CN106520063A - Heat-resistant adhesive containing phenanthrenyl(polyphenyl)phenyl structure and preparation method thereof - Google Patents
Heat-resistant adhesive containing phenanthrenyl(polyphenyl)phenyl structure and preparation method thereof Download PDFInfo
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- CN106520063A CN106520063A CN201610919633.1A CN201610919633A CN106520063A CN 106520063 A CN106520063 A CN 106520063A CN 201610919633 A CN201610919633 A CN 201610919633A CN 106520063 A CN106520063 A CN 106520063A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a heat-resistant adhesive containing a phenanthrenyl(polyphenyl)phenyl structure and a preparation method thereof and relates to a heat-resistant adhesive and a preparation method thereof. In the invention, benzene ring-containing methylvinyl silicone oil is adopted for the adhesive body, and the adhesive has good heat resistance and mechanical property; through molecular design, a liquid silicon-containing compound with a condensed ring structure is synthesized and added into the system as a heat-resistant aid of the silicone rubber adhesive, thus the heat resistance of the adhesive can be improved, and good compatibility with a silicone rubber matrix as well as processing property can be realized; and with the addition of the aid, the heat energy can be absorbed first when a silica gel material is heated, and the breakage of the main-chain chemical bond of the matrix material is avoided so as to protect the matrix material. The obtained adhesive can be used in a short period at a high temperature of 420 DEG C and in a long period at a high temperature of 350 DEG C. The silicone rubber adhesive disclosed by the invention can resist a temperature over 400 DEG C and also has good mechanical properties.
Description
Technical field
The present invention relates to a kind of heat-resistant adhesive and preparation method thereof, more particularly to a kind of containing luxuriant and rich with fragrance formula（Many phenyl）Benzene
Heat-resistant adhesive of based structures and preparation method thereof.
Background technology
As the unique structure of organosilicon has excellent weatherability, durability, resistant of high or low temperature, hydrophobicity, uvioresistant
Beta radiation and elastic cementing ability, even if remaining to keep in harsh use environment good physical property, thus it is extensive
The fields such as building, electronic apparatus, automobile, new forms of energy and the consumer goods are applied to as sealant, its remarkable performance section is offset
Fancy price.The low surface tension of organosilicon makes which become excellent release material again.In food, packaging, building, vapour
Organic silicon adhesive is widely used in the fields such as car, electronics, mechanograph, becomes indispensable new in national defence and national economy
Macromolecular material.But while there is the shortcomings of hardness is low, flame resistance is poor, price is higher in organosilicon.With the development of society, compel
It is essential and will develops the high silicone rubber adhesive of a kind of high temperature resistant, shear strength.Therefore, work out a kind of having for high-adhesion energy
Machine silicone sealant is necessary.
Some preparation methods with regard to high-temperature-resistant adhesive are disclosed in foreign patent, mainly from adhesive and structure design
Solve the above problems in terms of two, the adhesive for using there are the kinds such as resistant, toughened polyimides, high resiliency organic silicon adhesive,
But crucial additive synthesis difficulty and cumbersome, it is difficult to grasp；It is domestic that there is elastomeric high-temperature plastic kind seldom, its
So that the requirement in most of fields can not be met in mechanical property.High temperature resistant to be realized, high resiliency, low viscous material property, only
There is the high-temperature-resisting organic silicon rubber adhesive containing special construction to be possible to realize.
Chinese patent CN200610036843.2 reports the silicone rubber formulations with heat resistance, by adding iron oxide
The heat-resisting additives such as red or mixed rare-earth oxide, the glued membrane after sulfuration are only limited within 300 DEG C using temperature, in higher temperature
Degree cannot then meet requirement under requiring.
103289414 A of Chinese patent CN disclose a kind of room temperature silicon sulfide rubber composition of heat-proof combustion-resistant, its shortcoming
It is that after solidification, cubical contraction is larger using condensed type silicon rubber, it is impossible to meet requirement of the special dimension to adhesive.
Paper《The synthesis of the polysiloxanes containing condensed ring side chain and its shadow to Addition-type Heat Curable Silicone Rubber Compound performance
Ring》Condensed cyclic structure is introduced on the silicon rubber of methyl blocking, the heat resisting temperature of silicon rubber is successfully improve, but due to strand
Two ends do not have vinyl active group, and condensed cyclic structure can only be incorporated in side chain, and which affects unobvious to heat-resisting effect.
