CN106520062A - Heat-resistant room temperature vulcanization adhesive containing acenaphthene type (polyphenyl) phenyl structure and preparation method thereof - Google Patents
Heat-resistant room temperature vulcanization adhesive containing acenaphthene type (polyphenyl) phenyl structure and preparation method thereof Download PDFInfo
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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
- 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
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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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
- 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
- C09J11/06—Non-macromolecular additives organic
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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
- C09J11/08—Macromolecular additives
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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
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention provides a heat-resistant room temperature vulcanization adhesive containing an acenaphthene type (polyphenyl) phenyl structure and a preparation method thereof, and relates to an adhesive and a preparation method thereof. A colloid main body of the adhesive selects phenyl vinyl silicon resin and vinyl-terminated methyl phenyl silicone oil which can be cured at room temperature and has excellent heat resistance and mechanical properties at the same time; the selected hydrogen-containing crosslinking agents respectively contain a benzene ring, have high heat resistance compared with a common hydrogen-containing crosslinking agent and also can be better dispersed into a colloid; and the added liquid-state silicon containing compound containing a condensed ring structure contains active hydroxyls at the two ends respectively, can react with the hydrogen-containing crosslinking agent in the presence of a platinum catalyst at room temperature and is embedded into a system as a heat-resistant additive, so that the heat-resistant function of the adhesive is further improved, and compatibility with a silicone rubber matrix and machinability are good. The silicone rubber adhesive provided by the invention has the heat-resistant temperature reaching more than 400 DEG C and also has excellent mechanical properties at the same time.
Description
Technical field
The present invention relates to a kind of adhesive and preparation method thereof, more particularly to a kind of formula containing acenaphthene(Many phenyl)Phenyl structure
Heat-resisting room temperature vulcanization gluing agent 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 consumer goodss 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.
Disclose some preparation methoies with regard to high temperature resistant room temperature vulcanization binding agent in foreign patent, mainly from adhesive and
Solve the above problems in terms of structure design two, the adhesive for using has resistant, toughened polyimides, high resiliency organic silicone adhesive
The kinds such as agent, 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 in mechanical property so that requirement at this stage to high heat-resistant adhesive can not be met, while cannot also meet room temperature sulfur
The condition of change.Room temperature vulcanization to be realized, high temperature resistant, high resiliency, low viscous material property, the resistance to height only containing special construction
Warm organic silicone rubber adhesive is possible to realize.
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 silicone rubber, heat resisting temperature only has 300 DEG C or so, it is impossible to meet special
Requirement of the field to adhesive.
Chinese patent CN200610036843.2 reports the silicone rubber formulations with thermostability, by adding ferrum 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.
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 silicone rubber of methyl blocking, the heat resisting temperature of silicone rubber is successfully improve, but due to strand
Two ends do not have to react with cross-linking agent under active group, room temperature, and which is may be only available in high-temperature silicon disulfide rubber.
The content of the invention
It is an object of the invention to provide a kind of formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure and
Its preparation method, the present invention add the liquid silicon-containing compound containing condensed cyclic structure, and such compound molecule two ends are containing work
Property hydroxyl, can react with hydrogeneous cross-linking agent in the presence of platinum catalyst under room temperature, as the embedded system of heat resistance accessory in, make
Which further improves the heat-resisting function of binding agent, 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:
A kind of formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, is made up of by weight following components:
100 parts of phenyl vinyl polysiloxane;
10 ~ 50 parts of ethenyl blocking methyl phenyl silicone oil;
The hydrogeneous cross-linking agent 10-30 parts of phenyl;
Acenaphthene formula(Many phenyl)1 ~ 20 part of phenyl-vinyl silicon oil;
1 ~ 10 part of metal-oxide;
0.1~5 part of catalyst;
0.01 ~ 1 part of inhibitor;
0.1 ~ 10 part of viscosifier.
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, the phenyl vinyl silicon tree
Fat, viscosity be 5000mPa s ~ 20000mPa s, phenyl mass fraction be 5% ~ 55%, vinyl mass fraction be 0.1% ~
5%。
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, the ethenyl blocking methylbenzene
Base silicone oil, viscosity are 1000mPa s ~ 50000mPa s, and phenyl mass fraction is 5% ~ 55%, and vinyl mass fraction is
0.1%~5%。
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, the hydrogeneous cross-linking agent of the phenyl is
Methyl and phenyl hydrogen-containing silicon oil and the hydrogeneous silicones of phenyl, three silane of phenyl(cas:18027-45-7), diphenyl tetrasiloxane
(cas:66817-59-2), diphenyl trisiloxanes(cas:17875-55-7)In one or more.
Formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure, it is characterised in that the side
Method synthesis step is as follows:
(1)10.9 grams are added in 500 milliliters of three neck round bottom flask equipped with agitator, reflux condenser and constant pressure funnel
Acenaphthenequinone, 12.6 grams of dibenzyl ketones and 120ml dehydrated alcohol, after being heated to ethanol micro-boiling, are slowly added dropwise in there-necked flask
The ethanol solution of 8mlKOH, and it is passed through N2Protection;Reaction solution gradually, after blackening, is further continued for being heated to reflux 17 minutes, stops anti-
Should;Sucking filtration after being cooled to 0 DEG C, is precipitated three times with washing with alcohol.Dry in being put into baking oven, finally obtain black powder solid:
Acenaphthene formula cyclopentadienone;
(2)In the 250ml three neck round bottom flask equipped with backflow flow condenser and agitating device, plus people's terminal hydroxy ethylene silicone oil
30g, acenaphthene formula cyclopentadienone 3.6g, then plus people a- chloronaphthalene 30ml;Then in N2In atmosphere, agitating heating flows back 20 hours;Reaction
Thing becomes red, transparent solution by navy blue;Solution is poured in separatory funnel, stratification, separate lower floor's solvent;Use methanol
Washed product, after the solution in separatory funnel is close to water white transparency, installs vacuum distillation apparatus, removes small molecule solvent,
Obtain final product:The many phenyl vinyl silicone oils of acenaphthene formula.
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure, its described acenaphthene formula
(Many phenyl)Phenyl-vinyl silicon oil structure is as follows:
。
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure, the metal oxidation
Thing is ferrum oxide, stannum oxide, titanium oxide, Zinc Oxide, one or more in cerium oxide, and granularity is 20nm ~ 30um.
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure, the catalyst is
Karstedt platinum catalysts, content are 3000 ~ 5000ppm;The viscosifier are modified epoxy class viscosifier.
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure, the inhibitor is
3- methyl isophthalic acids-butine -3- alcohol, methylpentynol, 3- methyl isophthalic acids-hexin -3- alcohol, 1- acetenyl -1- Hexalin, 4-
One or more in the tert-butyl group -1- ethynylcyclohexanols, 4- phenyl -1- ethynylcyclohexanols and other alkynol compounds.
Described formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure, above-mentioned experimental drug
Using front through dehydration technology process, molecular sieve sealing preserve is put into afterwards.
Advantages of the present invention with effect is:
Colloid main body from ambient temperature curable phenyl vinyl polysiloxane and ethenyl blocking methyl phenyl silicone oil, this as
The excellent heat resistance of tool and mechanical property;Selected hydrogeneous cross-linking agent contains phenyl ring, has compared with common hydrogeneous cross-linking agent
Very high thermostability, while also preferably can be scattered in colloid:Liquid silicide-comprising of the addition for being added containing condensed cyclic structure
Compound, such compound molecule two ends contain activity hydroxy, can be with hydrogeneous crosslinking in the presence of platinum catalyst under room temperature
Agent is reacted, and is embedded in system as heat resistance accessory so as to further improve the heat-resisting function of binding agent, and energy and silicone rubber matrix
The compatibility having had and processability.
Description of the drawings
Fig. 1 is the synthetic reaction equation of acenaphthene formula cyclopentadienone;
Fig. 2 is acenaphthene 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.Acenaphthene formula in each embodiment(Many phenyl)Phenyl-vinyl silicon oil is equal
By obtained by the following manner, narration is not repeated.
(1)Add in 500 milliliters of three neck round bottom flask equipped with agitator, reflux condenser and constant pressure funnel
10.9 grams of acenaphthenequinones, 12.6 grams of dibenzyl ketones and 120ml dehydrated alcohol, water-bath arrange temperature be 80 DEG C, until ethanol it is micro-
Boiling, and after reactant is completely dissolved, l.6gKOH the ethanol solution for being slowly added dropwise 8mlKOH in there-necked flask (is dissolved in 8ml
In ethanol), the speed of titration is 1-2drop/s, and is passed through N2Protection.Reaction solution gradually, after blackening, is further continued for being heated to reflux
17 minutes, stopped reaction.Sucking filtration after being cooled to 0 DEG C, is then washed with 26 milliliter of 95% ethanol every time and is precipitated three times.It is put in baking oven
Drying 18 hours, finally obtains black powder solid:Acenaphthene formula cyclopentadienone.
