CN106810698A - A kind of epoxy silicones tackifier and its organosilicon thermal conductive insulation glue of preparation - Google Patents
A kind of epoxy silicones tackifier and its organosilicon thermal conductive insulation glue of preparation Download PDFInfo
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- CN106810698A CN106810698A CN201611259815.7A CN201611259815A CN106810698A CN 106810698 A CN106810698 A CN 106810698A CN 201611259815 A CN201611259815 A CN 201611259815A CN 106810698 A CN106810698 A CN 106810698A
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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
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- 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
- 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
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Abstract
The organosilicon thermal conductive insulation glue of preparation and its preparation of the present invention on a kind of epoxy silicones tackifier, the tackifier are that hydrolytic condensation is formed in acid condition by the siloxanes of vinylsiloxane and epoxy radicals, and the tackifier and vinyl silicone oil, catalyst, containing hydrogen silicone oil and heat filling are obtained into organosilicon thermal conductive insulation glue by mixing vacuum defoamation elevated cure.Epoxide group is incorporated into the present invention side chain of containing hydrogen silicone oil by Si―H addition reaction, tackifier are bad with matrix resin compatibility before solving the problems, such as, the organosilicon thermal conductive insulation glue that the tackifier are used to prepare overcomes the aging defect of the poor heat resistance of traditional epoxy-based material, easy xanthochromia, prepared organosilicon thermal conductive insulation glue energy normal temperature is preserved, and has the advantages that heat-resist, mechanical strength is high, caking property is good.
Description
Technical field
The invention belongs to technical field of semiconductor illumination, and in particular to a kind of epoxy silicones tackifier preparation and
Its organosilicon thermal conductive insulation glue for preparing.
Background technology
As long as having epoxies and organic silicon currently used for the binding material between chip and base material.Epoxies has good
Caking property, chemical resistance and excellent mechanical property etc..But, in use find epoxy systems meeting by
Gradually there is xanthochromia and melanism, significantly reduce light output efficiency so as to have impact on the reliability requirement of whole device.
In order to solve these problems, Dow corning, Japanese SHIN-ETSU HANTOTAI, Wan Neidengduo companies have studied and use organosilicon
Instead of traditional epoxy material.Because organosilicon has good heat resistance and uvioresistant performance, disclosure satisfy that powerful
It is required that.But the thermal conductive insulation glue of organic silicon has that mechanical property is not good enough, adhesive property is bad, such as
Mentioned in two documents of CN201410035224 and CN200910251588, CN201410035224 needs to add titanate esters conduct
Tackifier increase the adhesion strength between chip and support, the preservation of this organic silica gel synthesized in CN200910251588
Condition requirement low temperature.Tackifier and matrix resin are likely to occur therebetween the problem of phase separation, this influence indirectly heat resistance with
And the light output performance of device.And preservation condition requirement low temperature, this is also a big problem for the consumption of the energy.
The content of the invention
A kind of defect it is an object of the invention to overcome prior art, there is provided epoxy silicones tackifier.
Another object of the present invention is to provide organosilicon heat conduction prepared by a kind of above-mentioned epoxy silicones tackifier
Insulating cement.
The purpose of the present invention is achieved through the following technical solutions：
A kind of epoxy silicones tackifier, are in the lower water in pH=4~6 by vinylsiloxane with epoxy radical siloxane
Solution condensation is formed, and it has following structure：
Wherein R1=-H ,-CH3Or-CH2CH3；N=1~5, m=1~5.
Preferably, the vinylsiloxane and the mol ratio of epoxy radical siloxane are 1~4:1.
Preferably, described vinylsiloxane is vinyltrimethoxy silane, vinyl-dimethyl Ji Jia, ethyoxyl silicon
Alkane, 3- (isobutene acyl-oxygen) propyl group front three, Ethoxysilane more than one.
Preferably, described epoxy radical siloxane is γ-glycidyl ether oxygen propyl trimethoxy silicane, (3- of 1,3- bis-
Glycidylpropyl) -1,1,3,3- tetramethyl disiloxanes or γ-(2,3- glycidoxies) propyl-triethoxysilicane one
More than kind.
The above-mentioned preparation method for epoxy silicones tackifier, comprises the following steps：
S1. after vinylsiloxane being dissolved in into organic solvent, epoxy radical siloxane is instilled at 40~45 DEG C and is had
In the mixed liquor of machine solvent, while instilling HCl, after after completion of dropping, being warming up to 60~70 DEG C, 12~16h is reacted.
