone rubber, because of its excellent heat resistance and energy due to cold tolerance
It has a wide range of applications in the fields such as space flight and aviation, engine.In addition to this, organic silicon rubber product also has oil resistant, resistance to
The advantages that nonpolar chemical agents can be good, thus obtained pushing greatly in medical instrument, electronic equipment, fuel pipe, O-ring
Extensively.Higher and higher to the material requirements used under hot environment however as the development of China's hard-core technology, therefore, improvement has
Machine silastic material thermal stability has great importance.
High-temperature-resisting organic silicon rubber can be modified processing to silicon rubber main chain or side group in the synthesis process, such as adopt
Different end-capping groups are taken, rigid chain segment etc. is introduced, can also directly add in heat-resistant agent to silastic material.Obvious the latter is from behaviour
There is apparent advantage in the property made, continuous heat resistance and industrialization.Many patents also disclose the system of high-temperature resistant rubber material
Preparation Method, such as patent CN106867258A disclose one kind and are blended with fluorine silicone rubber, inclined fluoroether rubber by silicon rubber, and add
It is good that one or more of plus nano diatomite, nanometer calcium silicates, nano kaoline composition obtains a kind of mechanical property
It is good, while the also silicon rubber turbocharging sealing ring material with high temperature resistant, oil resistance.This method auxiliary material addition type is more,
It is at high cost, 3% heat-resistant agent can only make silicon rubber 220 DEG C at a temperature of be used for a long time.
Summary of the invention
Technical problems based on background technology, it is an object of the invention to provide a kind of high-temperature-resisting silicon rubber material and
Preparation method and application.
The present invention uses the boron system heat-resistant agent with excellent heat resistance as organic silicon rubber heat-resistant agent, passes through physical blending
Method is added in organic silicon rubber system, obtains the organic silicon rubber material with lasting high temperature resistant work.The material can be
It is used under the hot environment in the fields such as automobile engine, electronic component and space flight and aviation.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of high-temperature-resisting silicon rubber material is obtained by the component of following components and parts by weight is blend sulfurized:
In one of preferred embodiment of the invention, high-temperature-resisting silicon rubber material, by following components and parts by weight
Component blend sulfurized obtain:
In one of preferred embodiment of the invention, the organic silicon rubber is selected from methyl silicone rubber, methyl second
In alkenyl silicon rubber, phenyl siloxane rubber, methyl vinyl phenyl silicon rubber, nitrile silicone rubber, fluorine silicone rubber or copolymerization fluorine silicone rubber
One kind.
In one of preferred embodiment of the invention, the white carbon black is that specific surface area is greater than equal to 50m2/ g's
Nano silica.
In one of preferred embodiment of the invention, the antistructurizing agent is selected from hydroxy silicon oil, hydroxyl fluorine
Silicone oil, MethylethoxylsiliconFluid Fluid, methyl vinyl silicon oil, two silicon oxygen of diphenyl silanediol, hexamethyldisilazane or hexamethyl
The composition of one or more of alkane.
In one of preferred embodiment of the invention, boron system heat-resistant agent is selected from Inorganic Boron system heat-resistant agent or has
Machine boron system heat-resistant agent；
Inorganic Boron system heat-resistant agent is selected from boron, boron carbide, boron nitride, the group of one or more of boron oxide or boric acid
It closes；
It is different that organic boron system heat-resistant agent is selected from borosilicate oil, triphenylboroxin, triethyl borate, triproylborate, boric acid three
The combination of one or more of propyl ester, butyl borate, three monooctyl ester of boric acid or boric acid three (trimethylsilyl) ester.
In one of preferred embodiment of the invention, the Inorganic Boron system heat-resistant agent partial size 50nm~5 μm it
Between.
In one of preferred embodiment of the invention, the borosilicate oil is by boric acid and hydroxy silicon oil or hydroxyl fluorine
Silicone oil with the ratio of mass ratio 1:5~1:50 60 DEG C~130 DEG C at a temperature of reaction 2-6h obtain.
In one of preferred embodiment of the invention, the vulcanizing agent is selected from 2.4-dichlorobenzoperoxides
(DCBP), 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane (DBPH), cumyl peroxide (DCP), benzoyl peroxide
One of formyl or platinum vulcanizing agent, further preferably 2.4-dichlorobenzoperoxides (DCBP), 2,5- dimethyl-
2,5- bis(t-butylperoxy) hexanes (DBPH) or cumyl peroxide (DCP).