(2)In the 250ml three neck round bottom flask equipped with reflux condenser and agitating device, plus people's terminal hydroxy ethylene silicon
Oily 30g (containing Vi0.04mol), acenaphthene formula cyclopentadienone 3.6g(0.01mol), then plus people a- chloronaphthalene 30ml, then in N2Atmosphere
Middle agitating heating flows back 20 hours.Reaction is become, after red, transparent solution, solution to be poured in separatory funnel while hot by navy blue,
After cooling, solution left standstill layering, upper strata is product, and lower floor is solvent, separates lower floor's solvent.Use methanol washed product, Zhi Daofen
Till solution in liquid funnel is close to water white transparency.Vacuum distillation apparatus are installed, the temperature of oil bath pan is set as 150 DEG C, remove
After small molecule solvent, distillation terminates, and obtains final product:The many phenyl vinyl silicone oils of acenaphthene formula.
Embodiment 1
100 parts of phenyl vinyl polysiloxanes(Viscosity is 12000mPa s, and phenyl mass fraction is 45%, vinyl mass fraction
For 5%), 10 parts of acenaphthene formulas(Many phenyl)Phenyl-vinyl silicon oil, 2 parts of viscosifier (commercially available), 4 parts of nano tin dioxides, 0.5 part
Karstedt platinum catalysts (5000ppm), inhibitor PC-610(It is commercially available)Addition see the table below, mechanical agitation mix homogeneously,
With 100 DEG C of vaccum dewatering 5h after planetary mixer stirring 2h.Add the hydrogeneous cross-linking agent of 92.56 parts of phenyl(Viscosity is
1200mPa s, phenyl mass fraction are 45%, hydrogen content 0.26%), the bubble after mix homogeneously in low pressure removing system;Room temperature
Can be fully cured after lower 10h.With inhibitor addition as proportioning, hardening time such as following table is obtained:
Obviously, different use occasions has different requirements to adhesive hardening time, and the present invention is by changing adding for inhibitor
Enter the hardening time that amount can reasonably control adhesive.
Embodiment 2
By the phenyl vinyl polysiloxane of different ratio(Viscosity is 12000mPa s, and phenyl mass fraction is 45%, ethylene substrate
Amount fraction is 5%)With ethenyl blocking methyl phenyl silicone oil(Viscosity is 1000mPa s, and phenyl mass fraction is 45%, vinyl
Mass fraction is 0.45%), 10 parts of acenaphthene formulas(Many phenyl)Phenyl-vinyl silicon oil, 2 parts of viscosifier (commercially available), 4 parts are nano oxidized
Stannum, 0.5 part of Karstedt platinum catalyst (5000ppm), mechanical agitation mix homogeneously, with after planetary mixer stirring 2h 100
DEG C vaccum dewatering 5h.Add 0.06 part of inhibitor PC-610(It is commercially available), the hydrogeneous cross-linking agent of phenyl(Viscosity is 1200mPa s,
Phenyl mass fraction is 45%, hydrogen content 0.26%)Addition see the table below, the bubble after mix homogeneously in low pressure removing system;Room
Can be fully cured after the lower 10h of temperature.With phenyl vinyl polysiloxane, ethenyl blocking methyl phenyl silicone oil difference addition be with
Than the cured glue mechanics performance such as following table of survey:
The addition of a certain amount of ethenyl blocking methyl phenyl silicone oil can improve the elongation at break of colloid as seen from the above table, to intensity
Affect less.As ethenyl blocking methyl phenyl silicone oil addition increases, the elongation at break of colloid and tensile strength have
Decline.
Embodiment 3
85 parts of phenyl vinyl polysiloxanes(Viscosity is 12000mPa s, and phenyl mass fraction is 45%, and vinyl mass fraction is
5%), 15 parts of ethenyl blocking methyl phenyl silicone oils(Viscosity is 1000mPa s, and phenyl mass fraction is 45%, vinyl quality
Fraction is 0.45%), 10 parts of acenaphthene formulas(Many phenyl)Phenyl-vinyl silicon oil, 2 parts of viscosifier (commercially available), 4 parts of metal-oxides,
0.5 part of Karstedt platinum catalyst (5000ppm), mechanical agitation mix homogeneously are true with 100 DEG C after planetary mixer stirring 2h
Empty eliminating water 5h.Add 0.06 part of inhibitor PC-610(It is commercially available), the hydrogeneous cross-linking agent of 75.8 parts of phenyl(Viscosity is 1200mPa
S, phenyl mass fraction are 45%, hydrogen content 0.26%), the bubble after mix homogeneously in low pressure removing system;Under room temperature after 10h i.e.
Can be fully cured.With metal-oxide species as proportioning, colloidal property such as following table is obtained:
Can be obtained by data above, formula provided by the present invention is obtained the silicone rubber glue of Good Heat-resistance, good mechanical properties
Glutinous agent, is applicable to the different occasions for having special heat resistant requirements to adhesive by changing formula proportion.Above-mentioned is concrete
Embodiment is exemplary, is to preferably make skilled artisans appreciate that the present invention, it is impossible to be not understood as
The restriction of scope is included to the present invention;As long as according to any equivalent change made or modification of disclosed spirit,
Each fall within scope by the invention.
