CN105400446B - A kind of high refractive index LED liquid casting glue tackifier and preparation method thereof - Google Patents
A kind of high refractive index LED liquid casting glue tackifier and preparation method thereof Download PDFInfo
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- CN105400446B CN105400446B CN201510949866.1A CN201510949866A CN105400446B CN 105400446 B CN105400446 B CN 105400446B CN 201510949866 A CN201510949866 A CN 201510949866A CN 105400446 B CN105400446 B CN 105400446B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
Abstract
The present invention provides high refractive index LED liquid casting glue tackifier and preparation method thereof, the preparation method is using the organosiloxane with hydrolyzable alkoxy grp as monomer, under organic solvent dispersion, cohydrolysis polycondensation under the action of catalyst, a kind of water white transparency polymethyl-benzene base silicones oligomer solution is obtained after washing, then by polymethyl-benzene base silicones oligomer solution and with active function group silane coupling agent, under the effect of the catalyst, ester exchange reaction occurs, after filtering or catalyst neutralisation, after removed under reduced pressure lower-molecular substance, a kind of suitable high refractive index LED liquid casting glue tackifier are prepared.The tackifier refractive index of the present invention is greater than or equal to 1.50, has good compatibility with high refractive index LED liquid casting glues.The present invention has many advantages, such as simple for process, reproducible and structural controllability.The tackifier of the present invention can play an important role in the encapsulation field of LED light emitting diodes.
Description
Technical field
The present invention relates to tackifier technical field more particularly to a kind of high refractive index LED liquid casting glue tackifier and
Preparation method.
Background technology
Add-on type high refractive index LED liquid casting glue not only has in general add-on type liquid silicon rubber sulfidation without pair
The advantages that product, shrinking percentage are low and energy profound level cures, also has light transmittance high, refractive index is big, and thermal stability is good, stress
It is small, it the features such as hygroscopicity is low, is rapidly developed recently in LED Packaging Industries.Equally, add-on type high refractive index LED liquid fills
Sealing after hardening also have general liquid silastic surface energy it is low, with metal base (copper, aluminium, silver, gold and stainless steel etc.) and
The poor problem of the adhesive property of non-metallic substrate (PC, PBT, nylon and pcb board etc.).In view of practical application LED was encapsulated
It is always the research that this bonds field that embedding glue sticking requires higher, the exploitation of corresponding tackifier to substrate bonding in journey
Hot spot and difficult point.
Currently, it is similar with usual silicone rubber, it is bonding with a variety of materials to improve add-on type high refractive index LED liquid casting glue
There are mainly three types of the methods of property：First, pre-processed to substrate surface using silane coupling agent, the method increase production process and
Production time can especially greatly reduce production efficiency when producing LED lamp bead in enormous quantities and increase Material Cost, while bottom
Paint uses flammable solvent more, causes peril of transportation and environmental pollution；Second is that viscous by changing the enhancing of base rubber molecular structure
Connecing property, but this method is since in exploitation add-on type high refractive index LED liquid casting glue technologies and immature, actual production process also compares
More complex, the cost is relatively high, not yet industrializes at present；Third, being carried using the tackifier of general low-refraction by adding
High adhesiveness, this method is easy to operate, but there is also with high refractive index LED liquid embedding refractive index mismatch, it is compatible
The problems such as property is poor, and catalyst is easily poisoned.Ideal tackifier require with add-on type high refractive index LED liquid casting glues it is main at
Split-phase capacitive is good, and does not influence every physical mechanical property, electrical property and the heat resistance after silica gel curing process and solidification.
Invention content
The purpose of the present invention is being directed to above-mentioned deficiency in the prior art, a kind of high refractive index LED liquid casting glues are provided
With tackifier, which is greater than or equal to 1.50, has good compatibility with high refractive index LED liquid casting glues.
