CN106633064A - Preparation method for silicone rubber crosslinking agent with ethylbenzene hydrogen-based POSS (polyhedral oligomeric silsesquioxane) - Google Patents
Preparation method for silicone rubber crosslinking agent with ethylbenzene hydrogen-based POSS (polyhedral oligomeric silsesquioxane) Download PDFInfo
- Publication number
- CN106633064A CN106633064A CN201610837563.5A CN201610837563A CN106633064A CN 106633064 A CN106633064 A CN 106633064A CN 201610837563 A CN201610837563 A CN 201610837563A CN 106633064 A CN106633064 A CN 106633064A
- Authority
- CN
- China
- Prior art keywords
- crosslinking agent
- silicone rubber
- cage
- reaction
- hydrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
-
- 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
- C08G77/08—Preparatory processes characterised by the catalysts used
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method for a silicone rubber crosslinking agent with ethylbenzene hydrogen-based POSS (polyhedral oligomeric silsesquioxane), and relates to a preparation method of the rubber crosslinking agent. The preparation method comprises the following steps: synthesizing octahydridrosilsesquioxane T8H8; adding T8H8 in a reactor and dissolving T8H8 in a solvent, then adding styrene, adding a catalyst after stirring uniformly, vacuum-pumping for 15min, keeping a nitrogen atmosphere during the reaction process all the time, reacting for 24h at the temperature of 40 DEG C, and cooling to the room temperature after finishing the reaction, purifying and drying, and finally obtaining the product. The POSS containing benzene rings and further containing silicon hydrogen groups is prepared, the numbers of the benzene rings and silicon-hydrogen bonds are determined by a molar ratio of T8H8 to styrene, and a benzene ring structure is introduced in the POSS, so that the silicone rubber crosslinking agent can resist ultrahigh temperature.
Description
Technical field
The present invention relates to a kind of rubber crosslinker preparation method, more particularly to a kind of to carry ethylbenzene hydrogen-based cage model sesquialter
Siloxanes silicone rubber crosslinking agent preparation method.
Background technology
Silicon rubber has advantages below：Extremely wide use temperature range（- 100～250 DEG C）, hypotoxicity, height is thoroughly
Bright property, chemical inertness, splendid weatherability, good electrical insulating property etc..Single-component room-temperature-vulsilicone silicone rubber is due to using
It is convenient, without the need for hot setting, thus it is widely used in high temperature resistant element, with the development of Aeronautics and Astronautics technology, further carry
The heat resistance of high room temperature vulcanized silicone rubber becomes study hotspot.
At present conventional vinylsiloxane rubber crosslinking agent is containing hydrogen silicone oil, mostly straight chain type structure, gained colloid after solidification
Mechanical property is relatively low.Compared with the crosslinking agent of traditional silicon rubber-based products, cage-type silsesquioxane as crosslinking agent, due to cage modle
The introducing of silsesquioxane alkyl structure causes the silicone rubber kinds product after crosslinking to have higher heat resistance and mechanical property.
The content of the invention
It is an object of the invention to provide a kind of prepare with the agent of ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking
Method, the present invention synthesizes first the cage silsesquioxane structure containing si-h bond Yu phenyl ring simultaneously, and as silicon rubber
The crosslinking agent of glue is used, and successfully improves the combination property of silicon rubber.
The purpose of the present invention is achieved through the following technical solutions：
One kind carries ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation method, and methods described includes following step
Suddenly：
i）The synthesis of cage modle octahydro base silsesquioxane（T8H8）；
ii）Add cage modle octahydro base silsesquioxane to be dissolved in solvent in the reactor, add styrene, add after stirring
Enter catalyst, vacuumize 15min, nitrogen atmosphere is always maintained in course of reaction, 24h is reacted in reaction under the conditions of 40 DEG C, reacts
Room temperature is cooled to after end, drying is purified, product is finally obtained；Reaction equation is as follows：
。
Described one kind carries ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation method, and catalyst is Pt
Platinum catalyst.
Described one kind carries ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation method, and solvent is hexamethylene
Alkane or tetrahydrofuran.
Described one kind carries ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation method, in above-mentioned reaction
Octahydro base 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 reaction
Mol ratio is different, and the number of the R bases of product and position are also different（The number of phenyl ring and hydrogen bond is by cage modle octahydro base sesquialter silicon
Oxygen alkane and cinnamic mol ratio are determined）, it is n as silicone rubber crosslinking agent.
