CN109988307A - Promotor, liquid silicon rubber composition and the liquid silastic of liquid silastic - Google Patents
Promotor, liquid silicon rubber composition and the liquid silastic of liquid silastic Download PDFInfo
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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
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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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
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- 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
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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Abstract
The present invention relates to field of liquid silicone rubber, disclose the promotor, liquid silicon rubber composition and liquid silastic of liquid silastic.The promotor has chemical structure shown in formula (1) or formula (2):Formula (1),
Description
Technical field
The present invention relates to field of liquid silicone rubber, and in particular to the promotor of liquid silastic includes the promotor
Liquid silicon rubber composition, and the liquid silastic solidified by the liquid silicon rubber composition.
Background technique
Since add-on type liquid silica gel molecule itself is in nonpolarity, be bonded, this serious limitation is difficult to other materials
The application range of add-on type liquid silica gel.The technical solution for improvement its adhesive property being commonly used has: one, use bottom
Paint handles substrate surface；Two, change the molecular structure of base rubber polysiloxanes；Three, tackifier are added.
The defect of the prior art: one, using silane coupling agent, manufacturing procedure is increased, production efficiency is low；In addition, most of bottom
Paint contains volatile flammable solvent, easily causes peril of transportation, environmental pollution.Two, change the method for polysiloxane molecule structure,
Its actual production process is more complicated, leads to higher cost, is unfavorable for industrialization.Three, the method that tackifier are added in system,
Method easy to operate, easily controllable and more common at present, but there are poor compatibility, it is catalyzed easily poisoning, adhesive strength is not
The problems such as ideal, adhesives type is limited.
A kind of dual composition addition type mold silica gel of high strength easy demoulding of CN106854369A, contains: component A 50-80
Part, 3-12 parts of second component, 20-40 parts of white carbon black, 4-12 parts of white carbon black inorganic agent, 0.003-0.1 parts of catalyst and 0.002-
The inhibitor 2 of 0.03 part of inhibitor 1 and 0.1-1.0 part.Wherein, specifically, component A includes vinyl-terminated silicone fluid and end second
Alkenyl chain vinyl silicone oil；Component B is containing hydrogen silicone oil, comprising end group containing hydrogen silicone oil and end side chain containing the Silicon Containing Hydrogen of SiH
Oil.White carbon black inorganic agent is hexa methyl silazane, tetramethyl divinyl disilazane, heptamethyldisilazane, vinyl list
One of end socket or two kinds of mixtures.Product obtained has extraordinary mobility, and easy mold release can be used for dimensional accuracy
Demanding modelling.The mold silica gel requires to be easily separated from mold (generally metal), not may require that adhesive strength.
CN105622941A discloses a kind of UV and mixes solidification LED packaging plastic, which is characterized in that the packaging plastic is contained by phenyl
Hydrogen silicone oil, 4 vinyl epoxy cyclohexane and trimethylolpropane trimethacrylate react under platinum catalyst effect to be prepared into
It arrives；According to parts by weight, composition and content include: 100-180 parts of aminomethyl phenyl ring body to phenyl hydrogen-containing silicon oil, hydrogeneous ring body
10-60 parts, 30-50 parts of hydrogeneous double seal head, 20-60 parts of distilled water, 100-200 parts of solvent, 0.03-0.05 parts of catalyst；Solvent
For the one or two of toluene or benzene；Catalyst is the one or two of 98wt% sulfuric acid or the hydrochloric acid of 38wt%.The encapsulation
Glue can be packaged according to the dual cure mode of free radical and cationic curing, reduce prior art solidification temperature height with
And the problem that curing time is long.
As can be seen that the adhesive property of existing liquid silastic and other materials is not fine, it is desirable to provide new skill
Art scheme.
Summary of the invention
It is difficult to the purpose of the invention is to overcoming the problems, such as liquid silastic with other materials be bonded, provides liquid silicon
Promotor, liquid silicon rubber composition and the liquid silastic of rubber.The liquid silastic has good with other materials
Adhesive property.
To achieve the goals above, first aspect present invention provides a kind of promotor of liquid silastic, wherein the rush
There is chemical structure shown in formula (1) or formula (2) into agent:
Wherein, m=1-10, x=1-5, t=1-30, d=1-20, f=1-10, g=1-5, h=1-30, b=1-20
Positive integer.