The present invention also provides the preparation methods of the high-temperature-resisting silicon rubber material, by organic silicon rubber raw rubber, white carbon black, knot
Structure controlling agent, the mixing of boron system heat-resistant agent, add vulcanizing agent, are kneaded, vulcanization obtains the high-temperature-resisting silicon rubber material.
The equipment being used in mixed way can be the common mixing facilities such as mixer, open mill or kneader.
When mixing, charging sequence is preferably heat-resisting according to organic silicon rubber raw rubber, antistructurizing agent, white carbon black and boron system
The sequence of agent carries out uniformly mixed, finally adds vulcanizing agent.
The present invention also provides the applications of the high-temperature-resisting silicon rubber material, specifically, the high-temperature-resisting silicon rubber material
Suitable for 200 DEG C -350 DEG C of hot environment, the high-temperature-resisting silicon rubber material is suitable for production spacecraft, aircraft and automobile etc.
Engine, the application of fuel pipe, O-ring, electronic component etc..
In the present invention, organic silicon rubber raw rubber is as basis material；Reinforcing agent of the white carbon black as organic silicon rubber；Structure
The effect for changing controlling agent is reacted with the activity hydroxy of white carbon black, to reduce the structuring effect of white carbon black and organic silica gel；
Boron system heat-resistant agent is mainly used to promote the thermal stability of organic silicon rubber；Vulcanizing agent can make organic silicon rubber crosslinking become stereoscopic graticule
Shape structure, so that its mechanical property be made to greatly improve.The boron system heat-resistant agent that the present invention selects can be with organic silicon rubber raw rubber master
Chain generates nonbonding complexing, and so as to improve the mechanical property and heat resistance of rubber, it is resistance to that this point makes it be different from other
Thermit powder.
In addition, organic silicon rubber raw rubber is as basis material in the present invention, mass parts are 100 parts, the addition of remaining component
Amount determines in proportion after adjusting on this basis.White carbon black optimum amount is 10-50 parts, and white carbon black can excessively make organosilicon rubber
Glue is hardened, and excessively few organic silicon rubber mechanical property that then will lead to is insufficient, can not practical application；Antistructurizing agent optimum amount
It is 0.1-10 parts, antistructurizing agent additive amount is very few, and the structuring phenomenon of organic silicon rubber is obvious, excessively then will lead to organic
The resilience of silicon rubber is bad, curingprocess rate is partially slow；Boron system heat-resistant agent optimum amount be 0.1-20 part, additive amount excessively or
Very few mechanical property can all be deteriorated, but additive amount is very few unobvious to the promotion of organic silicon rubber thermal stability simultaneously；0.1-5 parts
Vulcanizing agent dosage it is best, using excessively will lead to crosslinking excessively, rubber can not be processed vulcanizing agent, excessively few degree of cross linking that then will lead to
Not enough, mechanical property is insufficient.The additive amount of each component of the present invention is the optimal proportion obtained after many experiments.
Compared with prior art, the present invention is using boron system heat-resistant agent as heat-resistant agent, and additive amount is small, to material physical property
Influence small, heat-resisting effect enhancing is significant.High-temperature-resisting silicon rubber material thermal resistance energy of the present invention is good, initial decomposition temperature is high,
Mechanical property is good.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain fluorine silicone rubber
Rubber compound: 100 parts of crude rubber of fluorinated silicone rubber (molecular weight 800,000, contents of ethylene 0.2%)；30 parts of white carbon black Aerosil A300；
5 parts of hydroxy terminated fluorosilicone oil (viscosity 100mPas)；10 parts of amorphous boron powder (partial size 500nm).
2 parts of 2,5- dimethyl -2,5- bis(t-butylperoxy)s are added in S2, above-mentioned fluorinated silicone rubber gross rubber on a mill
Hexane (DBPH) vulcanizing agent, is then molded 10min at 170 DEG C, and post-cure 4h at 200 DEG C obtains the vulcanization rubber of 2mm thickness
Glue.Then the test of the hardness, tensile property, initial decomposition temperature before and after 250 DEG C of thermo-oxidative ageings is carried out.
