CN105713201A - Organosilicon bonding promoter for LED packaging high-refractive-index addition-type silica gel and preparation method and application of organosilicon bonding promoter - Google Patents
Organosilicon bonding promoter for LED packaging high-refractive-index addition-type silica gel and preparation method and application of organosilicon bonding promoter 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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl 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
- C08G77/08—Preparatory processes characterised by the catalysts used
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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
- 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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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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
Abstract
The invention discloses an organosilicon bonding promoter for LED packaging high-refractive-index addition-type silica gel and a preparation method and application of the organosilicon bonding promoter.According to the preparation method, an organosilicon compound containing hydroxyl and phenyl, epoxy silane, ester silane and a solvent are stirred to be uniform at room temperature, a titanate catalyst is added, a reaction is performed at the temperature of 25-60 DEG C for 6-15 h and continued at the vacuum degree of 0.05-0.098 MPa and the temperature of 60-140 DEG C for 2-6 h, and then the high-refractive-index organosilicon bonding promoter containing epoxy and ester is prepared.The prepared bonding promoter is high in refractive index, compatibility with the LED packaging high-refractive-index addition-type silica gel is good, the bonding performance, particularly with polyphthalamide, poly-1,4-cyclohexylene dimethylene terephthalate and polycarbonate, of the silica gel can be remarkably improved, and the promoter can be widely applied to the field of LED device packaging.
Description
Technical field
The present invention relates to organosilicon encapsulating material technical field, particularly relate to a kind of LED and encapsulate high index of refraction add-on type silica gel organosilicon adhesion promoters and preparation method thereof, this organosilicon adhesion promoters encapsulates in high index of refraction add-on type silica gel for LED.
Background technology
In order to improve stability and the reliability of LED component, it is necessary to device is packaged protection so that it is from the infringement of dampness, salt fog, dust, vibration and impact.When add-on type packaging silicon rubber solidifies, the consumption of catalyst is few, and no coupling product produces, energy deep cure, linear shrinkage is low, electrical insulation capability is excellent, and especially high index of refraction add-on type packaging silicon rubber can also be effectively improved light extraction efficiency, is one of high-performance package material.But, it is nonpolar organic group that add-on type packaging silicon rubber solidifies the rear surface overwhelming majority, the cementability of LED base material is poor, easily there is dead lamp phenomenon when crossing Reflow Soldering in the lamp bead of encapsulation, silica gel easily comes off from LED base material or support when being subject to thermal shock, has had a strong impact on the service life of LED component.
At present, the main method improving add-on type packaging silicon rubber adhesive property is to add adhesion promoters.US Patent No. 4311739 discloses the partial hydrolysate added containing C=C double bond alkoxy silane, it is possible to improve the add-on type silica gel adhesive property to base materials such as glass, rustless steel and copper.Chinese invention patent application CN103755963A reports a kind of polysiloxanes adhesion promoters containing acryloxy, epoxy radicals and isocyanurate group synthesized by hydrolytic condensation method, and this adhesion promoters can significantly improve the add-on type packaging silicon rubber adhesive property to aluminium flake and copper sheet.But there is hydrolysis-condensation reaction difficulty to control, be easily generated the shortcomings such as gel, and epoxide group easy open loop under strongly acidic conditions.
In recent years, along with the extensive use of high index of refraction add-on type packaging silicon rubber, the requirement of its adhesive property is also more and more higher.But, existing adhesion promoters addition is relatively big, and refractive index is low, poor with the high index of refraction add-on type packaging silicon rubber compatibility, and easily damages the curing performance of silica gel, light transmittance and mechanical property.
Summary of the invention
It is an object of the invention to for the deficiencies in the prior art, it is provided that a kind of organosilicon adhesion promoters that can significantly improve LED encapsulation high index of refraction add-on type silica gel adhesive property and preparation method thereof.
Another object of the present invention is in that to provide described organosilicon adhesion promoters to encapsulate the application in high index of refraction add-on type silica gel at LED.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method that LED encapsulates high index of refraction add-on type silica gel organosilicon adhesion promoters: hydroxyl and phenyl organo-silicon compound, epoxy radicals silicone hydride, ester group silane and solvent are at room temperature stirred, add the titanate catalyst of reactant gross mass 0.2%～5%, it is reaction 6～15h at 25～60 DEG C in temperature, then be 0.05～0.098MPa, temperature in vacuum it is continuation reaction 2～6h at 60～140 DEG C, obtains the high index of refraction organosilicon adhesion promoters containing epoxy radicals and ester group；
The general structure of described hydroxyl and phenyl organo-silicon compound is:
Wherein, Me is methyl, and Ph is phenyl, and a is 0～10, and b is 0～20, and c is 0～10, b+c > 0；
The mol ratio of described hydroxyl and phenyl organo-silicon compound and epoxy radicals silicone hydride and ester group silane total amount is 0.8:1～2.5:1；The mol ratio of described epoxy radicals silicone hydride and ester group silane is 0.3:1～5:1.