S2. step S1 products therefroms are washed with deionized water to neutrality, the lower floor's product that then will be separated, in 60~70 DEG C
12~16h of lower vacuum drying, obtains epoxy silicones tackifier.
Preferably, organic solvent described in step S1 is tetrahydrofuran, dimethylformamide or toluene.
Preferably, the mass ratio of vinylsiloxane, epoxy radical siloxane and organic solvent described in step S1 for (1~
3):2:10, the time of dropwise addition is 2~5h.
A kind of organosilicon thermal conductive insulation glue prepared with above-mentioned epoxy silicones tackifier, in parts by weight, including with
Lower component：0~30 part of vinyl silicone oil, 50~70 parts of containing hydrogen silicone oil, the component of tackifier 10~20,0.05~1 part of catalyst is led
10~30 parts of hot filler.
Preferably, described catalyst is Karstedt catalyst, and the Pt contents in the Karstedt catalyst exist
Between 1000~5000ppm.
Preferably, described heat filling is one or more of carborundum, aluminium nitride, aluminum oxide or boron nitride.
The present invention is the organosiloxane with epoxide group, this new tackifier by designing the tackifier of synthesis
Compared with traditional tackifier, due to the presence of epoxide group, chemical bond can be formed with base material (such as aluminium flake, copper sheet).Make it
Compatibility with organic silicon substrate resin is more preferable, is not in the problem of phase separation, it is to avoid the situation for bonding damage layer occur.This
The organic silicon rigidity-increasing stick of invention can carry out Si―H addition reaction with containing hydrogen silicone oil, and to form the side chain organosilicon heat conduction that contains epoxide group exhausted
Edge glue, has excellent adhesive property, high temperature resistant and mechanical property, and can apply in normal temperature storage after mixing according to formula design
Organosilicon thermal conductive insulation glue, solve that organosilicon thermal conductive insulation glue adhesive property is poor, need the shortcoming of Cord blood.
Compared with prior art, the present invention has advantages below and beneficial effect：
1. the present invention is the organosiloxane class with epoxy radicals by the tackifier that autonomous Design synthesizes, make tackifier and
Organic silicon substrate resin has preferable compatibility.And the organosilicon heat conductive insulating that it is mixed to get with catalyst and heat filling
Glue has excellent adhesive property, hardness high, heat-resist, solve at present with epoxy resin as material of main part at high temperature
Xanthochromia and melanism problem.
2. present invention gained epoxy silicones tackifier are used to prepare organosilicon thermal conductive insulation glue, can lead in solidification
Cross Si―H addition reaction to be linked with containing hydrogen silicone oil crosslinking agent, epoxide group is introduced on side chain, by increasing capacitance it is possible to increase adhesive property.Institute
, without Cord blood, easy to use, condition of cure is gentle the organosilicon thermal conductive insulation glue of system, it is to avoid more in use
Unnecessary waste, reduces cost.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
1. 3- (isobutene acyl-oxygen) propyl trimethoxy silicanes of 4.924g (20mmol) and 20ml solvent DMFs are added three
In mouthful flask, and at 40 DEG C after 4.728g (20mol) γ-glycidyl ether oxygen propyl trimethoxy silicane is mixed with 5mlDMF
Lower constant pressure funnel is added dropwise in there-necked flask, while instilling the 0.3gHCl of dilution.After after completion of dropping, 60 are warming up to
DEG C, react 12h.Washing dries 12h and obtains prepolymer for epoxy silicones tackifier to neutrality, is designated as 2K-1.
2. by vinyl silicone oil (contents of ethylene=0.6%), the 2.5g containing hydrogen silicone oils of 1.2g tackifier 2K-1 and 1.5g
And after the 0.5umAlN of 1.0g is mixed in beaker, the Pt contents of 0.06g are added for the Karstedt of 3000ppm is urged
Agent, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in poly- Teflon mould, 90 DEG C of precuring 1h, then rises
Temperature obtains organosilicon thermal conductive insulation glue to 130 DEG C of solidification 2.5h.
Organosilicon thermal conductive insulation glue performance test：Hardness 92A, shear tension intensity 3.8MPa, temperature when weight-loss ratio is 5%
It is 425 DEG C to spend, thermal conductivity factor 0.75.Room temperature hardness above-mentioned after 5 months, shear tension intensity and weight-loss ratio keep substantially
It is constant.
