CN106519701A - Method for preparing heatproof silicone rubber having ethyl phenyl hydrogen-assisted cage-type silsesquioxane - Google Patents
Method for preparing heatproof silicone rubber having ethyl phenyl hydrogen-assisted cage-type silsesquioxane Download PDFInfo
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- CN106519701A CN106519701A CN201610918247.0A CN201610918247A CN106519701A CN 106519701 A CN106519701 A CN 106519701A CN 201610918247 A CN201610918247 A CN 201610918247A CN 106519701 A CN106519701 A CN 106519701A
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- cage
- type silsesquioxane
- hydrogen
- silicone 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
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to a method for preparing a heatproof silicone rubber having ethyl phenyl hydrogen-assisted cage-type silsesquioxane, which relates to the method for preparing the silicone rubber. The silicone rubber is obtained by methyl phenyl vinyl silicone oil, ethyl phenyl hydrogen-assisted cage-type silsesquioxane, a metal oxide, and a PC610 catalyst inhibitor under effect of a Pt catalyst. The cage-type silsesquioxane containing phenyl ring and silicon-hydrogen group (the number of phenyl ring and the silicon-hydrogen group is determined according to the mol ratio of cage-type octahydridospherosiloxane to styrene) is introduced into the silicone rubber, the vinyl in cage-type silsesquioxane and the silicone rubber is subjected to an addition reaction, crosslinking density of the silicone rubber is increased, and the novel POSS-enhanced room-temperature vulcanized silicone rubber having good heat stability and mechanical property is prepared.
Description
Technical field
The present invention relates to a kind of silicon rubber preparation method, more particularly to a kind of to carry ethylbenzene hydrogen-based cage model sesquialter silica
Alkane heat-resistant silicon rubber preparation method.
Background technology
As the application of the development silicon rubber of modern industry is more and more wider, send out as space flight and aviation Military Electronics electrical equipment
Motivation industry main parts size material, with host performance lifting mutually tackle parts material property requirement increasingly
Harshness, existing silicon rubber cannot meet stricter resistance to elevated temperatures and require, directly hinder the development of related industry.
Thus a kind of high temperature resistant is developed, the good silicon rubber of mechanical property becomes current study hotspot.
The content of the invention
It is an object of the invention to provide a kind of carry ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation side
Method, the method embedded in phenyl ring on the basis of cage-type silsesquioxane inorganic skeleton, also, and two kinds of structures mutually act synergistically,
Greatly improve silicon rubber heat-resisting temperature and its mechanical property.
The purpose of the present invention is achieved through the following technical solutions：
It is a kind of to carry ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method, prepared by following steps：
i）The synthesis of ethylbenzene hydrogen-based cage-type silsesquioxane；
ii）Sequentially add multi-vinyl silicone oil, metal oxide, PC610 inhibitor, Pt platinum catalysts, mechanical agitation mixing
Uniformly, 100 DEG C of vaccum dewatering 5h；Add above-mentioned preparation is dissolved in having containing ethylbenzene hydrogen-based cage-type silsesquioxane for toluene
Machine silicon crosslinking agent, the bubble being well mixed in rear low pressure removing system can be fully cured after being heat-treated 4h at 100 DEG C；
Reaction equation is as follows：
。
Described one kind carries ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method, multi-vinyl silicone oil
For methyl phenyl vinyl silicone oil, viscosity is 30200mPa s, and phenyl mass fraction is 55%, and vinyl mass fraction is
3.6%；
Described one kind carries ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method, and metal oxide is
Fe2O3、 CeO2、 ZnO、 TiO2、 V2O5, above-mentioned oxide using individually one or more, its granularity is 0.1～5
μm scope.