For realizing the object of the invention further, preferably, described epoxy radicals silicone hydride is 3 (2, 3 epoxy the third oxygen) propyl trimethoxy silicane, 3 (2, 3 epoxy the third oxygen) hydroxypropyl methyl dimethoxysilane, 3 (2, 3 epoxy the third oxygen) propyl-triethoxysilicane, 3 (2, 3 epoxy the third oxygen) hydroxypropyl methyl diethoxy silane, 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) ethyl trimethoxy silane, 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) ethyl-methyl dimethoxysilane, 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) ethyl triethoxysilane and 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) one or more in ethyl-methyl diethoxy silane.
Preferably, described solvent is one or more in toluene, dimethylbenzene, acetone, methanol, ethanol and isopropanol.
Preferably, described ester group silane is one or more in 3 methacryloxypropyl trimethoxy silane, 3 methacryloyloxypropyl methyl dimethoxysilane, 3 methacryloxypropyl and 3 methacryloyloxypropyl methyl diethoxy silanes.
Preferably, described titanate catalyst is one or more in tetraethyl titanate, metatitanic acid four n-propyl, tetraisopropyl titanate, tetra-n-butyl titanate, tetrabutyl titanate, metatitanic acid four tert-butyl ester, metatitanic acid four monooctyl ester, bis(acetylacetonate) titanium acid diisopropyl ester and two (ethyl acetoacetate) titanium diisopropyl ester.
Preferably, the mass ratio of described hydroxyl and phenyl organo-silicon compound and solvent is 0.4:1～2:1.
A kind of LED encapsulates high index of refraction add-on type silica gel organosilicon adhesion promoters, above-mentioned preparation method prepare.
Described organosilicon adhesion promoters encapsulates the application in high index of refraction add-on type silica gel at LED.Application process is preferably 1 acetenyl 1 Hexalin mix homogeneously of the Vinylphenyl silicon resin of 100 mass parts, the vinyl phenyl silicone oil of 5～60 mass parts, the phenyl hydrogen-containing silicon oil of 5～30 mass parts, the adhesion promoters of 0.8～6 mass parts and 0.002～0.02 mass parts, it is subsequently adding the platinum group catalyst of 0.05～0.5 mass parts, mix homogeneously, deaeration, at 60～100 DEG C, solidify 1～2h, then continue solidification 2～5h at 130～150 DEG C.The time of described deaeration is preferably 5～30min.
Organosilicon adhesion promoters of the present invention obtains with titanate esters for catalyst preparing, it is to avoid during with strong acid or highly basic for catalyst, the shortcoming of the easy open loop of epoxide group, and course of reaction relatively easily controls.Organosilicon adhesion promoters contains C=C double bond and polar group such as epoxy radicals, ester group etc. simultaneously, the former can participate in the curing reaction of add-on type packaging silicon rubber, the latter can form stronger interaction with base material, thus improve the adhesive property of add-on type LED packaging silicon rubber.Adhesion promoters makes it have high refractive index possibly together with phenyl chain link, and the compatibility encapsulating high index of refraction add-on type silica gel with LED is good.
Relative to prior art, present invention have the advantage that
1, the organosilicon adhesion promoters that prepared by the present invention, LED can be significantly improved and encapsulate the adhesive property of high index of refraction add-on type silica gel, the particularly adhesive property to plastic basis materials such as polyphthalamide (PPA), poly terephthalic acid Isosorbide-5-Nitrae cyclohexanedimethanoester ester (PCT) and Merlon (PC).Adding small amount (being generally less than 3 mass parts) organosilicon adhesion promoters in LED packaging silicon rubber, the adhesive strength of silica gel can improve more than 110%, especially the adhesive strength of PPA, PCT and PC base material is improve more than 240%.
2, the organosilicon adhesion promoters that prepared by the present invention, refractive index is high, and the compatibility encapsulating high index of refraction add-on type silica gel with LED is good and the performance impacts such as the light transmittance of silica gel, mechanical property and viscosity is less.