Embodiment 2
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain ethylene methacrylic
Base silicon rubber gross rubber: 100 parts of methyl vinyl silicon kautschuk (molecular weight 800,000, contents of ethylene 0.2%)；White carbon black
30 parts of Aerosil A300；5 parts of hydroxy silicon oil (viscosity 100mPas)；Borosilicate oil (viscosity 250mPas), 5 parts.Wherein,
Borosilicate oil be by boric acid and hydroxy silicon oil with the ratio of mass ratio 1:20 110 DEG C at a temperature of reaction 4h obtain.
2 part of 2.4-dichlorobenzoperoxide is added in S2, above-mentioned methyl vinyl silicone rubber rubber compound on a mill
(DCBP) then vulcanizing agent is molded 10min at 170 DEG C, post-cure 4h at 200 DEG C obtains the vulcanized rubber of 2mm thickness.So
The test of the hardness, tensile property, initial decomposition temperature before and after 250 DEG C of thermo-oxidative ageings is carried out afterwards.
Embodiment 3
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain phenyl silicon rubber
Glue rubber compound: 100 parts of phenyl siloxane rubber raw rubber (molecular weight 800,000, contents of ethylene 0.2%)；White carbon black Aerosil A300
30 parts；5 parts of diphenyl silanediol (viscosity 100mPas)；10 parts of boron carbide (5 μm of partial size).
2 parts of cumyl peroxide (DCP) vulcanizing agents are added in S2, above-mentioned phenyl siloxane rubber rubber compound on a mill, so
10min is molded at 170 DEG C afterwards, post-cure 4h at 200 DEG C obtains the vulcanized rubber of 2mm thickness.Then 250 DEG C of hot oxygen are carried out
The test of hardness, tensile property, initial decomposition temperature before and after aging.
Comparative example 1
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain fluorine silicone rubber
Rubber compound: 100 parts of crude rubber of fluorinated silicone rubber (molecular weight 800,000, contents of ethylene 0.2%)；30 parts of white carbon black Aerosil A300；
5 parts of hydroxy terminated fluorosilicone oil (viscosity 100mPas).
2 parts of 2,5- dimethyl -2,5- bis(t-butylperoxy)s are added in S2, above-mentioned fluorinated silicone rubber gross rubber on a mill
Hexane (DBPH) vulcanizing agent, is then molded 10min at 170 DEG C, and post-cure 4h at 200 DEG C obtains the vulcanization rubber of 2mm thickness
Glue.Then the test of the hardness, tensile property, initial decomposition temperature before and after 250 DEG C of thermo-oxidative ageings is carried out.
Comparative example 2
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain ethylene methacrylic
Base silicon rubber gross rubber: 100 parts of methyl vinyl silicon kautschuk (molecular weight 800,000, contents of ethylene 0.2%)；White carbon black
30 parts of Aerosil A300；5 parts of hydroxy silicon oil (viscosity 100mPas).
2 part of 2.4-dichlorobenzoperoxide is added in S2, above-mentioned methyl vinyl silicone rubber rubber compound on a mill
(DCBP) then vulcanizing agent is molded 10min at 170 DEG C, post-cure 4h at 200 DEG C obtains the vulcanized rubber of 2mm thickness.So
The test of the hardness, tensile property, initial decomposition temperature before and after 250 DEG C of thermo-oxidative ageings is carried out afterwards.
Comparative example 3
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain phenyl silicon rubber
Glue rubber compound: 100 parts of phenyl siloxane rubber raw rubber (molecular weight 800,000, contents of ethylene 0.2%)；White carbon black Aerosil A300
30 parts；5 parts of diphenyl silanediol (viscosity 100mPas).
2 parts of cumyl peroxide (DCP) vulcanizing agents are added in S2, above-mentioned phenyl siloxane rubber rubber compound on a mill, so
10min is molded at 170 DEG C afterwards, post-cure 4h at 200 DEG C obtains the vulcanized rubber of 2mm thickness.Then 250 DEG C of hot oxygen are carried out
The test of hardness, tensile property, initial decomposition temperature before and after aging.