Described one kind carries ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method, eight in above-mentioned reaction
Hydrogen-based cage-type silsesquioxane and styrene press 1：The mol ratio of n carries out reaction n=1, and 2,3,4,5,6,7,8, according to rubbing for reaction
, than difference, the product such as number of above formula R bases and position is also different for you（The number of phenyl ring and hydrogen bond is by cage modle octahydro base sesquialter
Siloxanes and cinnamic mol ratio are determined）, it is being that n is not equal to 8 as silicone rubber crosslinking agent, so reaction equation is with mol ratio
For 1:As a example by 1 reaction.
Advantages of the present invention with effect is：
In the present invention, silicon rubber is by methyl phenyl vinyl silicone oil, ethylbenzene hydrogen-based cage-type silsesquioxane crosslinking agent, metal oxygen
Compound, PC610 catalyst-initiators are reacted under Pt catalyst actions and are obtained.The present invention will not only contain phenyl ring but also contain silicon hydrogen
The cage-type silsesquioxane of base（The number of phenyl ring and si-h bond is determined by cage modle octahydro base silsesquioxane and cinnamic mol ratio
It is fixed）It is incorporated in the middle of silicon rubber, cage-type silsesquioxane and silicon rubber medium vinyl occur addition reaction, improve silicon rubber
Crosslink density, prepares the novel Room Temperature sulphurated siliastic of the POSS enhancement mode with good thermal stability and mechanical property.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
In embodiment, raw material removes specified otherwise, is commercial.
In embodiment crosslinking agent ethylbenzene hydrogen-based cage-type silsesquioxane used be by octahydro base cage-type silsesquioxane and
Styrene presses 1：4 mol ratio carries out reacting what is obtained.
Embodiment 1
Take 100 parts of methyl phenyl vinyl silicone oils, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, 0.2 part of PC610,0.5 part of Pt
Platinum catalyst, mechanical agitation are well mixed, 100 DEG C of vaccum dewatering 5h.Add 35 parts of ethylbenzene hydrogen-baseds being dissolved in toluene
Cage-type silsesquioxane organosilicon cross-linking agent, the bubble being well mixed in rear low pressure removing system；4h is heat-treated at 100 DEG C
Can be fully cured afterwards.The performance of gained cured glue body is tested according to GB/T 13477.6-2002.
Embodiment 2
Take 100 parts of methyl phenyl vinyl silicone oils, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, 0.2 part of PC610,0.5 part of Pt
Platinum catalyst, mechanical agitation are well mixed, 100 DEG C of vaccum dewatering 5h.Add 45 parts of ethylbenzene hydrogen-baseds being dissolved in toluene
Cage-type silsesquioxane organosilicon cross-linking agent, the bubble being well mixed in rear low pressure removing system；4h is heat-treated at 100 DEG C
Can be fully cured afterwards.The performance of gained cured glue body is tested according to GB/T 13477.6-2002.
Embodiment 3
Take 100 parts of methyl phenyl vinyl silicone oils, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, 0.2 part of PC610,0.5 part of Pt
Platinum catalyst, mechanical agitation are well mixed, 100 DEG C of vaccum dewatering 5h.Add 55 parts of ethylbenzene hydrogen-baseds being dissolved in toluene
Cage-type silsesquioxane organosilicon cross-linking agent, the bubble being well mixed in rear low pressure removing system；4h is heat-treated at 100 DEG C
Can be fully cured afterwards.The performance of gained cured glue body is tested according to GB/T 13477.6-2002：
The silicon rubber prepared from data above, present invention ethylbenzene hydrogen-based cage-type silsesquioxane, heat resistance
It is excellent, good mechanical properties.