Embodiment 2
1. 3- (isobutene acyl-oxygen) propyl trimethoxy silicanes of 4.924g (20mmol) and 20ml solvent DMFs are added three
In mouthful flask, and after 5.568g (20mol) γ-(2,3- glycidoxy) propyl-triethoxysilicane is mixed with 5mlDMF
It is added dropwise in there-necked flask with constant pressure funnel at 40 DEG C, while instilling the 0.3gHCl of dilution.After after completion of dropping, heat up
To 60 DEG C, 12h is reacted.Washing dries 14h and obtains prepolymer for epoxy silicones tackifier to neutrality, is designated as 3K-1.
2. by vinyl silicone oil (contents of ethylene=0.6%), the 2.5g containing hydrogen silicone oils of 1.2g tackifier 3K-1 and 1.5g
And after 0.5 μm of AlN of 1.0g is mixed in beaker, the Pt contents of 0.06g are added for the Karstedt of 3000ppm is urged
Agent, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in poly- Teflon mould, 90 DEG C of precuring 1h, then rises
Temperature obtains organosilicon thermal conductive insulation glue to 130 DEG C of solidification 2.5h.
The hardness of the organosilicon thermal conductive insulation glue for obtaining is 85A, shear tension intensity 3.5MPa, and weightlessness is 5% temperature
It is 418 DEG C, thermal conductivity factor 0.698.Room temperature hardness above-mentioned after 5 months, shear tension intensity and weight-loss ratio keep substantially
It is constant.Compare with embodiment 1, it can be seen that effect and the 2K-1 difference of the thermal conductive insulation glue prepared using this kind of tackifier are not
Greatly, properties 2K-1's is more preferable but in the case of equal consumption.
Embodiment 3
1. 3- (isobutene acyl-oxygen) propyl-triethoxysilicanes of 5.764g (20mmol) and 20ml solvent DMFs are added three
In mouthful flask, and after 5.568g (20mol) γ-(2,3- glycidoxy) propyl-triethoxysilicane is mixed with 5mlDMF
It is added dropwise in there-necked flask with constant pressure funnel at 40 DEG C, while instilling the 0.3gHCl of dilution.After after completion of dropping, heat up
To 60 DEG C, 12h is reacted.Washing dries 16h and obtains prepolymer for epoxy silicones tackifier to neutrality, is designated as 4K-1.
2. by vinyl silicone oil (contents of ethylene=0.6%), the 2.5g containing hydrogen silicone oils of 1.2g tackifier 4K-1 and 1.5g
And after the 0.5umAlN of 1.0g is mixed in beaker, the Pt contents of 0.06g are added for the Karstedt of 3000ppm is urged
Agent, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in Teflon mould, 90 DEG C of precuring 1h, then heats up
To 130 DEG C of solidification 2.5h, organosilicon thermal conductive insulation glue is obtained.
The hardness of the organosilicon thermal conductive insulation glue for obtaining is 80A, shear tension intensity 3.2MPa, temperature when weightless 5%
It is 410 DEG C, thermal conductivity factor 0.668.Room temperature hardness above-mentioned after 5 months, shear tension intensity and weight-loss ratio keep substantially
It is constant.Compare with embodiment 1~2, it can be seen that the thermal conductive insulation glue prepared using this kind of tackifier in the case of equal consumption
Effect differing greatly than 2K-1 and 3K-1, the very big reduction of what mechanical property and heat conductivility all occurred.
Embodiment 4
1. by 3- (isobutene acyl-oxygen) propyl trimethoxy silicanes of 4.924g (20mmol) and 20ml solvents tetrahydrofuranes
(THF) in adding there-necked flask, and by 2.364g (10mol) γ-glycidyl ether oxygen propyl trimethoxy silicane and 5ml THF
It is added dropwise in there-necked flask with constant pressure funnel at 40 DEG C after mixing, the mol ratio of the two is 2:1, while instilling dilution
0.3g HCl.After after completion of dropping, being warming up to 60 DEG C, 12h is reacted.
2. after reaction terminates, it is washed with deionized water to neutrality, lower floor's product is separated with separatory funnel, it is dry in vacuum at 60 DEG C
Dry 12h, the viscous prepolymer of gained water white transparency is epoxy silicones tackifier, is designated as 2K-2.