It is another object of the present invention to be directed to above-mentioned deficiency in the prior art, a kind of high refractive index LED liquid filling is provided
The preparation method of sealing tackifier, it is dilute in nonpolar solvent using the organosiloxane with hydrolyzable alkoxy grp as monomer
It releases down, under the action of catalyst cohydrolysis polycondensation, obtains a kind of water white transparency polymethyl-benzene base silicones oligomer, then will gather
With with active function group silane coupling agent under the effect of the catalyst, ester exchange reaction occurs for methyl phenyl silicone resin oligomer,
After removing solvent after filtering, a kind of suitable high refractive index LED liquid casting glue tackifier have been prepared.The present invention has technique
Simply, the advantages that reproducible and structure-controllable.
The purpose of the present invention is achieved through the following technical solutions.
The general structure of a kind of high refractive index LED liquid casting glue tackifier, the tackifier is (R1SiO3/2)a
(R2R3SiO2/2)b(R4) c (OH) d,
Wherein, R1SiO3/2、R2R3SiO2/2、R4Three-functionality-degree chain link, bifunctionality chain link, hydrolyzable are respectively represented with OH
Group and hydroxyl group, the entire infrastructure unit that a, b, c and d indicate to constitute tackifier rubbing shared by each chain link when being 1mol
That number；
Wherein, R1For vinyl, phenyl, methyl, γ-glycidyl ether oxygen propyl, β-(3,4- epoxycyclohexyl) ethyl
Or one kind in γ-methacryloxypropyl, R2For one kind in methyl, phenyl or vinyl, R3For phenyl, first
One kind in base, γ-glycidyl ether oxygen propyl or γ-methacryloxypropyl, R4For methoxyl group or ethyoxyl
In one kind, a, b, c, d are the number more than zero and less than 1, and a+b+c+d=1.
Preferably, a, b 0.1-0.5, c, d 0.5-0.9.
A kind of preparation method of high refractive index LED liquid casting glue tackifier, includes the following steps：
(1) using the organosiloxane of the hydrolyzable groups with different degrees of functionality as monomer, under organic solvent dispersion, in water
Under the conditions of solving catalyst and 30-80 DEG C, suitable deionized water cohydrolysis is added dropwise 3-5 hours, hydrolysis is washed with deionized water and urges
After agent, a kind of water white transparency polymethyl-benzene base silicones oligomer is obtained；Preferably, organic silica of the hydrolyzable groups
Alkane is the phenyl siloxane of hydrolyzable alkoxy base.Preferably, hydrolysis temperature is 40-60 DEG C, hydrolysis time 3.5-4.5
Hour.
(2) water white transparency polymethyl-benzene base silicones oligomer is heated to 75-100 DEG C, it is remaining is passed through nitrogen removing
After moisture, band active function group silane coupling agent is added, under the action of catalyst for ester exchange reaction, 3- is reacted at 70-120 DEG C
After 15 hours, it is cooled to room temperature, after removing catalyst for ester exchange reaction, cold filtration, at 75-140 DEG C of material temperature, in vacuum item
Removed under reduced pressure lower-molecular substance (lower-molecular substance includes the organic solvent), prepares suitable high refractive index LED liquid under part
The tackifier of casting glue.
And specifically, it is preferable to ground, the material temperature of the removing organic solvent is 75-130 DEG C.The vacuum of the removing organic solvent
Degree is 10-80mmHg.
Wherein, the monomer (i.e. organosiloxane monomer) is phenyltrimethoxysila,e, phenyl triethoxysilane, first
Base phenyidimethoxysilane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, methyl trimethoxy oxosilane, first
One in ethyl triethoxy silicane alkane, methylvinyldimethoxysilane, dimethylformamide dimethyl oxosilane, dimethyl diethyl oxosilane
Kind or more than one mixtures combined in any proportion.
Preferably, the monomer is phenyltrimethoxysila,e, phenyl triethoxysilane, aminomethyl phenyl dimethoxy silicon
Alkane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, methyl trimethoxy oxosilane, methyltriethoxysilane, first
Arbitrary two kinds in base vinyl dimethoxysilane, dimethylformamide dimethyl oxosilane, dimethyl diethyl oxosilane are in mass ratio
1:The mixture of 1 combination.