Comparative example 4
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain fluorine silicone rubber
Rubber compound: 100 parts of crude rubber of fluorinated silicone rubber (molecular weight 800,000, contents of ethylene 0.2%)；30 parts of white carbon black Aerosil A300；
5 parts of hydroxy terminated fluorosilicone oil (viscosity 100mPas), iron oxide (5 μm).
2 parts of 2,5- dimethyl -2,5- bis(t-butylperoxy)s are added in S2, above-mentioned fluorinated silicone rubber gross rubber on a mill
Hexane (DBPH) vulcanizing agent, is then molded 10min at 170 DEG C, and post-cure 4h at 200 DEG C obtains the vulcanization rubber of 2mm thickness
Glue.Then the test of the hardness, tensile property, initial decomposition temperature before and after 250 DEG C of thermo-oxidative ageings is carried out.
Comparative example 5
S1, by the formula of component below and parts by weight in mixer, mix 10min at 170 DEG C, obtain phenyl silicon rubber
Glue rubber compound: 100 parts of phenyl siloxane rubber raw rubber (molecular weight 800,000, contents of ethylene 0.2%)；White carbon black Aerosil A300
30 parts；5 parts of diphenyl silanediol (viscosity 100mPas)；20 parts of boron carbide (5 μm of partial size).
2 parts of cumyl peroxide (DCP) vulcanizing agents are added in S2, above-mentioned phenyl siloxane rubber rubber compound on a mill, so
10min is molded at 170 DEG C afterwards, post-cure 4h at 200 DEG C obtains the vulcanized rubber of 2mm thickness.Then 250 DEG C of hot oxygen are carried out
The test of hardness, tensile property, initial decomposition temperature before and after aging.
Evaluation
1, vulcanization silica gel piece obtained by embodiment 1-3, comparative example 1-5 is toasted 72 hours at 250 DEG C respectively, and to aging before
Mechanical property afterwards is evaluated, while testing the mass loss rate after 350 DEG C of constant temperature agings for 24 hours and TGA test.
2, evaluation index and test method:
Hardness: GB/T 531.1-2008
Tensile strength: GB/T 528-2009
Elongation: GB/T 528-2009
Mass loss rate: weighing after constant temperature is placed for 24 hours in 350 DEG C of Muffle furnace, takes out the quality after weighing aging,
Calculate mass loss rate.
Initial decomposition temperature: it is tested using the 409 PC type thermogravimetric analyzer of STA of Netzsch company, Germany.
Embodiment 1-3, comparative example 1-5 the performance test results as shown in the following table 1, table 2, table 3.
The initial mechanical the performance test results of 1 embodiment 1-3 of table, comparative example 1-5
2 embodiment 1-3 of table, comparative example 1-5 mechanical experimental results after 250 DEG C of aging 72h
The performance test results after 2 embodiment 1-3 of table, comparative example 1-5TGA, 350 DEG C of constant temperature agings for 24 hours
| Test content | TGA | 350 DEG C of constant temperature agings are for 24 hours |
| Performance parameter | Initial decomposition temperature (DEG C) | Mass loss rate (%) |
| Embodiment 1 | 398 | 44.4 |
| Embodiment 2 | 387 | 42.9 |
| Embodiment 3 | 450 | 38.7 |
| Comparative example 1 | 349 | 53.7 |
| Comparative example 2 | 359 | 51.6 |
| Comparative example 3 | 380 | 45.8 |
| Comparative example 4 | 371 | 41.3 |
| Comparative example 5 | 449 | 36.5 |
The present invention selects suitable antistructurizing agent to react with the activity hydroxy on white carbon black, reduce white carbon black and
Organic silicon rubber recurring structure phenomenon；Suitable boron system heat-resistant agent can make on the basis of promoting organic silicon rubber heat resistance
It keeps excellent mechanical property, it is also ensured that it is evenly dispersed in rubber base material；And suitable vulcanizing agent can
It is excessively crosslinked to avoid organic silicon rubber and is unlikely to not processing.By adjusting the proportion of each raw material, assist the performance of each raw material
With promotion, finally obtained high-temperature-resisting organic silicon rubber material has the characteristics that long-time high temperature resistant, excellent in mechanical performance.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of high-temperature-resisting silicon rubber material, which is characterized in that obtained by the component of following components and parts by weight is blend sulfurized:
2. a kind of high-temperature-resisting silicon rubber material according to claim 1, which is characterized in that the organic silicon rubber is selected from first
Base silicon rubber, methyl vinyl silicone rubber, phenyl siloxane rubber, methyl vinyl phenyl silicon rubber, nitrile silicone rubber, fluorine silicone rubber or
It is copolymerized one of fluorine silicone rubber.