Advantages of the present invention is with effect：
The crosslinking agent cage-type silsesquioxane of the present invention is using cage modle hydrogen-based silsesquioxane and styrene as reactant, platinum
React under conditions of catalysis.The present invention is prepared not only containing phenyl ring but also containing the cage-type silsesquioxane of silicon hydrogen-based, phenyl ring and silicon
The number of hydrogen bond is determined by cage modle octahydro base silsesquioxane and cinnamic mol ratio, introduced on cage-type silsesquioxane
Benzene ring structure so as to which itself has the heat resisting temperature of superelevation.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Raw material removes specified otherwise in embodiment, is commercial.Ethylbenzene hydrogen-based cage-type silsesquioxane silicon in each embodiment
Rubber crosslinker is not repeated narration by the following manner gained.
By cage modle hydrogen-based silsesquioxane and styrene in molar ratio 1:4, accurately weigh cage modle hydrogen-based silsesquioxane and
Styrene monomer, in adding it to 100ml there-necked flasks, stirs.15min is vacuumized, nitrogen is always maintained in course of reaction
24h is reacted in gas atmosphere, reaction under the conditions of 40 DEG C, after reaction terminates, takes out product and is cooled to room temperature, purifies drying, finally
To product i.e. containing the cage-type silsesquioxane of ethylbenzene hydrogen-based.
Embodiment 1
Weigh 100 parts of vinylsiloxane rubber（Viscosity is 20000mPas）, add 30 parts of ethylbenzenes being dissolved in hexamethylene
Hydrogen-based cage-type silsesquioxane, with glass bar stirring it is mixed.It is put into vacuum drying chamber and vacuumizes de-bubble.Then, add
0.2 part of PC610 inhibitor, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, the white carbon that 10 parts of silane couplers were processed.Glass
Glass rod 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, places into room
Under warm environment, a period of time is placed, until silicon rubber becomes the elastomer for having certain degree of hardness.According to GB/T 13477.6-2002
The performance of test gained cured glue body：Elongation at break is 170%, draws high intensity for 2.1MPa.Temperature of initial decomposition is 420.
1℃。
Embodiment 2
Weigh 100 parts of vinylsiloxane rubber（Viscosity is 20000mPas）, add 40 parts of ethylbenzenes being dissolved in hexamethylene
Hydrogen-based cage-type silsesquioxane, with glass bar stirring it is mixed.It is put into vacuum drying chamber and vacuumizes de-bubble.Then, add
0.2 part of PC610 inhibitor, 5 parts of nano tin dioxides, 5 parts of nano-cerium oxides, the white carbon that 10 parts of silane couplers were processed.Glass
Glass rod 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, places into room
Under warm environment, a period of time is placed, until silicon rubber becomes the elastomer for having certain degree of hardness.According to GB/T 13477.6-2002
The performance of test gained cured glue body：Elongation at break is 200%, draws high intensity for 2.7MPa.Temperature of initial decomposition is 435.
3℃。
From data above, the present invention provides a kind of not only cage-type silsesquioxane containing phenyl ring but also containing silicon hydrogen-based and makees
For crosslinking agent（The number of phenyl ring and si-h bond is determined by cage modle octahydro base silsesquioxane and cinnamic mol ratio）, made with it
The standby silicon rubber for having obtained heat resistance and good mechanical properties.
Claims (4)
1. it is a kind of to carry ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation method, it is characterised in that the side
Method is comprised the following steps：
The synthesis of cage modle octahydro base silsesquioxane（T8H8）；
Add cage modle octahydro base silsesquioxane to be dissolved in solvent in the reactor, add styrene, be stirring evenly and then adding into
Catalyst, vacuumizes 15min, and nitrogen atmosphere is always maintained in course of reaction, and 24h, reaction knot are reacted in reaction under the conditions of 40 DEG C
Room temperature is cooled to after beam, drying is purified, product is finally obtained；Reaction equation is as follows：
。
2. according to claim 1 a kind of with ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation side
Method, it is characterised in that catalyst is Pt platinum catalysts.
3. according to claim 1 a kind of with ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation side
Method, it is characterised in that solvent is hexamethylene or tetrahydrofuran.