3, the preparation technology of the present invention is easy, it is easy to control, and to producing, equipment requirements is relatively low, and raw material is cheap and easy to get, it is easy to accomplish industrialized production, has a good application prospect.
Detailed description of the invention
For a better understanding of the present invention, below in conjunction with embodiment, the present invention is further illustrated, but embodiments of the present invention are not limited to this.
Embodiment 1
It is HO (MePhSiO) by 55.93g molecular formula5The phenyl hydroxy silicon oil of H, 11.82g3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, 12.42g3-methacryloxypropyl trimethoxy silane and 60g toluene adds the 250mL there-necked flask with thermometer, mechanical agitation and condensing reflux pipe, at room temperature stir, add 1.6g tetraisopropyl titanate, it is reaction 8h at 30 DEG C in temperature, then be 0.08MPa, temperature in vacuum being continue reaction 5h at 80 DEG C, obtain adhesion promoters 1, refractive index is 1.529.
By 1-acetenyl-1-Hexalin mix homogeneously under the effect of homogenizer of adhesion promoters 1 and 0.02 mass parts that 100 mass parts contents of ethylene to be the Vinylphenyl silicon resin of 4wt%, 15 mass parts viscosity the be vinyl phenyl silicone oil of 500mPa s, 30 mass parts active hydrogen content are the phenyl hydrogen-containing silicon oil of 0.45wt%, 3 mass parts, it is subsequently adding the platinum-methyl phenyl silicone coordination compound of 0.4 mass parts, mix homogeneously, deaeration 20min in vacuum drying oven, at 80 DEG C, solidify 1h, then continue to solidify 3h at 150 DEG C.The performance of sample is as shown in Table 1 and Table 2.
Embodiment 2
It is HO (Ph by 61.29g molecular formula2SiO)3The phenyl hydroxy silicon oil of H, 11.14g3-(2,3-epoxy the third oxygen) propyl-triethoxysilicane, 17.42g3-methacryloxypropyl and 150g dimethylbenzene adds the 500mL there-necked flask with thermometer, mechanical agitation and condensing reflux pipe, at room temperature stir, add 0.45g tetra-n-butyl titanate, it is reaction 6h at 50 DEG C in temperature, then be 0.06MPa, temperature in vacuum it is at 110 DEG C, continue reaction 3h, obtaining adhesion promoters 2, refractive index is 1.532.
By 1-acetenyl-1-Hexalin mix homogeneously under the effect of high speed dispersor of adhesion promoters 2 and 0.01 mass parts that 100 mass parts contents of ethylene to be the Vinylphenyl silicon resin of 2wt%, 6 mass parts viscosity the be vinyl phenyl silicone oil of 800mPa s, 14 mass parts active hydrogen content are the phenyl hydrogen-containing silicon oil of 0.3wt%, 2 mass parts, it is subsequently adding the platinum-methyl phenyl silicone coordination compound of 0.2 mass parts, mix homogeneously, deaeration 15min in vacuum drying oven, at 60 DEG C, solidify 2h, then continue to solidify 5h at 130 DEG C.The performance of sample is as shown in Table 1 and Table 2.
Embodiment 3
It is HO (MePhSiO) by 143.92g molecular formula4(Ph2SiO)2The phenyl hydroxy silicon oil of H, 19.71g2-(3,4-7-oxa-bicyclo[4.1.0 base) ethyl trimethoxy silane, 4.97g3-methacryloxypropyl trimethoxy silane and 350g toluene adds the 1000mL there-necked flask with thermometer, mechanical agitation and condensing reflux pipe, at room temperature stir, add 1.69g tetraethyl titanate, it is reaction 15h at 25 DEG C in temperature, then be 0.05MPa, temperature in vacuum it is at 140 DEG C, continue reaction 2h, obtaining adhesion promoters 3, refractive index is 1.538.
By 1-acetenyl-1-Hexalin mix homogeneously under the effect of high speed dispersor of adhesion promoters 3 and 0.008 mass parts that 100 mass parts contents of ethylene to be the Vinylphenyl silicon resin of 5wt%, 30 mass parts viscosity the be vinyl phenyl silicone oil of 2000mPa s, 25 mass parts active hydrogen content are the phenyl hydrogen-containing silicon oil of 0.6wt%, 6 mass parts, it is subsequently adding the platinum-methyl phenyl silicone coordination compound of 0.16 mass parts, mix homogeneously, deaeration 30min in vacuum drying oven, at 70 DEG C, solidify 1h, then continue to solidify 3h at 150 DEG C.The performance of sample is as shown in Table 1 and Table 2.