The content of the invention
It is an object of the invention to provide a kind of containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive of phenyl structure and its preparation
Method, colloid main body inherently have excellent heat resistance and mechanical property concurrently from the methyl vinyl silicon oil containing phenyl ring class
Energy；Add the liquid silicon-containing compound containing condensed cyclic structure, as heat resistance accessory addition system in so as to further improve viscous
The heat-resisting function of mixture, and can and the compatibility that have of silicone rubber matrix and processability.
The purpose of the present invention is achieved through the following technical solutions：
It is a kind of to contain luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive of phenyl structure, is made up of by weight following components：
100 parts of methyl phenyl vinyl silicone oil；
The hydrogeneous crosslinking agent 10-30 parts of phenyl；
Acenaphthene formula（Many phenyl）1 ~ 20 weight portion of phenyl-vinyl silicon oil；
1 ~ 10 part of metal oxide；
0.1～20 weight portion of catalyst；
0.1～10 weight portion of tackifier.
It is described containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive of phenyl structure, the methyl phenyl vinyl silicone oil glue
Spend for 15000mPa s ~ 50000mPa s, phenyl mass fraction is 5% ~ 55%, vinyl mass fraction is 0.1% ~ 5%.
It is described containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive of phenyl structure, the hydrogeneous crosslinking agent of the phenyl contain for phenyl
One or more in hydrogen silicone oil and phenyl-based hydrogen-based silicone resin, viscosity are 100 mPa s ~ 2000 mPa s, and hydrogen content is
0.1%~1%。
Containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, methods described synthesis step are as follows：
（1）10.6 gram two is added in 500 milliliters of three neck round bottom flask equipped with stirring, reflux condenser and constant pressure funnel
Benzyl ketone, 10.0 grams of phenanthrenequione and 100 milliliters of absolute ethyl alcohols, after heating is completely dissolved ethanol micro-boiling, question response thing, Xiang Sankou
The ethanol solution (3.0 grams of KOH are dissolved in 15 milliliters of absolute ethyl alcohols) of 8 milliliters of KOH, and logical N is slowly added dropwise in flask2Protection；
Solution is gradually switched to blackish green by yellow, is further continued for being heated to reflux terminating reaction after 15 minutes；0 DEG C is cooled to, suction filtration, then often
It is secondary to use 15 milliliter of 95% ethanol to wash precipitation three times, it is put in baking oven and dries, finally obtains black powder solid：Luxuriant and rich with fragrance formula ring penta 2
Ketenes；
（2）Luxuriant and rich with fragrance formula（Many phenyl）Phenyl-vinyl silicon oil can be by the vinyl on the multi-vinyl silicone oil of ethenyl blocking and phenanthrene
Formula cyclopentadienone carries out Diels-Alder reactions to synthesize；In the there-necked flask equipped with backflow and agitating device, ethene is added
The multi-vinyl silicone oil 30g (containing Vi0.015mol) of base end-blocking, luxuriant and rich with fragrance formula cyclopentadienone about 3.9g (0.01mol), add α-
Chloronaphthalene 30ml. is in N2In atmosphere, agitating heating flows back 10 hours；Reaction is by blackish green yellowing clear solution. solution after cooling
Layering, upper strata is product, and lower floor is solvent；Methyl alcohol washed product, till methyl alcohol is water white transparency；150 DEG C of product Jing does
Dry 5 hours, obtain many phenyl vinyl silicone oils of luxuriant and rich with fragrance formula.
It is described containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, the luxuriant and rich with fragrance formula（Many phenyl）Benzene
Base vinyl silicone oil structure is as follows：
。
It is described containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, the metal oxide are oxygen
Change iron, tin oxide, titanium oxide, zinc oxide, one or more in cerium oxide, granularity are 20nm ~ 30um.
It is described containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, the catalyst is
Karstedt platinum catalysts, content are 3000 ~ 5000ppm.
It is described containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, the tackifier are modified ring
Oxygen class tackifier.