3. by vinyl silicone oil (contents of ethylene=0.6%), the 2.5g containing hydrogen silicone oils of 0.5g tackifier 2K-2 and 1.5g
And after the 0.5um aluminium nitride (AlN) of 1.0g is mixed in beaker, it is 3000ppm's to add the Pt contents of 0.06g
Karstedt catalyst, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in poly- Teflon mould, and 90 DEG C pre-
Solidification 1h, then 130 DEG C of solidification 2.5h are warming up to, obtain organosilicon thermal conductive insulation glue.
The performance test of organosilicon thermal conductive insulation glue：Hardness 75A, shear tension intensity 2.3MPa, temperature when weightless 5%
It is 380 DEG C, thermal conductivity factor 0.48.Room temperature hardness above-mentioned after 5 months, shear tension intensity and weight-loss ratio keep not substantially
Become.
Difference with embodiment 1 is：With example 1 contrast find, in embodiment 1 gained thermal conductive insulation glue hardness with
And tensile strength is higher, heat conductivility is more preferable.Result shows that the ratio for increasing tackifier epoxide epoxy group group is favorably improved heat conduction
The mechanical property and heat conductivility of insulating cement.
Embodiment 5
Difference with embodiment 2 is：
Preceding step with embodiment 2, by the vinyl silicone oil of 1.2g tackifier 3K-1 and 1.5g (contents of ethylene=
0.6%) after, the 2.0umAlN of 2.5g containing hydrogen silicone oils and 1.0g is mixed in beaker, the Pt contents for adding 0.06g are
The Karstedt catalyst of 3000ppm, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in poly- Teflon mould
In, 90 DEG C of precuring 1h, then 130 DEG C of solidification 2.5h are warming up to, obtain organosilicon thermal conductive insulation glue.
The hardness of the organosilicon thermal conductive insulation glue for obtaining is 88A, shear tension intensity 3.7MPa, and weightlessness is 5% temperature
It is 426 DEG C, thermal conductivity factor 0.728.Room temperature hardness above-mentioned after 5 months, shear tension intensity and weight-loss ratio keep substantially
It is constant.
Compare with embodiment 2, with the increase of the AlN particle diameters of heat filling, what is prepared in the presence of tackifier of the same race leads
The thermal conductivity of heat insulation glue is significantly improved.
Embodiment 6
Difference with embodiment 2 is：
Preceding step with embodiment 2, by the vinyl silicone oil of 1.2g tackifier 3K-1 and 1.5g (contents of ethylene=
0.6%) after, the 1.0umSiC of 2.5g containing hydrogen silicone oils and 1.0g is mixed in beaker, the Pt contents for adding 0.06g are
The Karstedt catalyst of 3000ppm, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in poly- Teflon mould
In, 90 DEG C of precuring 1h, then 130 DEG C of solidification 2.5h are warming up to, obtain organosilicon thermal conductive insulation glue.
The hardness of the organosilicon thermal conductive insulation glue for obtaining is 82A, shear tension intensity 3.3MPa, and weightlessness is 5% temperature
It is 436 DEG C, thermal conductivity factor 0.658.Room temperature hardness above-mentioned after 5 months, shear tension intensity and weight-loss ratio keep substantially
It is constant.
Compare with embodiment 2, heat filling is for the thermal conductive insulation glue of SiC and using the thermal conductive insulation glue pair prepared by AlN
Than finding, in addition to heat resistance will get well than the latter, remaining properties all decreases compared with AlN, illustrates that AlN can conduct for the former
More preferably heat filling.
Embodiment 7
Difference with embodiment 3 is：
1. 3- (isobutene acyl-oxygen) propyl-triethoxysilicanes of 5.764g (20mmol) and 20ml solvents THF are added three
In mouthful flask, and after 5.568g (20mol) γ-(2,3- glycidoxy) propyl-triethoxysilicane is mixed with 5mlTHF
It is added dropwise in there-necked flask with constant pressure funnel at 40 DEG C, while instilling the 0.3gHCl of dilution.After after completion of dropping, heat up
To 60 DEG C, 16h is reacted.Washing is dry that prepolymer is epoxy silicones tackifier to neutrality, is designated as 5K-1.