Embodiment 4
The present embodiment difference from Example 1 is in that 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane changes into 2-(3,4-7-oxa-bicyclo[4.1.0 base) ethyl triethoxysilane, and its consumption is 14.42g, preparing adhesion promoters 4, refractive index is 1.527.
Adhesion promoters 1 in embodiment 1 is changed into adhesion promoters 4, and its consumption is 4 mass parts.The performance of sample is as shown in Table 1 and Table 2.
Embodiment 5
The present embodiment difference from Example 2 is in that the consumption of adhesion promoters 2 is become 3 mass parts.The performance of sample is as shown in Table 1 and Table 2.
Comparative example 1
1-acetenyl-1-Hexalin mix homogeneously under the effect of high speed dispersor by phenyl hydrogen-containing silicon oil that 100 mass parts contents of ethylene to be the Vinylphenyl silicon resin of 4wt%, 15 mass parts viscosity the be vinyl phenyl silicone oil of 500mPa s, 30 mass parts active hydrogen content are 0.45wt% and 0.02 mass parts, it is subsequently adding the platinum-methyl phenyl silicone coordination compound of 0.4 mass parts, mix homogeneously, deaeration 20min in vacuum drying oven, at 80 DEG C, solidify 1h, then continue to solidify 3h at 150 DEG C.The performance of sample is as shown in Table 1 and Table 2.
Comparative example 2
1-acetenyl-1-Hexalin mix homogeneously under the effect of high speed dispersor by phenyl hydrogen-containing silicon oil that 100 mass parts contents of ethylene to be the Vinylphenyl silicon resin of 2%wt, 6 mass parts viscosity the be vinyl phenyl silicone oil of 800mPa s, 14 mass parts active hydrogen content are 0.3%wt and 0.01 mass parts, it is subsequently adding the platinum-methyl phenyl silicone coordination compound of 0.2 mass parts, mix homogeneously, deaeration 15min in vacuum drying oven, at 60 DEG C, solidify 2h, then continue to solidify 5h at 130 DEG C.The performance of sample is as shown in Table 1 and Table 2.
Comparative example 3
1-acetenyl-1-Hexalin mix homogeneously under the effect of high speed dispersor by phenyl hydrogen-containing silicon oil that 100 mass parts contents of ethylene to be the Vinylphenyl silicon resin of 5wt%, 30 mass parts viscosity the be vinyl phenyl silicone oil of 2000mPa s, 25 mass parts active hydrogen content are 0.6wt% and 0.008 mass parts, it is subsequently adding the platinum-methyl phenyl silicone coordination compound of 0.16 mass parts, mix homogeneously, deaeration 30min in vacuum drying oven, at 70 DEG C, solidify 1h, then continue to solidify 3h at 150 DEG C.The performance of sample is as shown in Table 1 and Table 2.
In table 1 and table 2, sample performance test methods is as follows:
1, measure LED according to GB/T2794 1995 and encapsulate the viscosity of add-on type silica gel.
2, measure LED according to GB/T2410 2008 and encapsulate the light transmittance of add-on type silica gel.
3, adhesion promoters and the refractive index of LED encapsulation add-on type silica gel are measured according to GB/T614 2006.
4, measure LED according to GB/T13936 1992 and encapsulate the bonding tensile shear strength of add-on type silica gel and base material.
5, measure LED according to GB/T528 2009 and encapsulate the hot strength of add-on type silica gel.
6, measure LED according to GB/T531.1 2008 and encapsulate the shore D hardness of add-on type silica gel.
Table 1
As it can be seen from table 1 when not adding organosilicon adhesion promoters, the adhesive property that LED encapsulates high index of refraction add-on type silica gel is poor, particularly to the adhesive strength of PPA, PCT and PC base material less than 0.63MPa (see comparative example 1-3).And after adding the adhesion promoters of present invention synthesis, LED encapsulates the adhesive property of high index of refraction add-on type silica gel and is obviously improved, its adhesive strength can improve more than 110%, and the adhesive strength of PPA, PCT and PC base material especially improves more than 240% (see embodiment 1-5).This contains C=C double bond mainly due to one side adhesion promoters and can react with the SiH key in silica gel, adhesion promoters contains the interaction that polar group such as epoxy radicals, ester group etc. can be stronger with base material formation on the other hand, so that silica gel has good adhesive property.Additionally, from table 2 it can be seen that addition adhesion promoters is less to the LED encapsulation viscosity of high index of refraction add-on type silica gel, refractive index, light transmittance and Effect on Mechanical Properties.