It is highly preferred that the monomer be phenyltrimethoxysila,e, phenyl triethoxysilane, methyl trimethoxy oxosilane and
Methyltriethoxysilane is with mass ratio for 2:2:1:1 mixture or the monomer be aminomethyl phenyl dimethoxysilane,
Aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane are with mass ratio for 1:1:1 mixture or the monomer
With mass ratio it is 1 for methylvinyldimethoxysilane, dimethylformamide dimethyl oxosilane, dimethyl diethyl oxosilane:1:1 it is mixed
Close object.
Wherein, the organic solvent is at least one of hexamethylene, toluene, dimethylbenzene.Preferably, the solvent is
Hexamethylene, toluene, dimethylbenzene are with mass ratio for 3:1:1 mixture.The dosage of the organic solvent is the matter for having the monomer
2-4 times of amount, preferably 3 times.
Wherein, the molal quantity of the deionized water is 0.8-1.5 times of molal quantity of the hydrolyzable groups of the monomer, excellent
It is selected as 1-1.2 times.
Wherein, the hydrolyst is one kind in concentrated hydrochloric acid, trifluoromethane sulfonic acid, the concentrated sulfuric acid, phosphoric acid.Specifically,
The mass concentration of the concentrated hydrochloric acid is 37%, and the mass concentration of the concentrated sulfuric acid is 98%, and the mass concentration of the phosphoric acid is
85%.Preferably, the hydrolyst and the mass ratio of deionized water are 0.05:99.5-5:95.
Wherein, the band active function group silane coupling agent is vinyltrimethoxysilane, vinyl triethoxyl silicon
Alkane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-(methyl
Acryloyl-oxy) propyl-triethoxysilicane, γ-glycidyl ether oxygen propyl methyl dimethoxysilane, γ-(methacryls
Oxygen) hydroxypropyl methyl dimethoxysilane, at least one of 2- (3,4- 7-oxa-bicyclo[4.1.0s) ethyl trimethoxy silane.
Preferably, the band active function group silane coupling agent is vinyltrimethoxysilane, vinyl triethoxyl
Silane, 2- (3,4- 7-oxa-bicyclo[4.1.0s) ethyl trimethoxy silanes are with mass ratio for 2:2:1 mixture or band activity
Function base silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy
Base silane, γ-(methacryloxypropyl) propyl-triethoxysilicanes with equal-quality than mixture, or, the band is lived
Sexual function base silane coupling agent is γ-glycidyl ether oxygen propyl methyl dimethoxysilane, γ-(methacryloxypropyl) propyl
Methyl dimethoxysilane is with mass ratio for 2：1 mixture.
Wherein, the molal quantity of the active function group silane coupling agent is 0.5-1.0 times of total mole number of the monomer,
Preferably 0.6-0.8 times.
Wherein, the catalyst for ester exchange reaction be sodium hydroxide, sodium ethoxide, potassium hydroxide, potassium ethoxide, to toluene sulphur
One kind in acid, storng-acid cation exchange resin, alchlor, titanium tetrachloride.
Wherein, the dosage of the catalyst for ester exchange reaction is the 20-500ppm of active function group silane coupling agent, preferably
For 80-350ppm, ppm, that is, mg/L.
The beneficial effects of the invention are as follows：
(1) present invention is using the organosiloxane with hydrolyzable alkoxy grp as monomer, under nonpolar solvent dilution,
Cohydrolysis polycondensation under catalyst action obtains a kind of water white transparency polymethyl-benzene base silicones oligomer, then by polymethyl-benzene
With with active function group silane coupling agent under the effect of the catalyst, transesterification occurs for base silicones oligomer.
(2) refractive index of tackifier of the invention is more than or equal to 1.50, preferably 1.50-1.53, the tackifier and height
Refractive index LED liquid casting glues have good compatibility.