4. according to claim 1 a kind of with ethylbenzene hydrogen-based cage-type silsesquioxane silicone rubber crosslinking agent preparation side
Method, it is characterised 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 number of R bases and position are also different in product（Phenyl ring and hydrogen bond
Number determined by cage modle octahydro base silsesquioxane and cinnamic mol ratio）, it is n as silicone rubber crosslinking agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610837563.5A CN106633064A (en) | 2016-09-21 | 2016-09-21 | Preparation method for silicone rubber crosslinking agent with ethylbenzene hydrogen-based POSS (polyhedral oligomeric silsesquioxane) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610837563.5A CN106633064A (en) | 2016-09-21 | 2016-09-21 | Preparation method for silicone rubber crosslinking agent with ethylbenzene hydrogen-based POSS (polyhedral oligomeric silsesquioxane) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106633064A true CN106633064A (en) | 2017-05-10 |
Family
ID=58852481
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610837563.5A Withdrawn CN106633064A (en) | 2016-09-21 | 2016-09-21 | Preparation method for silicone rubber crosslinking agent with ethylbenzene hydrogen-based POSS (polyhedral oligomeric silsesquioxane) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106633064A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101397309A (en) * | 2008-11-04 | 2009-04-01 | 东华大学 | Transporting material containing POSS hybrid electron and preparation method thereof |
| CN101397308A (en) * | 2008-11-04 | 2009-04-01 | 东华大学 | POSS hybrid hole-transporting material and preparation method thereof |
| CN104282428A (en) * | 2013-07-10 | 2015-01-14 | 天津工业大学 | Method for preparing magnetic POSS |
| 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
- 2016-09-21 CN CN201610837563.5A patent/CN106633064A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101397309A (en) * | 2008-11-04 | 2009-04-01 | 东华大学 | Transporting material containing POSS hybrid electron and preparation method thereof |
| CN101397308A (en) * | 2008-11-04 | 2009-04-01 | 东华大学 | POSS hybrid hole-transporting material and preparation method thereof |
| CN104282428A (en) * | 2013-07-10 | 2015-01-14 | 天津工业大学 | Method for preparing magnetic POSS |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106432728B (en) | A kind of pheiiyldimetliyl siloxy cage-type silsesquioxane silicone rubber crosslinking agent and preparation method thereof | |
| CN101768363A (en) | Method for preparing addition highly heat-conducting room temperature-curing silicon rubber | |
| CN107353871A (en) | A kind of high temperature resistant adhering and sealing silicones and preparation method thereof | |
| CN105802237B (en) | Heat-conducting silica gel composition, heat-conducting silica gel and preparation method thereof | |
| CN105778104B (en) | A kind of add-on type liquid fluorine silicon rubber base glue and preparation method thereof | |
| CN109880585A (en) | A kind of liquid silastic and preparation method thereof of pair of selective bonding of plastic basis material | |
| CN106479189B (en) | A kind of silicon rubber of the three silylation cage-type silsesquioxane containing phenyl | |
| CN106519237A (en) | Diphenyl siloxy polyhedral oligomeric silsesquioxane silicone rubber cross-linking agent and preparation method thereof | |
| CN106433146A (en) | Room-temperature vulcanization heat-resistant silicon rubber with active hydrogen based cage structure and preparation method thereof | |
| CN105837617A (en) | Preparation and application of trifluorovinyl-ether-containing cyclosiloxane capable of direct heat curing | |
| Guo et al. | Luminescent and robust perovskite–silicone elastomers prepared by light induced thiol–ene reaction | |
| CN105669980B (en) | A kind of alpha, omega end vinyl silicone oil of phenyl-fluoride hydrocarbon backbone boracic and preparation method thereof | |
| CN106519701A (en) | Method for preparing heatproof silicone rubber having ethyl phenyl hydrogen-assisted cage-type silsesquioxane | |
| CN107446356B (en) | A kind of heat resistant transparent add-on type liquid silicon rubber and preparation method thereof | |
| CN106317411A (en) | Diphenyl trisiloxane cage type silsesquioxane organic silicon crosslinking agent and preparation method thereof | |
| CN106497075A (en) | A kind of silicone rubber of the base of trisiloxanes containing diphenyl cage-type silsesquioxane and preparation method thereof | |
| JP6373148B2 (en) | Silicone porous body and method for producing silicone porous body | |
| CN106519233A (en) | Dibenzyl tetrasiloxane cage-like silsesquioxane organosilicon cross-linking agent and preparation method thereof | |
| CN106633064A (en) | Preparation method for silicone rubber crosslinking agent with ethylbenzene hydrogen-based POSS (polyhedral oligomeric silsesquioxane) | |
| CN108164705A (en) | A kind of odorlessness add-on type liquid silicon rubber tackifier and its preparation method and application | |
| CN106800781A (en) | One kind is used（Tetraphenyl）Silicon rubber prepared by phenethyl POSS heat resistance accessories | |
| CN106810874A (en) | A kind of silicon rubber of use itrile group POSS auxiliary agents synthesis | |
| TW201809146A (en) | Formulation containing a metal aprotic organosilanoxide compound | |
| JPH0616812A (en) | Trifunctional hydrogenated siloxane fluid | |
| CN106633072A (en) | Preparation method of diphenyl siloxyl cage type silsesquioxane heat-resisting silicone rubber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170510 |
|
| WW01 | Invention patent application withdrawn after publication |