Preferably, the promotor will be by that will contain acrylic acid bifunctional in the presence of catalyst and reaction dissolvent
Ester carries out synthetic reaction with component A and obtains, wherein the component A is that the hydrogeneous silicone resin of phenyl or phenyl hydrogen-containing siloxane are low
Polymers.
Second aspect of the present invention provides a kind of liquid silicon rubber composition, and the composition includes:
The vinyl silicone oil of 100 parts by weight, the epoxy modified polysiloxane of 5-60 parts by weight, 10-50 parts by weight white carbon black, 5-
Containing hydrogen silicone oil, the promotor provided by the invention of 0.5-30 parts by weight, the silazane of 5-35 parts by weight, the 1-20 weight of 30 parts by weight
That measures the deionized water of part, the organic solvent of 0.002-0.02 parts by weight and 0.05-0.5 parts by weight contains platinum complex.
Preferably, viscosity of the epoxy modified polysiloxane at 25 DEG C is 50-10000cP, the epoxy modified polysiloxane
Epoxide number is 0.1-0.9 equivalent/100g.
Third aspect present invention provides a kind of liquid silastic, silicon rubber liquid silastic combination provided by the present invention
Object is cured to be obtained, and the shear bond strength of the liquid silastic and aluminium flake is 4MPa or more, and the stretching of the liquid silastic is strong
Degree is 8.1MPa or more, and the elongation at break of the liquid silastic is 580% or more.
Through the above technical solutions, a kind of firm liquid silastic Nian Jie with other materials can be provided.The liquid silicon
Rubber adhesives is extensive, high mechanical strength；And safety and environmental protection, cost is relatively low, easy to operate, high production efficiency, Ke Yizeng
Add the application range of vinylsiloxane rubber.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
First aspect present invention provides a kind of promotor of liquid silastic, wherein the promotor has formula (1) or formula
(2) chemical structure shown in:
Wherein, m=1-10, x=1-5, t=1-30, d=1-20, f=1-10, g=1-5, h=1-30, b=1-20
Positive integer.
There is promotor provided by the invention above-mentioned chemical structure can contribute to liquid silastic acquisition and other materials
Good bonding.Preferably, the promotor will be by that will contain bifunctional third in the presence of catalyst and reaction dissolvent
Olefin(e) acid ester carries out synthetic reaction with component A and obtains, wherein the component A is the hydrogeneous silicone resin of phenyl or phenyl Silicon Containing Hydrogen oxygen
Alkane oligomer.
In the present invention, to obtain the promotor with above-mentioned chemical structure, it is preferable that described to contain propylene bifunctional
Acid esters is selected from 2- ethyoxyl -1,6 hexanediol diacrylate, 1,4- butylene glycol aerylate or 1,6-HD diacrylate
Ester.
In the present invention, it is preferable that the viscosity of the phenyl hydrogen-containing siloxane oligomer is 50-1000cP, preferably 150-
250cP, the phenyl content of the phenyl hydrogen-containing siloxane oligomer are 35-40 weight %, and hydrogen content is 0.2-1 weight %.Its
In, viscosity is 25 DEG C.Phenyl content and hydrogen content are all on the basis of the total amount of the phenyl hydrogen-containing siloxane oligomer.Institute
Stating phenyl hydrogen-containing siloxane oligomer is known substance, can be commercially available.Such as Jiangxi fly new material Co., Ltd, the trade mark
PH-3 (viscosity 150-250cP, phenyl content be 38 weight %, hydrogen content be 0.5 weight %).
In the present invention, it is preferable that the viscosity of the hydrogeneous silicone resin of phenyl is 1000-5000cP, preferably 1200-
2300cP, the phenyl content of the hydrogeneous silicone resin of phenyl are 40-50 weight %, and hydrogen content is 0.1-0.4 weight %.Wherein,
Viscosity is 25 DEG C.Phenyl content and hydrogen content are all on the basis of the total amount of the hydrogeneous silicone resin of the phenyl.Such as Jiangxi is taken wing
Xiang new material Co., Ltd, (viscosity 2100-2500cP, phenyl content are 15 weight %, hydrogen content 0.26 to the PH-2 of the trade mark
Weight %).
It is described to contain containing acrylate bifunctional and the hydrogeneous silicone resin of the phenyl or phenyl in the present invention
The dosage of hydrogen siloxane oligomer meets the synthetic reaction and obtains the promotor with above-mentioned chemical structure.Preferably,
It is described to contain double officials on the basis of the catalyst, reaction dissolvent, the total amount containing acrylate bifunctional and component A
The dosage for the acrylate that can be rolled into a ball is 20-30 weight %；The dosage of the component A is 20-30 weight %.The i.e. described phenyl is hydrogeneous
The dosage of silicone resin or phenyl hydrogen-containing siloxane oligomer is 20-30 weight %.