(3) tackifier obtained with the preparation method of the present invention, are added directly into additional organosilicon glue, can improve
The cementability of silica gel and base material, and this method raw material is easy to get, reaction condition is mild, simple for process, operability is strong, is easy to industry
Metaplasia is produced.
(4) preparation method of the invention has many advantages, such as simple for process, reproducible and structure-controllable.The addition present invention's
Tackifier can make high refractive index LED liquid casting glue be more than with LED lamp bead timbering material polyphthalamide
90% cohesional failure degree greatly improves adhesive force, and the air-tightness of enhancing LED chip encapsulation, extend LED lamp bead uses the longevity
Life.The tackifier of the high refractive index LED liquid casting glues of the present invention can play important work in the encapsulation of LED light emitting diodes
With.
Specific implementation mode
The invention will be further described with the following Examples.
Embodiment 1
In the 1L four-hole bottles with condensing unit, thermometer and blender, 297.5g (1.5mol) phenyl trimethoxy is added
Base silane, 446.2g dimethylbenzene, 0.38g trifluoromethane sulfonic acids, it is to be mixed uniformly after, be heated to 50 DEG C, then through 1 hour slowly
81g (4.5mol) deionized water is added dropwise, after reacting 3h after being added dropwise, is washed to neutrality, separates organic layer, obtain water white transparency
Polymethyl-benzene base silicones oligomer, then puts up water knockout drum stirring and is warming up to 90 DEG C and is passed through nitrogen and remove remaining moisture, until
Until water knockout drum is distillated without water droplet, then be added 59.0g (0.25mol) γ-glycidyl ether oxygen propyl trimethoxy silicane and
The 125 DEG C of reactions of 0.2g sodium hydroxides are added in 110.0g (0.50mol) γ-glycidyl ether oxygen propyl methyl dimethoxysilane
The reaction was continued, and 3h waits for that after reaction, stirring is cooled to room temperature, and is added in 0.3g glacial acetic acids and remains sodium hydroxide, after filtering,
Finally at 130 DEG C, vacuum degree is that 20mmHg obtains the thick tackifier that appearance is micro- Huang, its refractive index is measured at 25 DEG C is
1.50。
Embodiment 2
In the 2L four-hole bottles with condensing unit, thermometer and blender, 297.5g (1.5mol) phenyl trimethoxy is added
Base silane, 244g (1.0mol) diphenyl dimethoxy, 600g dimethylbenzene, 0.5g trifluoromethane sulfonic acids, it is to be mixed uniformly after, add
Then to 70 DEG C 93.6 (5.2mol) deionized waters were slowly added dropwise through 1 hour in heat, after reacting 3h after being added dropwise, in being washed to
Property, separate organic layer, water white transparency polymethyl-benzene base silicones oligomer then puts up water knockout drum stirring and is warming up to 90 DEG C and is passed through
Nitrogen removes remaining moisture, until water knockout drum is distillated without water droplet, then adds 59.0g (0.25mol) γ-glycidyl ether oxygen
0.2g is added in propyl trimethoxy silicane and 110.0g (0.50mol) γ-glycidyl ether oxygen propyl methyl dimethoxysilane
The reaction was continued that 3h waits for that after reaction, stirring is cooled to room temperature for the reaction of 125 DEG C of sodium hydroxide, is added in 0.3g glacial acetic acids and remains
Sodium hydroxide, after filtering, finally at 130 DEG C, vacuum degree is that 20mmHg obtains thick tackifier, and refractive index is measured at 25 DEG C
It is 1.53.