Claims (10)
1. a kind of formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, it is characterised in that pressed by following components
Weight portion meter is constituted:
100 parts of phenyl vinyl polysiloxane;
10 ~ 50 parts of ethenyl blocking methyl phenyl silicone oil;
The hydrogeneous cross-linking agent 10-30 parts of phenyl;
Acenaphthene formula(Many phenyl)1 ~ 20 part of phenyl-vinyl silicon oil;
1 ~ 10 part of metal-oxide;
0.1~5 part of catalyst;
0.01 ~ 1 part of inhibitor;
0.1 ~ 10 part of viscosifier.
2. formula containing acenaphthene according to claim 1(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, its feature exist
In the phenyl vinyl polysiloxane, viscosity are 5000mPa s ~ 20000mPa s, and phenyl mass fraction is 5% ~ 55%, second
Thiazolinyl mass fraction is 0.1% ~ 5%.
3. formula containing acenaphthene according to claim 1(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, its feature exist
In, the ethenyl blocking methyl phenyl silicone oil, viscosity is 1000mPa s ~ 50000mPa s, phenyl mass fraction is 5% ~
55%, vinyl mass fraction is 0.1% ~ 5%.
4. formula containing acenaphthene according to claim 1(Many phenyl)The heat-resisting room temperature vulcanization gluing agent of phenyl structure, its feature exist
In the hydrogeneous cross-linking agent of the phenyl is methyl and phenyl hydrogen-containing silicon oil and the hydrogeneous silicones of phenyl, three silane of phenyl(cas:18027-
45-7), diphenyl tetrasiloxane(cas:66817-59-2), diphenyl trisiloxanes(cas:17875-55-7)In one kind or
It is various.
5. formula containing acenaphthene(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure, it is characterised in that methods described
Synthesis step is as follows:
(1)10.9 grams are added in 500 milliliters of three neck round bottom flask equipped with agitator, reflux condenser and constant pressure funnel
Acenaphthenequinone, 12.6 grams of dibenzyl ketones and 120ml dehydrated alcohol, after being heated to ethanol micro-boiling, are slowly added dropwise in there-necked flask
The ethanol solution of 8mlKOH, and it is passed through N2Protection;Reaction solution gradually, after blackening, is further continued for being heated to reflux 17 minutes, stops anti-
Should;Sucking filtration after being cooled to 0 DEG C, is precipitated three times with washing with alcohol;
Dry in being put into baking oven, finally obtain black powder solid:Acenaphthene formula cyclopentadienone;
(2)In the 250ml three neck round bottom flask equipped with backflow flow condenser and agitating device, plus people's terminal hydroxy ethylene silicone oil
30g, acenaphthene formula cyclopentadienone 3.6g, then plus people a- chloronaphthalene 30ml;Then in N2In atmosphere, agitating heating flows back 20 hours;Reaction
Thing becomes red, transparent solution by navy blue;Solution is poured in separatory funnel, stratification, separate lower floor's solvent;Use methanol
Washed product, after the solution in separatory funnel is close to water white transparency, installs vacuum distillation apparatus, removes small molecule solvent,
Obtain final product:The many phenyl vinyl silicone oils of acenaphthene formula.
6. formula containing acenaphthene according to claim 5(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure,
Characterized in that, the acenaphthene formula(Many phenyl)Phenyl-vinyl silicon oil structure is as follows:
。
7. formula containing acenaphthene according to claim 5(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure,
Characterized in that, the metal-oxide is ferrum oxide, and stannum oxide, titanium oxide, Zinc Oxide, one or more in cerium oxide,
Granularity is 20nm ~ 30um.
8. formula containing acenaphthene according to claim 5(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure,
Characterized in that, the catalyst is Karstedt platinum catalysts, content is 3000 ~ 5000ppm;The viscosifier are modified
Epoxiess viscosifier.
9. formula containing acenaphthene according to claim 5(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure,
Characterized in that, the inhibitor is 3- methyl isophthalic acids-butine -3- alcohol, methylpentynol, 3- methyl isophthalic acids-hexin -3-
Alcohol, 1- acetenyl -1- Hexalin, the 4- tert-butyl group -1- ethynylcyclohexanols, 4- phenyl -1- ethynylcyclohexanols and other alkynols
One or more in class compound.
10. formula containing acenaphthene according to claim 5(Many phenyl)The heat-resisting room temperature vulcanization gluing agent preparation method of phenyl structure,
Characterized in that, above-mentioned experimental drug is processed through dehydration technology using front, molecular sieve sealing preserve is put into afterwards.
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