In the present invention, it is preferable that the catalyst is containing platinum complex, and platinum content is 2000-2400 mass ppm, preferably
The catalyst is selected from chloroplatinic acid, methyl vinyl silicone coordination platinum, tetrahydrofuran coordination platinum or alcohol and is coordinated platinum；The reaction
Solvent is selected from toluene, 1- ethynylcyclohexanol or 3- methyl-1-butine-3- alcohol.
In the present invention, it is preferable that with the catalyst, reaction dissolvent, containing acrylate bifunctional and component A
On the basis of total amount, the dosage of the catalyst is 0.03-1 weight %；The dosage of the reaction dissolvent is 20-59.95 weight %.
In the present invention, it is preferable that synthesis reaction temperature is 50-80 DEG C, synthesising reacting time 2-4h.
A kind of preferred embodiment of the present invention, on the basis of each component summation for synthesizing the promotor, synthesis
The component of the promotor include: 20-30 weight % bifunctional acrylate (be not limited to 2- ethyoxyl -1,6- oneself two
Alcohol diacrylate, 1,4-butanediol acrylate or 1,6- hexanediyl ester), the catalysis of 0.03-1 weight %
Agent, the reaction dissolvent of 20-59.95 weight %, the hydrogeneous silicone resin of phenyl or phenyl hydrogen-containing siloxane of 20-30 weight %
Oligomer.
A kind of preferred embodiment of the present invention, the method for synthesizing the promotor include:
S1, the bifunctional acrylate of 20-30 parts by weight (is not limited to 2- ethyoxyl-two propylene of 1,6-HD
Acid esters, 1,4-butanediol acrylate or 1,6- hexanediyl ester), the catalyst of 0.03-1 parts by weight be (platinum
Mass fraction is that 2200 mass ppm) and the part reaction dissolvent are added in round-bottomed flask, is stirred with the revolving speed of 200r/min
It mixes and is warming up to 50-80 DEG C, constant temperature 1-3h；
S2, the hydrogeneous silicone resin of phenyl or phenyl hydrogen-containing siloxane oligomer and part are instilled into the mixture that S1 is obtained
(wherein the hydrogeneous silicone resin of phenyl or phenyl hydrogen-containing siloxane oligomer are 20-30 weight to the mixed solution of the reaction dissolvent
Part)；Then it is warming up to 50-80 DEG C and keeps the temperature and carry out synthetic reaction 2-4h；
S3, reaction product is cooled to room temperature, a certain amount of activated carbon adsorption catalyst is added；Then reaction product is taken out
Filter, rotary evaporation remove solvent, are finally evaporated under reduced pressure to no low-boiling-point substance product at 100 DEG C and steam, obtain the promotor.
In this method, the total amount of the part reaction dissolvent used respectively in step S1 and S2 is 20-59.95 weight
Part.And in the above method of the invention, the bifunctional acrylate, catalyst, reaction dissolvent and component A (phenyl
Hydrogeneous silicone resin or phenyl hydrogen-containing siloxane oligomer) inventory summation be 100 parts by weight.
In the present invention, shown in the chemical structure that the promotor has such as formula (1) or formula (2).Can by it is above-mentioned synthesize it is anti-
Reactant bifunctional acrylate, the hydrogeneous silicone resin of phenyl or the phenyl hydrogen-containing siloxane oligomer that should be participated in are specifically used
Compound determine, the structure of the promotor can also be determined by Fourier's infrared test approach.
Second aspect of the present invention provides a kind of liquid silicon rubber composition, and the composition includes:
The vinyl silicone oil of 100 parts by weight, the epoxy modified polysiloxane of 5-60 parts by weight, 10-50 parts by weight white carbon black, 5-
Containing hydrogen silicone oil, the promotor provided by the invention of 0.5-30 parts by weight, the silazane of 5-35 parts by weight, the 1-20 weight of 30 parts by weight
That measures the deionized water of part, the organic solvent of 0.002-0.02 parts by weight and 0.05-0.5 parts by weight contains platinum complex.
The organic solvent, containing platinum complex as described above, repeating no more.
