CN106750306A - A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent and preparation method thereof - Google Patents
A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent and preparation method thereof Download PDFInfo
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- CN106750306A CN106750306A CN201611142684.4A CN201611142684A CN106750306A CN 106750306 A CN106750306 A CN 106750306A CN 201611142684 A CN201611142684 A CN 201611142684A CN 106750306 A CN106750306 A CN 106750306A
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- crosslinking agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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Abstract
A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent and preparation method thereof, is related to a kind of rubber crosslinker and preparation method thereof, and the present invention has synthesized a kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent.It obtains phenyl three (dimethyl siloxane) trimethoxy silane by (dimethyl siloxane) silane of phenyl three and vinyltrimethoxy silane reaction first, pheiiyldimetliyl siloxy cage-type silsesquioxane is being prepared by hydrolysis-condensation reaction, it can be as vinylsiloxane rubber and the crosslinking agent of silicones, compared with common crosslinking agent, this kind of crosslinking agent makes silicon rubber have heat resisting temperature and good mechanical property higher due to own structural characteristics.
Description
Technical field
The present invention relates to a kind of rubber crosslinker and preparation method thereof, more particularly to a kind of pheiiyldimetliyl siloxy cage
Type silsesquioxane silicone rubber crosslinking agent and preparation method thereof.
Background technology
Silicon rubber is, with linear polysiloxane as primary raw material, to add reinforcing material, crosslinking agent and other cooperation drug, solidification
Elastomer, polysiloxane molecule chain is alternately made up of silicon atom and oxygen atom, and silicon oxygen bond bond energy is 443KJ/mol, and
C-C keys bond energy is 335KJ/mol, so organosilicon product heat endurance is high, under such as General Purpose Rubber intensity is raised rapidly with temperature
Drop, and silicon rubber almost can be used forever at 150 DEG C again, it is seen that., compared with General Purpose Rubber, temperature tolerance is most prominent silicon rubber
One of premium properties for going out, therefore it is used for high temperature applicationss.With the progress of science and technology, the particularly hair of national defence and sophisticated technology
Exhibition, the heat resistance to silicon rubber proposes requirement higher, thus it is that silicon rubber grinds to improve the temperature in use of silicon rubber and life-span
One of focus studied carefully.
Start with from crosslinking agent, current silastic elastomer is as crosslinking agent, due to its straight chain type typically using containing hydrogen silicone oil
Structure causes the silicon rubber heat-resisting temperature after solidification, mechanical property to tend not to meet operation requirement.And cage-type silsesquioxane
(POSS), its general molecular formula is（RSiO3/2）n.It is organic-inorganic nanocomposite materials that latest development is got up, with excellent
Thermal stability and mechanical property, being added in the middle of silicon rubber as crosslinking agent can successfully improve the thermally-stabilised of silicon rubber
Property and mechanical property.
The content of the invention
It is an object of the invention to provide a kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent and
Its preparation method, crosslinking agent prepared by the present invention also introduces benzene on the basis of cage-type silsesquioxane inorganic skeleton is introduced
Ring, two kinds of structures mutually act synergistically, and substantially increase silicon rubber heat-resisting temperature and mechanical property..
The purpose of the present invention is achieved through the following technical solutions：
A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent, the crosslinking agent structure is as follows：
A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent preparation method, methods described is by following steps
Composition：
i）(dimethyl siloxane) silane of phenyl three and vinyltrimethoxy silane are entered under the catalytic action of chloroplatinic acid
Row hydrosilylation, reaction is completed under the conditions of 40 DEG C, and low pressure removes unreacted reactant after the completion of reaction, and reaction equation is as follows：
ii）Methyl alcohol and concentrated hydrochloric acid are added in there-necked flask, at ambient temperature, stirring in water bath 30min is passed through N2, then slow drop
Plus the product of above-mentioned steps, continue to stir after completion of dropwise addition；Reaction is washed after terminating with methyl alcohol, suction filtration, after vacuum drying
Obtain solid powdery product；
iii）Reaction equation is as follows：
A kind of described pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent preparation method, in above-mentioned reaction,
Reaction time is 24~48h.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Raw material removes specified otherwise in embodiment, is purchased in market.
Pheiiyldimetliyl siloxy cage-type silsesquioxane is not repeated to chat by the following manner gained in each embodiment
State.
By the vinyltrimethoxy silane of (dimethyl siloxane) silane of phenyl three of 40ml and 10ml in chloroplatinic acid
Catalytic action under carry out hydrosilylation, reaction can be completed under the conditions of 40 DEG C, and low pressure removes not anti-after the completion of reaction
Answer thing.
20ml methyl alcohol and 10ml concentrated hydrochloric acids will be added in there-necked flask, at ambient temperature, stirring in water bath 30min is passed through
N2It is slowly added dropwise the product of 10ml above-mentioned steps again afterwards, continues to stir 48h after completion of dropwise addition.Reaction is washed after terminating with methyl alcohol
Wash, suction filtration, solid powdery product pheiiyldimetliyl siloxy cage-type silsesquioxane is obtained after vacuum drying.