Table 2
Claims (10)
1.LED encapsulates the high index of refraction add-on type silica gel preparation method of organosilicon adhesion promoters, it is characterized in that: hydroxyl and phenyl organo-silicon compound, epoxy radicals silicone hydride, ester group silane and solvent are at room temperature stirred, add the titanate catalyst of reactant gross mass 0.2%～5%, it is reaction 6～15h at 25～60 DEG C in temperature, then be 0.05～0.098MPa, temperature in vacuum it is continuation reaction 2～6h at 60～140 DEG C, obtains the high index of refraction organosilicon adhesion promoters containing epoxy radicals and ester group；
The general structure of described hydroxyl and phenyl organo-silicon compound is:
Wherein, Me is methyl, and Ph is phenyl, and a is 0～10, and b is 0～20, and c is 0～10, b+c > 0；
The mol ratio of described hydroxyl and phenyl organo-silicon compound and epoxy radicals silicone hydride and ester group silane total amount is 0.8:1～2.5:1；The mol ratio of described epoxy radicals silicone hydride and ester group silane is 0.3:1～5:1.
2.LED encapsulates the high index of refraction add-on type silica gel preparation method of organosilicon adhesion promoters, it is characterized in that, described epoxy radicals silicone hydride is 3 (2, 3 epoxy the third oxygen) propyl trimethoxy silicane, 3 (2, 3 epoxy the third oxygen) hydroxypropyl methyl dimethoxysilane, 3 (2, 3 epoxy the third oxygen) propyl-triethoxysilicane, 3 (2, 3 epoxy the third oxygen) hydroxypropyl methyl diethoxy silane, 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) ethyl trimethoxy silane, 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) ethyl-methyl dimethoxysilane, 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) ethyl triethoxysilane and 2 (3, 4 7-oxa-bicyclo[4.1.0 bases) one or more in ethyl-methyl diethoxy silane.
3.LED encapsulates the high index of refraction add-on type silica gel preparation method of organosilicon adhesion promoters, it is characterised in that described solvent is one or more in toluene, dimethylbenzene, acetone, methanol, ethanol and isopropanol.
4.LED encapsulates the high index of refraction add-on type silica gel preparation method of organosilicon adhesion promoters, it is characterized in that, described ester group silane is one or more in 3 methacryloxypropyl trimethoxy silane, 3 methacryloyloxypropyl methyl dimethoxysilane, 3 methacryloxypropyl and 3 methacryloyloxypropyl methyl diethoxy silanes.
5.LED encapsulates the high index of refraction add-on type silica gel preparation method of organosilicon adhesion promoters, it is characterized in that, described titanate catalyst is one or more in tetraethyl titanate, metatitanic acid four n-propyl, tetraisopropyl titanate, tetra-n-butyl titanate, tetrabutyl titanate, metatitanic acid four tert-butyl ester, metatitanic acid four monooctyl ester, bis(acetylacetonate) titanium acid diisopropyl ester and two (ethyl acetoacetate) titanium diisopropyl ester.
6.LED encapsulates the high index of refraction add-on type silica gel preparation method of organosilicon adhesion promoters, it is characterised in that the mass ratio of described hydroxyl and phenyl organo-silicon compound and solvent is 0.4:1～2:1.
7.LED encapsulates high index of refraction add-on type silica gel organosilicon adhesion promoters, it is characterised in that its preparation method described in claim 1 prepares.
8. organosilicon adhesion promoters described in claim 7 encapsulates the application in high index of refraction add-on type silica gel at LED.
9. organosilicon adhesion promoters according to claim 8 encapsulates the application in high index of refraction add-on type silica gel at LED, it is characterized in that, the 1 acetenyl 1 Hexalin mix homogeneously by the Vinylphenyl silicon resin of 100 mass parts, the vinyl phenyl silicone oil of 5～60 mass parts, the phenyl hydrogen-containing silicon oil of 5～30 mass parts, the adhesion promoters of 0.8～6 mass parts and 0.002～0.02 mass parts, it is subsequently adding the platinum group catalyst of 0.05～0.5 mass parts, mix homogeneously, deaeration, at 60～100 DEG C, solidify 1～2h, then continue solidification 2～5h at 130～150 DEG C.