The available liquid silastic can with other materials with cementability of composition provided by the invention.
In the present invention, the vinyl silicone oil can be vinyl-terminated silicone fluid, such as viscosity is 5000-100000cP, second
Amount vinyl content is 0.02-0.06mmol/g.
In the present invention, it is preferable that viscosity of the epoxy modified polysiloxane at 25 DEG C is 50-10000cP, and the epoxy changes
Property silicone oil epoxide number be 0.1-0.9 equivalent/100g.The epoxy modified polysiloxane also can contribute to liquid-phase silicone rubber of the invention
The cementability with other materials that glue has had can be end epoxy silicon oil, side group epoxy silicone oil and end side epoxy silicon oil, preferably
To hold epoxy silicon oil.The epoxy modified polysiloxane can be commercially available, such as Anhui Ai Yueta silicone oil Co., Ltd, the trade mark
105-4 (viscosity 50-10000cP, epoxide number are 0.1-0.9 equivalent/100g).The epoxy modified polysiloxane can be with formula
(3) chemical structural formula shown in:
Wherein, the positive integer of n=1-50；R is
In the present invention, the silazane can be hexamethyldisilazane and/or divinyl tetramethyl-disilazane.
In the present invention, it is preferable that it is 250-350m that the white carbon black, which can be specific surface area,2The vapor phase method titanium dioxide of/g
Silicon.
Other components, such as heat filling, fire retardant, Conductive inorganic powder can also be contained in composition provided by the invention
End, organic pigment, heat stabilizer, mould inhibitor, antibacterial agent, plasticizer etc..Additive amount control is not influencing required performance, and
Effect of the invention is not covered.
Third aspect present invention provides a kind of liquid silastic, silicon rubber liquid silastic combination provided by the present invention
Object is cured to be obtained, and the shear bond strength of the liquid silastic and aluminium flake is 4MPa or more, and the stretching of the liquid silastic is strong
Degree is 8.1MPa or more, and the elongation at break of the liquid silastic is 580% or more.
In the present invention, the fluid silicone rubber is obtained by the liquid silicon rubber composition, it is preferable that preparation method packet
It includes:
Added into the vinyl silicone oil of 100 parts by weight the white carbon blacks of 10-50 parts by weight, 5-35 parts by weight silazane and
The deionized water of 1-20 parts by weight is less than 25rpm with kneader control revolving speed, uniformly mediates 3-5h in the case where temperature is lower than 60 DEG C；
It is warming up to 170-190 DEG C by obtained product is mediated, remixes 2-4h；Then stirring 1-3h is vacuumized；
The vinyl silicone oil of 100 parts by weight is slowly added to, then carries out kneading 2-4h, then cooling discharge, by product into
Row grinding obtains liquid silastic base-material.
By the epoxy modified polysiloxane of 5-60 parts by weight, the containing hydrogen silicone oil of 5-30 parts by weight, 0.5-30 parts by weight the present invention
The promotor of offer, the organic solvent of 0.002-0.02 parts by weight and 0.05-0.5 parts by weight are uniformly mixed containing platinum complex,
Obtain liquid silicon rubber composition；
The liquid silicon rubber composition is dried at 110-130 DEG C and carries out solidification 1-2h, obtains liquid silastic.
The present invention will be described in detail by way of examples below.In following embodiment,
Using the adhesive strength of GB/T 7124-2008 test liquid silica-gel composition and substrate.
The tensile strength and elongation at break of liquid silica gel composition after being solidified using GB/T 528-2009 test.
Embodiment 1
For illustrating the synthesis of promotor of the invention.
By the chloroplatinic acid of 2- ethyoxyl -1,6 hexanediol diacrylate of 40g, 0.05g, (Pt content is 2200 mass
Ppm it) is added in round-bottomed flask with the toluene of 40g, is stirred with the revolving speed of 200r/min and is warming up to 50 DEG C, constant temperature 1h；
Then the mixed solution of phenyl hydrogen-containing siloxane oligomer (PH-3) and toluene is instilled (containing the benzene of 39g in mixed liquor
Base hydrogen-containing siloxane oligomer) total 80g；It is warming up to 80 DEG C and keeps the temperature and carry out synthetic reaction 2h；
Reaction product is cooled to room temperature, and the activated carbon adsorption catalyst of 8g is added, then filters solution, rotary evaporation removes
Solvent is removed, finally product is evaporated under reduced pressure at 100 DEG C to no low-boiling-point substance and is steamed, obtains diphenylguanidine 1, chemical structure such as formula (4) institute
Show, the structural unit that wherein m, x, t are limited comes from PH-3, and PH-3 is mixture, meets m=1-10, x=1-5, t=1-30.