2. by vinyl silicone oil (contents of ethylene=0.6%), the 2.5g containing hydrogen silicone oils of 1.2g tackifier 5K-1 and 1.5g
And after the 0.5umAlN of 1.0g is mixed in beaker, the Pt contents of 0.06g are added for the Karstedt of 3000ppm is urged
Agent, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in Teflon mould, 90 DEG C of precuring 1h, then heats up
To 130 DEG C of solidification 2.5h, organosilicon thermal conductive insulation glue is obtained.
The hardness of the organosilicon thermal conductive insulation glue for obtaining is 84A, shear tension intensity 3.5MPa, temperature when weightless 5%
It is 416 DEG C, thermal conductivity factor 0.688.Room temperature hardness above-mentioned after 5 months, shear tension intensity and weight-loss ratio keep substantially
It is constant.Compare with embodiment 3, it can be seen that the effect of the thermal conductive insulation glue prepared using this kind of tackifier in the case of equal consumption
Fruit slightly being lifted than 4K-1, it may be possible to because the extension in reaction time causes epoxy radical siloxane and vinylsiloxane water
Solution is more abundant, and structure is more tight, and the density of epoxide group is bigger so that prepare thermal conductive insulation glue mechanical property with
And heat conductivility all occurs in that less lifting.
Embodiment 8
Difference with embodiment 1 is：
The step 3 is：By the vinyl silicone oil (contents of ethylene=0.6%) of 0.8g tackifier 2K-1 and 1.5g,
After 0.5 μm of aluminium nitride (AlN) of 2.5g containing hydrogen silicone oils and 1.0g is mixed in beaker, the Pt contents of 0.06g are added
It is the Karstedt catalyst of 4000ppm, is placed in normal temperature deaeration 30min in vacuum drying chamber, pours in poly- polytetrafluoroethylene (PTFE) mould
In tool, 90 DEG C of precuring 1h, then 130 DEG C of solidification 2.5h are warming up to, obtain organosilicon thermal conductive insulation glue.
Organosilicon thermal conductive insulation glue performance test：Hardness 82A, shear tension intensity 2.9MPa, temperature when weightless 5% is
410 DEG C, thermal conductivity factor 0.68.5 months properties above-mentioned afterwards of room temperature are held essentially constant.
Embodiment 8
Difference with embodiment 1 is：
The step 3 is：By the vinyl silicone oil (contents of ethylene=0.6%) of 1.5g tackifier 2K-1 and 1.5g,
After 0.5 μm of AlN of 2.5g containing hydrogen silicone oils and 1.0g is mixed in beaker, the Pt contents for adding 0.06g are 5000ppm
Karstedt catalyst, be placed in normal temperature deaeration 30min in vacuum drying chamber, pour in Teflon mould, 90 DEG C are pre-
Solidification 1h, then 130 DEG C of solidification 2.5h are warming up to, obtain organosilicon thermal conductive insulation glue.
Organosilicon thermal conductive insulation glue performance test：Hardness 75A, shear tension intensity 3.0MPa, temperature when weightless 5% is
406 DEG C, thermal conductivity factor 0.65.Room temperature 5 months hardness above-mentioned afterwards, shear tension intensity and weight-loss ratios keep not substantially
Become.
Being stepped up with tackifier 2K-1 consumptions is can be seen that from embodiment 7~8, the thermal conductive insulation glue of preparation
Mechanical property and heat conductivility can be lifted accordingly, and performance is optimal on the basis of consumption 1.2g.But with consumption
Further increase performance can decline.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine and simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of epoxy silicones tackifier, it is characterised in that the tackifier are by vinylsiloxane and epoxy radicals
Siloxanes is formed in the lower hydrolytic condensation in pH=4~6, and it has following structure：
Wherein R1=-H ,-CH3Or-CH2CH3；N=1~5, m=1~5.
2. epoxy silicones tackifier according to claim 1, it is characterised in that the vinylsiloxane and epoxy
The mol ratio of radical siloxane is 1~4:1.
3. epoxy silicones tackifier according to claim 1, it is characterised in that described vinylsiloxane is second
Alkenyl trimethoxy silane, vinyl-dimethyl Ji Jia, Ethoxysilane, 3- (isobutene acyl-oxygen) propyl group front three, Ethoxysilane
More than one.