It is described containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, above-mentioned all experimental drugs are equal
Through dehydration technology process, molecular sieve preservation is put into afterwards.
Advantages of the present invention with effect is：
Colloid main body of the present invention inherently has excellent heat resistance and power concurrently from the methyl vinyl silicon oil containing phenyl ring class
Learn performance；Secondly by MOLECULE DESIGN, synthesize a kind of liquid silicon-containing compound containing condensed cyclic structure, bond as silicon rubber
In the heat resistance accessory addition system of agent so as to the heat resistance of adhesive can be improved, and can be compatible with what silicone rubber matrix had had
Property and processability；With the addition of auxiliary agent, can be when silica gel material be heated, preferential absorption thermal energy, it is to avoid matrix material
The fracture of material backbone chemistry key, so that play protect the substrate material effects.The adhesive for finally giving can be short under 420 DEG C of high temperature
Phase uses, Long-Time Service under 350 DEG C of high temperature.
Description of the drawings
Fig. 1 is the synthetic reaction equation of luxuriant and rich with fragrance formula cyclopentadienone；
Fig. 2 is luxuriant and rich with fragrance formula（Many phenyl）The synthetic reaction equation of phenyl-vinyl silicon oil.
Specific embodiment
The present invention is further described with reference to specific embodiment, but does not limit the invention to these tools
Body embodiment.One skilled in the art would recognize that present invention encompasses being potentially included in Claims scope
All alternatives, improvement project and equivalents.
Water process is removed through low pressure before medicine experiment used in following examples, and be put into molecular sieve sealing preserve, with
Prevent moisture from impacting to silicone rubber adhesive solidification process.Each embodiment China and Philippines formula（Many phenyl）Phenyl-vinyl silicon oil is equal
By obtained by the following manner, narration is not repeated.
（1）10.6 are added in 500 milliliters of three neck round bottom flask equipped with stirring, reflux condenser and constant pressure funnel
Gram dibenzyl ketone, 10.0 grams of phenanthrenequione and 100 milliliters of absolute ethyl alcohols, after heating is completely dissolved ethanol micro-boiling, question response thing, to
The ethanol solution (3.0 grams of KOH are dissolved in 15 milliliters of absolute ethyl alcohols) of 8 milliliters of KOH, and logical N is slowly added dropwise in there-necked flask2Protect
Shield.Solution is gradually switched to blackish green by yellow, is further continued for being heated to reflux terminating reaction after 15 minutes.0 DEG C is cooled to, suction filtration, so
Washed with 15 milliliter of 95% ethanol every time afterwards and precipitated three times, dried in being put into baking oven, finally obtain black powder solid：Luxuriant and rich with fragrance formula ring
Pentadienone.
（The many phenyl vinyl silicone oils of 2 luxuriant and rich with fragrance formulas can by the vinyl on the multi-vinyl silicone oil of ethenyl blocking and
Luxuriant and rich with fragrance formula cyclopentadienone carries out Diels-Alder reactions to synthesize.In the there-necked flask equipped with backflow and agitating device, second is added
The multi-vinyl silicone oil 30g (containing Vi0.04mol) of thiazolinyl end-blocking, luxuriant and rich with fragrance formula cyclopentadienone about 3.9g (0.01mol), add α-
Chloronaphthalene 30ml. is in N2In atmosphere, agitating heating flows back 10 hours.Reaction is by blackish green yellowing clear solution. solution after cooling
Layering, upper strata is product, and lower floor is solvent. methyl alcohol washed product is used, till methyl alcohol is water white transparency.150 DEG C of product Jing
It is dried 5 hours, obtains many phenyl vinyl silicone oils of luxuriant and rich with fragrance formula.