Embodiment 2
For illustrating the synthesis of promotor of the invention.
By 1, the 6- hexanediyl ester of 80g, the chloroplatinic acid (Pt content is 2200 mass ppm) and 100g first of 0.1g
Benzene is added in round-bottomed flask, is stirred with the revolving speed of 200r/min and is warming up to 60 DEG C, constant temperature 2h；
Then (phenyl in mixed liquor containing 75g is hydrogeneous for the mixed solution of the instillation hydrogeneous silicone resin of phenyl (PH-2) and toluene
Siloxane oligomer) total 150g；It is warming up to 80 DEG C and keeps the temperature and carry out synthetic reaction 3h；
Reaction product is cooled to room temperature, and the activated carbon adsorption catalyst of 10g is added, then filters solution, rotary evaporation
Solvent is removed, finally product is evaporated under reduced pressure at 100 DEG C to no low-boiling-point substance and is steamed, diphenylguanidine 2, chemical structure such as formula (5) are obtained
Shown, the structural unit that wherein f, g, h are limited comes from PH-2, and PH-2 is mixture, meets f=1-10, g=1-5, h=1-30.
Embodiment 3
For illustrating the synthesis of promotor of the invention.
By the 1,4-butanediol acrylate of 20g, the tetrahydrofuran coordination platinum of 0.05g (Pt content is 2200 mass ppm)
It is added in round-bottomed flask with 20g toluene, is stirred with the revolving speed of 200r/min and is warming up to 80 DEG C, constant temperature 3h；
Then the mixed solution of phenyl hydrogen-containing siloxane oligomer (PH-3) and toluene is instilled (containing the benzene of 18g in mixed liquor
Base hydrogen-containing siloxane oligomer) total 40g；Synthetic reaction 3h is carried out in 80 DEG C of heat preservations；
Reaction product is cooled to room temperature, and the activated carbon adsorption catalyst of 5g is added, then filters solution, rotary evaporation removes
Solvent is removed, finally product is evaporated under reduced pressure at 100 DEG C to no low-boiling-point substance and is steamed, obtains diphenylguanidine 3, chemical structure such as formula (6) institute
Show, the structural unit that wherein f, g, h are limited comes from PH-3, and PH-3 is mixture, meets f=1-10, g=1-5, h=1-30.
Embodiment 4
For illustrating the preparation of liquid silastic.
To 50 parts of vinyl silicone oils (vinyl-terminated silicone fluid, viscosity 5000-100000cP, contents of ethylene 0.02-
In 0.06mmol/g), adding 30 parts of specific surface areas is 300m2The fumed silica of/g, 10 parts of divinyl tetramethyl
Disilazane, 5 parts of deionized water control revolving speed in kneader and are lower than 25rpm, and temperature is lower than 60 DEG C, uniformly mixes 3h, rises
Temperature vacuumizes stirring 1h, is slowly added to 50 parts of vinyl silicone oil, mediate 2h, cooling discharge grinding obtains to 180 DEG C of mixing 2h
To liquid silicon rubber base-material.
20 parts of epoxy modified polysiloxane (105-4), 10 parts of containing hydrogen silicone oil, 5 parts of rush are added into the silicon rubber base-material
Into agent D1, each component is uniformly mixed to get liquid silicon rubber composition by 0.01 part of cyclohexanol and 0.5 part of chloroplatinic acid.
Liquid silicon rubber composition is solidified into 1h in 120 DEG C of baking ovens, obtains liquid silicon rubber composition cured article.
Embodiment 5
According to the method for embodiment 4, the difference is that, diphenylguanidine 1 is substituted with diphenylguanidine 2.
Embodiment 6
According to the method for embodiment 4, the difference is that, diphenylguanidine 1 is substituted with diphenylguanidine 3.
Embodiment 7
To 50 parts of vinyl silicone oils (vinyl-terminated silicone fluid, viscosity 5000-100000cP, contents of ethylene 0.02-
In 0.06mmol/g), adding 50 parts of specific surface areas is 300m2The fumed silica of/g, 5 parts of hexamethyldisilazane,
20 parts of deionized water controls revolving speed in kneader and is lower than 25rpm, and temperature is lower than 60 DEG C, uniformly mixes 3h, be warming up to 170
DEG C mixing 3h, vacuumizes stirring 1h, is slowly added to 50 parts of vinyl silicone oil, mediate 1h, cooling discharge grinding obtains liquid silicon
Rubber base-material.