3. a kind of high-temperature-resisting silicon rubber material according to claim 1, which is characterized in that the white carbon black is specific surface area
More than or equal to 50m2The nano silica of/g.
4. a kind of high-temperature-resisting silicon rubber material according to claim 1, which is characterized in that the antistructurizing agent is selected from
Hydroxy silicon oil, hydroxy terminated fluorosilicone oil, MethylethoxylsiliconFluid Fluid, methyl vinyl silicon oil, diphenyl silanediol, hexamethyldisilazane
Or the composition of one or more of hexamethyldisiloxane.
5. a kind of high-temperature-resisting silicon rubber material according to claim 1, which is characterized in that boron system heat-resistant agent is selected from nothing
Machine boron system's heat-resistant agent or organic boron system heat-resistant agent；
Inorganic Boron system heat-resistant agent is selected from boron, boron carbide, boron nitride, the combination of one or more of boron oxide or boric acid；
Organic boron system heat-resistant agent be selected from borosilicate oil, triphenylboroxin, triethyl borate, triproylborate, triisopropyl borate ester,
The combination of one or more of butyl borate, three monooctyl ester of boric acid or boric acid three (trimethylsilyl) ester.
6. a kind of high-temperature-resisting silicon rubber material according to claim 5, which is characterized in that the Inorganic Boron system heat-resistant agent grain
Diameter is between 50nm~5 μm.
7. a kind of high-temperature-resisting silicon rubber material according to claim 5, which is characterized in that the borosilicate oil be by boric acid and
Hydroxy silicon oil or hydroxy terminated fluorosilicone oil are obtained with the ratio of mass ratio 1:5~1:50 in 60 DEG C~130 DEG C of at a temperature of reaction 2-6h.
8. a kind of high-temperature-resisting silicon rubber material according to claim 1, which is characterized in that the vulcanizing agent is selected from 2.4-
Dichlorobenzoperoxide, 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane, cumyl peroxide, benzoyl peroxide
One of formyl or platinum vulcanizing agent.
9. the preparation method of high-temperature-resisting silicon rubber material as described in any one of claim 1-8, which is characterized in that by organosilicon
Rubber raw rubber, white carbon black, antistructurizing agent, the mixing of boron system heat-resistant agent, add vulcanizing agent, and mixing, vulcanization obtain described resistance to
High temperature silicone rubber material.
10. the application of high-temperature-resisting silicon rubber material as described in any one of claim 1-8, which is characterized in that the high temperature resistant
Silastic material is suitable for 200 DEG C -350 DEG C of hot environment, and the high-temperature-resisting silicon rubber material is for making spacecraft, aircraft
With the engine of automobile, fuel pipe, O-ring, electronic component.
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| CN110982277A (en) * | 2019-12-23 | 2020-04-10 | 成都硅宝科技股份有限公司 | Single-component temperature-resistant heat-conducting silicon mud composition and preparation method thereof |
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| CN111073057B (en) * | 2019-12-23 | 2021-10-12 | 广州市白云化工实业有限公司 | Heat-resistant additive, silicone rubber material and preparation method of silicone rubber material |
| CN110982277B (en) * | 2019-12-23 | 2022-02-22 | 成都硅宝科技股份有限公司 | Single-component temperature-resistant heat-conducting silicon mud composition and preparation method thereof |
| CN112358728A (en) * | 2020-12-06 | 2021-02-12 | 西安长峰机电研究所 | Low-characteristic signal heat insulation layer material |
| CN113308120A (en) * | 2021-06-30 | 2021-08-27 | 华南理工大学 | Light ceramizable silicone rubber and preparation method thereof |
| CN113308120B (en) * | 2021-06-30 | 2022-05-24 | 华南理工大学 | Light ceramizable silicone rubber and preparation method thereof |
| CN113698883A (en) * | 2021-08-20 | 2021-11-26 | 广东天跃新材料股份有限公司 | Intelligent touch organic silicon synthetic leather |
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Application publication date: 20190611 |