Embodiment 1
100 parts of methyl phenyl vinyl silicone oils（Viscosity is 30200mPa s, and phenyl mass fraction is 55%, vinyl quality point
Number is 3.6%）, 10 parts of luxuriant and rich with fragrance formulas（Many phenyl）Phenyl-vinyl silicon oil, 2 parts of tackifier (commercially available), 4 parts of nano tin dioxides, 0.5 part
Karstedt platinum catalysts (5000ppm), mechanical agitation is well mixed, then with planetary mixer stir 2h, last 100 DEG C
Vaccum dewatering 5h.Add the hydrogeneous crosslinking agent of 51 parts of phenyl（Viscosity is 2500mPa s, and phenyl mass fraction is 37.5%, hydrogeneous
Amount 0.34%）, the bubble being well mixed in rear low pressure removing system；Can be fully cured after 4h is heat-treated at 100 DEG C.Press
The performance of gained cured glue body is tested according to GB/T 13477.6-2002：Elongation at break is 212%, draws high intensity and is
3.8Mpa.Temperature of initial decomposition is 417. 9 DEG C.According to GB/T7124-2008 test gained, normal temperature tensile shear strength（Steel-
Steel）For 1.84MPa, 400 DEG C of heat treatment, one hour after-drawing shear strength（Steel-steel）For 0.6MPa.
Embodiment 2
100 parts of methyl phenyl vinyl silicone oils（Viscosity is 30200mPa s, and phenyl mass fraction is 55%, vinyl quality point
Number is 3.6%）, 10 parts of luxuriant and rich with fragrance formulas（Many phenyl）Phenyl-vinyl silicon oil, 2 parts of tackifier (commercially available), 4 parts of nano tin dioxides, 5 parts
Nano-cerium oxide, 0.5 part of Karstedt platinum catalyst (5000ppm), mechanical agitation is well mixed, then uses planetary mixer
Stirring 3h, last 100 DEG C of vaccum dewatering 5h.Add the hydrogeneous crosslinking agent of 51 parts of phenyl（Viscosity be 2500mPa s, phenyl quality
Fraction is 37.5%, hydrogen content 0.34%）, the bubble being well mixed in rear low pressure removing system；After 4h is heat-treated at 100 DEG C
Can be fully cured.The performance of gained cured glue body is tested according to GB/T 13477.6-2002：Elongation at break is 198%,
Intensity is drawn high for 3.3Mpa.Temperature of initial decomposition is 436. 5 DEG C.According to GB/T7124-2008 test gained, normal temperature stretching is cut
Shearing stress（Steel-steel）For 1.71MPa, 400 DEG C of heat treatment, one hour after-drawing shear strength（Steel-steel）For 0.7MPa.
Embodiment 3
100 parts of methyl phenyl vinyl silicone oils（Viscosity is 15000mPa s, and phenyl mass fraction is 25%, vinyl quality point
Number is 1.8%）, 10 parts of luxuriant and rich with fragrance formulas（Many phenyl）Phenyl-vinyl silicon oil, 2 parts of tackifier (commercially available), 4 parts of nano tin dioxides, 0.5
Part Karstedt platinum catalysts (5000ppm), mechanical agitation is well mixed, then stirs 2h with planetary mixer, and last 100
DEG C vaccum dewatering 5h.Add the hydrogeneous crosslinking agent of 25 parts of phenyl（Viscosity is 2500mPa s, and phenyl mass fraction is 37.5%, is contained
Hydrogen amount 0.34%）, the bubble being well mixed in rear low pressure removing system；Can be fully cured after 4h is heat-treated at 100 DEG C.
The performance of gained cured glue body is tested according to GB/T 13477.6-2002：Elongation at break is 237%, draws high intensity and is
2.5Mpa.Temperature of initial decomposition is 409. 5 DEG C.According to GB/T7124-2008 test gained, normal temperature tensile shear strength（Steel-
Steel）For 1.88MPa, 400 DEG C of heat treatment, one hour after-drawing shear strength（Steel-steel）For 0.6MPa.
Embodiment 4
100 parts of methyl phenyl vinyl silicone oils（Viscosity is 15000mPa s, and phenyl mass fraction is 25%, vinyl quality point
Number is 1.8%）, 10 parts of luxuriant and rich with fragrance formulas（Many phenyl）Phenyl-vinyl silicon oil, 2 parts of tackifier (commercially available), 4 parts of nano tin dioxides, 0.5
Part Karstedt platinum catalysts (5000ppm), mechanical agitation is well mixed, then stirs 2h with planetary mixer, and last 100
DEG C vaccum dewatering 5h.Add the hydrogeneous crosslinking agent of 17 parts of phenyl（Viscosity is 150mPa s, and phenyl mass fraction is 30%, hydrogeneous
Amount 0.5%）, the bubble being well mixed in rear low pressure removing system；Can be fully cured after 2h is heat-treated at 80 DEG C.According to
The performance of GB/T 13477.6-2002 test gained cured glue bodies：Elongation at break is 219%, draws high intensity for 2.1Mpa.