Claims (4)
1. it is a kind of to carry ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method, it is characterised in that by following step
Rapid preparation：
The synthesis of ethylbenzene hydrogen-based cage-type silsesquioxane；
ii）Sequentially add multi-vinyl silicone oil, metal oxide, PC610 inhibitor, Pt platinum catalysts, mechanical agitation mixing
Uniformly, 100 DEG C of vaccum dewatering 5h；Add above-mentioned preparation is dissolved in having containing ethylbenzene hydrogen-based cage-type silsesquioxane for toluene
Machine silicon crosslinking agent, the bubble being well mixed in rear low pressure removing system can be fully cured after being heat-treated 4h at 100 DEG C；
Reaction equation is as follows：
。
2. according to claim 1 a kind of with ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method,
Characterized in that, multi-vinyl silicone oil is methyl phenyl vinyl silicone oil, viscosity is 30200mPa s, and phenyl mass fraction is
55%, vinyl mass fraction is 3.6%.
3. according to claim 1 a kind of with ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method,
Characterized in that, metal oxide is Fe2O3、 CeO2、 ZnO、 TiO2、 V2O5, above-mentioned oxide is using individually one kind or two
More than kind, its granularity is 0.1～5 μm of scope.
4. according to claim 1 a kind of with ethylbenzene hydrogen-based cage-type silsesquioxane heat-resistant silicon rubber preparation method,
Characterized in that, octahydro base cage-type silsesquioxane and styrene press 1 in above-mentioned reaction：The mol ratio of n carries out reaction n=1,2,
3,4,5,6,7,8, different according to the mol ratio of reaction, the product such as number of above formula R bases and position is also different（Phenyl ring and hydrogen
The number of key is determined by cage modle octahydro base silsesquioxane and cinnamic mol ratio）, it is being n as silicone rubber crosslinking agent
In 8, so reaction equation is with mol ratio as 1:As a example by 1 reaction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610918247.0A CN106519701A (en) | 2016-10-21 | 2016-10-21 | Method for preparing heatproof silicone rubber having ethyl phenyl hydrogen-assisted cage-type silsesquioxane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610918247.0A CN106519701A (en) | 2016-10-21 | 2016-10-21 | Method for preparing heatproof silicone rubber having ethyl phenyl hydrogen-assisted cage-type silsesquioxane |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108913089A (en) * | 2018-07-23 | 2018-11-30 | 深圳天鼎新材料有限公司 | Two-component packaging plastic, preparation method and application method and application |
| CN110387054A (en) * | 2019-08-14 | 2019-10-29 | 北京化工大学 | A kind of preparation method of low-cost transparent hydridization silicon rubber |
| CN110536933A (en) * | 2017-04-26 | 2019-12-03 | 信越化学工业株式会社 | Addition curable silicone rubber compound |
| CN112888715A (en) * | 2018-10-18 | 2021-06-01 | 东亚合成株式会社 | Silsesquioxane derivative composition and use thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327273A (en) * | 2014-10-22 | 2015-02-04 | 上海大学 | Organic silicon potting adhesive containing POSS group and preparation method of organic silicon potting adhesive |
-
2016
- 2016-10-21 CN CN201610918247.0A patent/CN106519701A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327273A (en) * | 2014-10-22 | 2015-02-04 | 上海大学 | Organic silicon potting adhesive containing POSS group and preparation method of organic silicon potting adhesive |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110536933A (en) * | 2017-04-26 | 2019-12-03 | 信越化学工业株式会社 | Addition curable silicone rubber compound |
| CN110536933B (en) * | 2017-04-26 | 2022-04-01 | 信越化学工业株式会社 | Addition curing type silicone rubber composition |
| CN108913089A (en) * | 2018-07-23 | 2018-11-30 | 深圳天鼎新材料有限公司 | Two-component packaging plastic, preparation method and application method and application |
| CN112888715A (en) * | 2018-10-18 | 2021-06-01 | 东亚合成株式会社 | Silsesquioxane derivative composition and use thereof |
| CN112888715B (en) * | 2018-10-18 | 2023-11-03 | 东亚合成株式会社 | Silsesquioxane derivative composition and use thereof |
| CN110387054A (en) * | 2019-08-14 | 2019-10-29 | 北京化工大学 | A kind of preparation method of low-cost transparent hydridization silicon rubber |
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