10. organosilicon adhesion promoters according to claim 9 encapsulates the application in high index of refraction add-on type silica gel at LED, it is characterised in that the time of described deaeration is 5～30min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108129845A (en) * | 2017-12-23 | 2018-06-08 | 广东新翔星科技股份有限公司 | A kind of preparation method of additional organosilicon packaging plastic adhesion promoters |
| CN108517036A (en) * | 2018-04-25 | 2018-09-11 | 广州惠利电子材料有限公司 | A kind of synthetic method of phenyl hydrogen-containing silicon oil |
| CN109054731A (en) * | 2018-08-03 | 2018-12-21 | 广东新翔星科技股份有限公司 | A kind of cementability high refractive index additional organosilicon packaging plastic and preparation method thereof |
| CN112322221A (en) * | 2020-11-28 | 2021-02-05 | 唐山三友硅业有限责任公司 | Tackifier and preparation method thereof, method for preparing adhesive pouring sealant for power adapter by using tackifier and pouring sealant |
| CN115926169A (en) * | 2019-03-22 | 2023-04-07 | 三菱瓦斯化学株式会社 | Method for producing polycarbonate copolymer and polysiloxane compound, polycarbonate copolymer, polysiloxane compound, composition, and molded article |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775611A (en) * | 2012-07-24 | 2012-11-14 | 东莞兆舜有机硅新材料科技有限公司 | Tackifier and production method thereof |
| CN104650795A (en) * | 2015-03-05 | 2015-05-27 | 江西欧普特实业有限公司 | Preparation method and application of organosilicone pouring sealant adhesive |
| CN104774333A (en) * | 2015-04-30 | 2015-07-15 | 绵阳惠利电子材料有限公司 | Addition type organic silicon rubber tackifier, preparation method and application thereof |
| CN104877139A (en) * | 2015-05-14 | 2015-09-02 | 深圳新宙邦科技股份有限公司 | Tackifier for LED packaging adhesive and preparation method of tackifier |
-
2016
- 2016-02-04 CN CN201610080932.0A patent/CN105713201A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775611A (en) * | 2012-07-24 | 2012-11-14 | 东莞兆舜有机硅新材料科技有限公司 | Tackifier and production method thereof |
| CN104650795A (en) * | 2015-03-05 | 2015-05-27 | 江西欧普特实业有限公司 | Preparation method and application of organosilicone pouring sealant adhesive |
| CN104774333A (en) * | 2015-04-30 | 2015-07-15 | 绵阳惠利电子材料有限公司 | Addition type organic silicon rubber tackifier, preparation method and application thereof |
| CN104877139A (en) * | 2015-05-14 | 2015-09-02 | 深圳新宙邦科技股份有限公司 | Tackifier for LED packaging adhesive and preparation method of tackifier |
Cited By (7)
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|---|---|---|---|---|
| CN108129845A (en) * | 2017-12-23 | 2018-06-08 | 广东新翔星科技股份有限公司 | A kind of preparation method of additional organosilicon packaging plastic adhesion promoters |
| CN108129845B (en) * | 2017-12-23 | 2021-01-05 | 广东新翔星科技股份有限公司 | Preparation method of adhesion promoter for addition type organic silicon packaging adhesive |
| CN108517036A (en) * | 2018-04-25 | 2018-09-11 | 广州惠利电子材料有限公司 | A kind of synthetic method of phenyl hydrogen-containing silicon oil |
| CN109054731A (en) * | 2018-08-03 | 2018-12-21 | 广东新翔星科技股份有限公司 | A kind of cementability high refractive index additional organosilicon packaging plastic and preparation method thereof |
| CN115926169A (en) * | 2019-03-22 | 2023-04-07 | 三菱瓦斯化学株式会社 | Method for producing polycarbonate copolymer and polysiloxane compound, polycarbonate copolymer, polysiloxane compound, composition, and molded article |
| CN115926169B (en) * | 2019-03-22 | 2024-03-22 | 三菱瓦斯化学株式会社 | Method for producing polysiloxane compound, composition, and molded article |
| CN112322221A (en) * | 2020-11-28 | 2021-02-05 | 唐山三友硅业有限责任公司 | Tackifier and preparation method thereof, method for preparing adhesive pouring sealant for power adapter by using tackifier and pouring sealant |
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