4. epoxy silicones tackifier according to claim 1, it is characterised in that described epoxy radical siloxane is
γ-glycidyl ether oxygen propyl trimethoxy silicane, 1,3- bis- (3- glycidylpropyls) -1,1,3,3- tetramethyl disiloxanes
Or γ-(2,3- glycidoxies) propyl-triethoxysilicane more than one.
5. the preparation method of the epoxy silicones tackifier according to claim any one of 1-4, it is characterised in that including
Following steps：
S1. after vinylsiloxane being dissolved in into organic solvent, epoxy radical siloxane is instilled at 40~45 DEG C molten with organic
In the mixed liquor of agent, while instilling HCl, time for adding is 2~5h, is warming up to 60~70 DEG C after completion of dropping, reaction 12~
16h。
S2. step S1 products therefroms are washed with deionized water to neutrality, the lower floor's product that then will be separated, in true at 60~70 DEG C
Sky dries 12~16h, obtains epoxy silicones tackifier.
6. the preparation method of epoxy silicones tackifier according to claim 5, it is characterised in that described in step S1
Organic solvent is tetrahydrofuran, dimethylformamide or toluene.
7. the preparation method of epoxy silicones tackifier according to claim 5, it is characterised in that described in step S1
The mass ratio of vinylsiloxane, epoxy radical siloxane and organic solvent is (1~3):2:10, the time of dropwise addition is 2~5h.
8. the organosilicon thermal conductive insulation glue that prepared by tackifier described in a kind of any one of claim 1-4, it is characterised in that with weight
Part meter, including following components：0~30 part of vinyl silicone oil, 50~70 parts of containing hydrogen silicone oil, the component of tackifier 10~20, catalyst
0.05~1 part, 10~30 parts of heat filling.
9. organosilicon thermal conductive insulation glue according to claim 8, it is characterised in that described catalyst is urged for Karstedt
Agent, the Pt contents in the Karstedt catalyst are between 1000~5000ppm.
10. organosilicon thermal conductive insulation glue according to claim 8, it is characterised in that described heat filling be carborundum,
One or more of aluminium nitride, aluminum oxide or boron nitride.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397771A (en) * | 2016-09-08 | 2017-02-15 | 烟台德邦先进硅材料有限公司 | Preparation method of tackifier used for organosilicone LED packaging colloidal system |
| CN108976814A (en) * | 2018-08-08 | 2018-12-11 | 四川大学 | A kind of heat-resisting liquid silastic improving intensity and interfacial adhesion |
| CN114656884A (en) * | 2021-10-18 | 2022-06-24 | 广东思泉新材料股份有限公司 | Organic silicon heat-conducting insulating film and preparation method thereof |
| CN114835901A (en) * | 2022-06-17 | 2022-08-02 | 四川大学 | Epoxy modified vinyl silicone rubber and preparation method and application thereof |
| CN115583963A (en) * | 2022-12-06 | 2023-01-10 | 桂林宝龙达新材料有限公司 | Phenyl organosilicon tackifier and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2012007126A (en) * | 2010-06-28 | 2012-01-12 | Aica Kogyo Co Ltd | Addition-type silicone resin composition |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397771A (en) * | 2016-09-08 | 2017-02-15 | 烟台德邦先进硅材料有限公司 | Preparation method of tackifier used for organosilicone LED packaging colloidal system |
| CN108976814A (en) * | 2018-08-08 | 2018-12-11 | 四川大学 | A kind of heat-resisting liquid silastic improving intensity and interfacial adhesion |
| CN108976814B (en) * | 2018-08-08 | 2023-07-04 | 四川大学 | Heat-resistant liquid silicone rubber with improved strength and interface bonding performance |
| CN114656884A (en) * | 2021-10-18 | 2022-06-24 | 广东思泉新材料股份有限公司 | Organic silicon heat-conducting insulating film and preparation method thereof |
| CN114835901A (en) * | 2022-06-17 | 2022-08-02 | 四川大学 | Epoxy modified vinyl silicone rubber and preparation method and application thereof |
| CN115583963A (en) * | 2022-12-06 | 2023-01-10 | 桂林宝龙达新材料有限公司 | Phenyl organosilicon tackifier and preparation method thereof |
| CN115583963B (en) * | 2022-12-06 | 2024-04-16 | 桂林宝龙达新材料有限公司 | Phenyl organosilicon tackifier and preparation method thereof |
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Application publication date: 20170609 |