Temperature of initial decomposition is 400. 8 DEG C.According to GB/T7124-2008 test gained, normal temperature tensile shear strength（Steel-steel）For
1.26MPa, 400 DEG C of heat treatment, one hour after-drawing shear strength（Steel-steel）For 0.5MPa.
Embodiment 5
100 parts of methyl phenyl vinyl silicone oils（Viscosity is 38000mPa s, and phenyl mass fraction is 10%, vinyl quality point
Number is 0.3%）, 10 parts of luxuriant and rich with fragrance formulas（Many phenyl）Phenyl-vinyl silicon oil, 2 parts of tackifier (commercially available), 4 parts of nano tin dioxides, 0.5
Part Karstedt platinum catalysts (5000ppm), mechanical agitation is well mixed, then stirs 2h with planetary mixer, and last 100
DEG C vaccum dewatering 5h.Add the hydrogeneous crosslinking agent of 5 parts of phenyl（Viscosity is 2500mPa s, and phenyl mass fraction is 37.5%, is contained
Hydrogen amount 0.34%）, the bubble being well mixed in rear low pressure removing system；Can be fully cured after 4h is heat-treated at 100 DEG C.
The performance of gained cured glue body is tested according to GB/T 13477.6-2002：Elongation at break is 343%, draws high intensity and is
2.6Mpa.Temperature of initial decomposition is 411. 2 DEG C.According to GB/T7124-2008 test gained, normal temperature tensile shear strength（Steel-
Steel）For 1.7MPa, 400 DEG C of heat treatment, one hour after-drawing shear strength（Steel-steel）For 0.4MPa.
Can be obtained by 5 embodiment contrasts, with the raising of metal oxide addition, the heat resistance of adhesive has been carried
Height, but mechanical property declines therewith；The change of methyl phenyl vinyl silicone oil viscosity can affect the machinability of colloid, viscosity
I.e. molecular weight is big greatly, and mechanical property is relatively preferable, but gradually complicated using technique；Use the small molecule crosslinking agent can be so that colloid is consolidated
Change is faster and low to temperature requirement, but the mechanical property after the big crosslinking agent solidification of viscosity, heat resistance are more preferable.In sum,
According to the difference of practical application condition, corresponding formula may be selected.Above-mentioned specific embodiment is exemplary, be in order to
Preferably make skilled artisans appreciate that this patent, it is impossible to be not understood as including this patent the restriction of scope；As long as
It is any equivalent change made or modification of the spirit according to disclosed in this patent, each falls within the scope that this patent includes.
Claims (9)
1. a kind of containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive of phenyl structure, it is characterised in that by following components by weight
Meter composition：
100 parts of methyl phenyl vinyl silicone oil；
The hydrogeneous crosslinking agent 10-30 parts of phenyl；
Acenaphthene formula（Many phenyl）1 ~ 20 weight portion of phenyl-vinyl silicon oil；
1 ~ 10 part of metal oxide；
0.1～20 weight portion of catalyst；
0.1～10 weight portion of tackifier.
2. according to claim 1 containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive of phenyl structure, it is characterised in that described
Methyl phenyl vinyl silicone oil, viscosity are 15000mPa s ~ 50000mPa s, and phenyl mass fraction is 5% ~ 55%, vinyl
Mass fraction is 0.1% ~ 5%.
3. according to claim 1 containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive of phenyl structure, it is characterised in that described
The hydrogeneous crosslinking agent of phenyl be phenyl hydrogen-containing silicon oil and phenyl-based hydrogen-based silicone resin in one or more, viscosity be 100 mPa s ~
2000 mPa s, hydrogen content are 0.1% ~ 1%.
4. containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, it is characterised in that methods described synthesis step
It is rapid as follows：
（1）10.6 gram two is added in 500 milliliters of three neck round bottom flask equipped with stirring, reflux condenser and constant pressure funnel
Benzyl ketone, 10.0 grams of phenanthrenequione and 100 milliliters of absolute ethyl alcohols, after heating is completely dissolved ethanol micro-boiling, question response thing, Xiang Sankou
The ethanol solution (3.0 grams of KOH are dissolved in 15 milliliters of absolute ethyl alcohols) of 8 milliliters of KOH, and logical N is slowly added dropwise in flask2Protection；
Solution is gradually switched to blackish green by yellow, is further continued for being heated to reflux terminating reaction after 15 minutes；0 DEG C is cooled to, suction filtration, then often
It is secondary to use 15 milliliter of 95% ethanol to wash precipitation three times, it is put in baking oven and dries, finally obtains black powder solid：Luxuriant and rich with fragrance formula ring penta 2
Ketenes；
（2）Luxuriant and rich with fragrance formula（Many phenyl）Phenyl-vinyl silicon oil can be by the vinyl on the multi-vinyl silicone oil of ethenyl blocking and phenanthrene
Formula cyclopentadienone carries out Diels-Alder reactions to synthesize；In the there-necked flask equipped with backflow and agitating device, ethene is added
The multi-vinyl silicone oil 30g (containing Vi0.015mol) of base end-blocking, luxuriant and rich with fragrance formula cyclopentadienone about 3.9g (0.01mol), add α-
Chloronaphthalene 30ml. is in N2In atmosphere, agitating heating flows back 10 hours；Reaction is by blackish green yellowing clear solution. solution after cooling
Layering, upper strata is product, and lower floor is solvent；Methyl alcohol washed product, till methyl alcohol is water white transparency；150 DEG C of product Jing does
Dry 5 hours, obtain many phenyl vinyl silicone oils of luxuriant and rich with fragrance formula.
5. according to claim 4 containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, its feature
It is, the luxuriant and rich with fragrance formula（Many phenyl）Phenyl-vinyl silicon oil structure is as follows：
。
6. according to claim 4 containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, its feature
It is that the metal oxide is iron oxide, tin oxide, titanium oxide, zinc oxide, one or more in cerium oxide, and granularity is
20nm~30um。
7. according to claim 4 containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, its feature
It is that the catalyst is Karstedt platinum catalysts, and content is 3000 ~ 5000ppm.
8. according to claim 4 containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, its feature
It is that the tackifier are modified epoxy class tackifier.
9. according to claim 4 containing luxuriant and rich with fragrance formula（Many phenyl）The heat-resistant adhesive preparation method of phenyl structure, its feature
It is that above-mentioned all experimental drugs are put into molecular sieve preservation afterwards through dehydration technology process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610919633.1A CN106520063A (en) | 2016-10-21 | 2016-10-21 | Heat-resistant adhesive containing phenanthrenyl(polyphenyl)phenyl structure and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610919633.1A CN106520063A (en) | 2016-10-21 | 2016-10-21 | Heat-resistant adhesive containing phenanthrenyl(polyphenyl)phenyl structure and preparation method thereof |
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| CN106520063A true CN106520063A (en) | 2017-03-22 |
Family
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013431A (en) * | 2012-12-03 | 2013-04-03 | 烟台德邦先进硅材料有限公司 | High-refractivity LED (Light-Emitting Diode) package silica gel |
-
2016
- 2016-10-21 CN CN201610919633.1A patent/CN106520063A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013431A (en) * | 2012-12-03 | 2013-04-03 | 烟台德邦先进硅材料有限公司 | High-refractivity LED (Light-Emitting Diode) package silica gel |
Non-Patent Citations (3)
| Title |
|---|
| W. DILTHEY, ET•AL: ""Tieffarbige aromatische funfringketone. [Heteropolare, XXVII]"", 《ADVANCED SYNTHESIS & CATALYSIS》 * |
| 刘嘉等: "《航空橡胶与密封材料》", 30 November 2011, 国防工业出版社 * |
| 杜作栋等: "含有稠环侧链的聚硅氧烷的合成及其对加成型高温硫化硅橡胶性能的影响", 《高分子学报》 * |
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Application publication date: 20170322 |