5 parts of epoxy modified polysiloxane (105-4), 30 parts of containing hydrogen silicone oil, 30 parts of rush are added into the silicon rubber base-material
Into agent D1,0.02 part of cyclohexanol and 0.1 part of tetrahydrofuran are coordinated platinum, and each component is uniformly mixed to get liquid silastic
Composition.
Liquid silicon rubber composition is solidified into 3h in 110 DEG C of baking ovens, obtains liquid silicon rubber composition cured article.
Embodiment 8
To 50 parts of vinyl silicone oils (vinyl-terminated silicone fluid, viscosity 5000-100000cP, contents of ethylene 0.02-
In 0.06mmol/g), adding 10 parts of specific surface areas is 300m2The fumed silica of/g, 35 parts of divinyl tetramethyl
Disilazane, 1 part of deionized water control revolving speed in kneader and are lower than 25rpm, and temperature is lower than 60 DEG C, uniformly mixes 3h, rises
Temperature vacuumizes stirring 3h, is slowly added to 50 parts of vinyl silicone oil, mediate 4h, cooling discharge grinding obtains to 190 DEG C of mixing 1h
To liquid silicon rubber base-material.
60 parts of epoxy modified polysiloxane (105-4), 5 parts of containing hydrogen silicone oil, 0.5 part of rush are added into the silicon rubber base-material
Into agent D1, each component is uniformly mixed to get liquid silicon rubber composition by 0.002 part of cyclohexanol and 0.05 part of chloroplatinic acid.
Liquid silicon rubber composition is solidified into 1.5h in 130 DEG C of baking ovens, obtains liquid silicon rubber composition cured article.
Comparative example 1
According to the method for embodiment 4, the difference is that, it is not added with epoxy modified polysiloxane, obtains silicon rubber.
Comparative example 2
According to the method for embodiment 4, the difference is that, diphenylguanidine 1 is not added, silicon rubber is obtained.
Comparative example 3
According to the method for embodiment 4, the difference is that, epoxy modified polysiloxane and diphenylguanidine 1 are not added, silicon rubber is obtained.
The silicon rubber that embodiment 4-8 and comparative example 1-3 are obtained carries out shear bond strength and Mechanics Performance Testing.
Table 1
The promotor that can be seen that three kinds of synthesis provided by the invention by the result of embodiment, comparative example and table 1 is all right
The effect of being significantly improved of the shear bond strength of liquid silicon rubber composition, and the addition of adhesion promoters is to liquid silastic
The Effect on Mechanical Properties of composition is little.Secondly, diphenylguanidine 1 (such as comparative example 1) individually is added in liquid silica gel component, make
Liquid silica gel composition increases to the adhesive strength of aluminium flake and PA piece, but improves not to the adhesive strength of PC piece and PET sheet
Obviously.In addition, epoxy modified polysiloxane (such as comparative example 2) individually is added in liquid silica gel component, to liquid silica gel composition pair
Aluminium flake, PA piece, PC piece and PET sheet adhesive strength improve it is undesirable.So promotor and epoxy modified polysiloxane are used cooperatively
Optimal effect can be played.
In terms of cementability, the embodiment of the present invention test result is bonding interface cohesional failure；The test result of comparative example
Destruction or stripping damage are mixed for bonding interface.
Test result of the invention is tensile strength > 8.1MPa, elongation at break > 580%；The test of comparative example experiment
It as a result is tensile strength 7.4-8.0MPa, elongation at break 499-548%.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of promotor of liquid silastic, which is characterized in that the promotor has chemistry shown in formula (1) or formula (2)
Structure:
Wherein, m=1-10, x=1-5, t=1-30, d=1-20, f=1-10, g=1-5, h=1-30, b=1-20's is just whole
Number.
2. promotor according to claim 1, wherein the promotor by the presence of catalyst and reaction dissolvent,
It will carry out synthetic reaction with component A containing acrylate bifunctional to obtain, wherein the component A is phenyl Silicon Containing Hydrogen tree
Rouge or phenyl hydrogen-containing siloxane oligomer.