Embodiment 1
Weigh 100 parts of vinylsiloxane rubber（Viscosity is 20000mPas）, add 30 parts of phenyl two being dissolved in hexamethylene
Methyl siloxy cage-type silsesquioxane, being stirred with glass bar mixes it.It is put into vacuum drying chamber and vacuumizes de-bubble.So
Afterwards, 0.2 part of PC610 inhibitor is added, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, treated white of 10 parts of silane couplers
Carbon black.Glass bar adds 0.5 part of platinum catalyst after stirring and evenly mixing, and is put into after stirring evenly in vacuum drying chamber and vacuumizes de-bubble, then
Put under room temperature environment, place a period of time, until silicon rubber turns into the elastomer for having certain degree of hardness.According to GB/T
The performance of 13477.6-2002 test gained cured glue bodies：Elongation at break is 190%, draws high intensity for 2.2MPa.Initial point
Solution temperature is 423. 1 DEG C.
Embodiment 2
Weigh 100 parts of vinylsiloxane rubber（Viscosity is 20000mPas）, add 40 parts of phenyl two being dissolved in hexamethylene
Methyl siloxy cage-type silsesquioxane, being stirred with glass bar mixes it.It is put into vacuum drying chamber and vacuumizes de-bubble.So
Afterwards, 0.2 part of PC610 inhibitor of addition, 5 parts of nano tin dioxides, 5 parts are received
Rice cerium oxide, the treated white carbon of 10 parts of silane couplers.Glass bar adds 0.5 part of platinum catalysis after stirring and evenly mixing
Agent, is put into vacuum drying chamber after stirring evenly and vacuumizes de-bubble, places under room temperature environment, a period of time is placed, until silicon rubber
Glue turns into the elastomer for having certain degree of hardness.The performance of gained cured glue body is tested according to GB/T 13477.6-2002：Fracture is stretched
Rate long is 210%, draws high intensity for 2.9MPa.Temperature of initial decomposition is 437. 3 DEG C.
From data above, the present invention provides pheiiyldimetliyl siloxy cage-type silsesquioxane as crosslinking agent, by
Addition reaction can be carried out with silicon rubber medium vinyl double bond containing si-h bond in its structure, the crosslinking that improve silicon rubber is close
Degree, introduces benzene ring structure again, and two kinds of factor collective effects have obtained the silicon rubber of heat resistance and good mechanical properties.
Claims (3)
1. a kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent, it is characterised in that the crosslinking agent knot
Structure is as follows：
。
2. a kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent preparation method, it is characterised in that described
Method is comprised the steps of：
i）(dimethyl siloxane) silane of phenyl three and vinyltrimethoxy silane are entered under the catalytic action of chloroplatinic acid
Row hydrosilylation, reaction is completed under the conditions of 40 DEG C, and low pressure removes unreacted reactant after the completion of reaction, and reaction equation is as follows：
ii）Methyl alcohol and concentrated hydrochloric acid are added in there-necked flask, at ambient temperature, stirring in water bath 30min is passed through N2, then be slowly added dropwise
The product of above-mentioned steps, continues to stir after completion of dropwise addition；Reaction is washed after terminating with methyl alcohol, suction filtration, after vacuum drying
To solid powdery product；
iii）Reaction equation is as follows：
。
3. a kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent preparation side according to claim 2
Method, it is characterised in that in above-mentioned reaction, the reaction time is 24~48h.
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|---|---|---|---|
| CN201611142684.4A CN106750306A (en) | 2016-12-13 | 2016-12-13 | A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent and preparation method thereof |
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| CN201611142684.4A CN106750306A (en) | 2016-12-13 | 2016-12-13 | A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109679104A (en) * | 2018-12-10 | 2019-04-26 | 沈阳化工大学 | A kind of eight amino pyrene propyl cage-type silsesquioxane silicon rubber heat-resisting auxiliary agents |
| CN110776748A (en) * | 2019-09-18 | 2020-02-11 | 宁波泰意德过滤技术有限公司 | Addition type fluorosilicone rubber and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106432728A (en) * | 2016-09-21 | 2017-02-22 | 沈阳化工大学 | Phenyl(dimethylsiloxy) cage type silsesquioxane silicone rubber crosslinking agent and preparation method thereof |
-
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- 2016-12-13 CN CN201611142684.4A patent/CN106750306A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106432728A (en) * | 2016-09-21 | 2017-02-22 | 沈阳化工大学 | Phenyl(dimethylsiloxy) cage type silsesquioxane silicone rubber crosslinking agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109679104A (en) * | 2018-12-10 | 2019-04-26 | 沈阳化工大学 | A kind of eight amino pyrene propyl cage-type silsesquioxane silicon rubber heat-resisting auxiliary agents |
| CN110776748A (en) * | 2019-09-18 | 2020-02-11 | 宁波泰意德过滤技术有限公司 | Addition type fluorosilicone rubber and preparation method thereof |
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