3. promotor according to claim 2, wherein described to be selected from 2- ethyoxyl-containing acrylate bifunctional
1,6 hexanediol diacrylate, 1,4- butylene glycol aerylate or 1,6 hexanediol diacrylate；Preferably, the phenyl
The viscosity of hydrogen-containing siloxane oligomer be 50-1000cP, preferably 150-250cP, the phenyl hydrogen-containing siloxane oligomer
Phenyl content is 35-40 weight %, and hydrogen content is 0.2-1 weight %；The viscosity of the hydrogeneous silicone resin of phenyl is 1000-
The phenyl content of 5000cP, preferably 1200-2300cP, the hydrogeneous silicone resin of phenyl are 40-50 weight %, and hydrogen content is
0.1-0.4 weight %.
4. promotor according to claim 2 or 3, wherein with the catalyst, reaction dissolvent, containing bifunctional
On the basis of the total amount of acrylate and component A, the dosage containing acrylate bifunctional is 20-30 weight %；Institute
The dosage for stating component A is 20-30 weight %.
5. promotor according to claim 2 or 3, wherein the catalyst is containing platinum complex, platinum content 2000-
2400 mass ppm, the preferably described catalyst be selected from chloroplatinic acid, methyl vinyl silicone be coordinated platinum, tetrahydrofuran coordination platinum or
Alcohol is coordinated platinum；The organic solvent is selected from toluene, 1- ethynylcyclohexanol or 3- methyl-1-butine-3- alcohol.
6. promotor according to claim 2 or 3, wherein with the catalyst, reaction dissolvent, containing bifunctional
On the basis of the total amount of acrylate and component A, the dosage of the catalyst is 0.03-1 weight %；The dosage of the reaction dissolvent
For 20-59.95 weight %.
7. promotor according to claim 2 or 3, wherein synthesis reaction temperature is 50-80 DEG C, and synthesising reacting time is
2-4h。
8. a kind of liquid silicon rubber composition, the composition include:
The vinyl silicone oil of 100 parts by weight, the epoxy modified polysiloxane of 5-60 parts by weight, the white carbon black of 10-50 parts by weight, 5-30 weight
Measure the silicon of promotor described in any one of the containing hydrogen silicone oil of part, claim 1-7 of 0.5-30 parts by weight, 5-35 parts by weight
Azane, the deionized water of 1-20 parts by weight, the organic solvent of 0.002-0.02 parts by weight and 0.05-0.5 parts by weight platiniferous network
Close object.
9. composition according to claim 8, wherein viscosity of the epoxy modified polysiloxane at 25 DEG C is 50-
10000cP, the epoxide number of the epoxy modified polysiloxane are 0.1-0.9 equivalent/100g.
10. a kind of liquid silastic, silicon rubber liquid silicon rubber composition as described in claim 8 or 9 is cured to be obtained,
The shear bond strength of the liquid silastic and aluminium flake is 4MPa or more, the tensile strength of the liquid silastic be 8.1MPa with
On, the elongation at break of the liquid silastic is 580% or more.
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| CN110684357A (en) * | 2019-09-16 | 2020-01-14 | 安徽若水化工有限公司 | Low-density heat-conducting flame-retardant organic silicon material |
| CN115505270A (en) * | 2022-11-24 | 2022-12-23 | 武汉市三选科技有限公司 | Silicon-containing thermal interface material, preparation method thereof and chip packaging structure |
| CN116285875A (en) * | 2023-03-27 | 2023-06-23 | 湖北兴瑞硅材料有限公司 | Low-density heat-conducting organic silicon pouring sealant and preparation method thereof |
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| CN106279700A (en) * | 2016-08-08 | 2017-01-04 | 岳胜武 | Add-on type liquid silicon rubber viscosifier, preparation method and applications |
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| CN103351467A (en) * | 2013-07-18 | 2013-10-16 | 东莞市贝特利新材料有限公司 | Addition type liquid silicone rubber bonding accelerant and preparation method and application thereof |
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| CN110684357A (en) * | 2019-09-16 | 2020-01-14 | 安徽若水化工有限公司 | Low-density heat-conducting flame-retardant organic silicon material |
| CN115505270A (en) * | 2022-11-24 | 2022-12-23 | 武汉市三选科技有限公司 | Silicon-containing thermal interface material, preparation method thereof and chip packaging structure |
| CN116285875A (en) * | 2023-03-27 | 2023-06-23 | 湖北兴瑞硅材料有限公司 | Low-density heat-conducting organic silicon pouring sealant and preparation method thereof |
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