Embodiment 3
In the 2L four-hole bottles with condensing unit, thermometer and blender, 297.5g (1.5mol) phenyl trimethoxy is added
Base silane, 244g (1.0mol) diphenyl dimethoxy, 600g toluene, 0.5g trifluoromethane sulfonic acids, it is to be mixed uniformly after, heating
To 70 DEG C, 93.6 (5.2mol) deionized waters then were slowly added dropwise through 1 hour, after reacting 3h after being added dropwise, are washed to neutrality,
Separate organic layer, water white transparency polymethyl-benzene base silicones oligomer then puts up water knockout drum stirring and is warming up to 90 DEG C and is passed through nitrogen
Gas removes remaining moisture, until water knockout drum is distillated without water droplet, then adds 62.14g (0.25mol) γ-(methacryls
Oxygen) propyl trimethoxy silicane and 116.17g (0.50mol) γ-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane, add
Entering the 85 DEG C of reactions of 0.2g sodium hydroxides, the reaction was continued 12 hours, waits for that after reaction, stirring is cooled to room temperature, 0.3g ice second is added
Acid neutralizes residual sodium hydroxide, and after filtering, finally at 80 DEG C, vacuum degree is that 10mmHg obtains colorless viscous shape tackifier, 25
It is 1.52 that refractive index is measured at DEG C.
Embodiment 4
In the 2L four-hole bottles with condensing unit, thermometer and blender, 297.5g (1.5mol) phenyl trimethoxy is added
Base silane, 244g (1.0mol) diphenyl dimethoxy, 600g toluene, 0.5g trifluoromethane sulfonic acids, it is to be mixed uniformly after, heating
To 70 DEG C, 93.6 (5.2mol) deionized waters then were slowly added dropwise through 1 hour, after reacting 3h after being added dropwise, are washed to neutrality,
Separate organic layer, water white transparency polymethyl-benzene base silicones oligomer then puts up water knockout drum stirring and is warming up to 90 DEG C and is passed through nitrogen
Gas removes remaining moisture, until water knockout drum is distillated without water droplet, then adds 58.09 (0.25mol) γ-(methacryloxypropyl)
Hydroxypropyl methyl dimethoxysilane and 124.28 (0.50mol), the 85 DEG C of reactions of 0.2g sodium hydroxides are added, and the reaction was continued 12 hours,
It waits for that after reaction, stirring is cooled to room temperature, be added in 0.3g glacial acetic acids and remain sodium hydroxide, after filtering, finally at 80 DEG C,
Vacuum degree is that 10mmHg obtains colorless viscous shape tackifier, and it is 1.52 that refractive index is measured at 25 DEG C.
Embodiment 5
In the 2L four-hole bottles with condensing unit, thermometer and blender, 297.5g (1.5mol) phenyl trimethoxy is added
Base silane, 122g (0.5mol) diphenyl dimethoxies and 60.11g (0.5mol) dimethylformamide dimethyl oxygroup, 600g dimethylbenzene,
0.5g trifluoromethane sulfonic acids, it is to be mixed uniformly after, be heated to 70 DEG C, then through be slowly added dropwise within 1 hour 93.6 (5.2mol) go from
Sub- water is washed to neutrality after reacting 3h after being added dropwise, and separates organic layer, water white transparency polymethyl-benzene base silicones oligomer,
Then it puts up water knockout drum stirring and is warming up to 90 DEG C and is passed through nitrogen and remove remaining moisture, until water knockout drum is distillated without water droplet, so
Afterwards plus after 177.0g (0.75mol) γ-glycidyl ether oxygen propyl trimethoxy silicane beam, stirring is cooled to room temperature, and is added
In 0.3g glacial acetic acids and sodium hydroxide is remained, after filtering, finally at 130 DEG C, vacuum degree is that 20mmHg obtains thick tackifier,
It is 1.51 that refractive index is measured at 25 DEG C.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art answer
Work as understanding, technical scheme of the present invention can be modified or replaced equivalently, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (10)
1. a kind of high refractive index LED liquid casting glue tackifier, it is characterised in that：The general structure of the tackifier is
(R1SiO3/2)a(R2R3SiO2/2)b(R4) c (OH) d,
Wherein, R1SiO3/2、R2R3SiO2/2、R4With OH respectively represent three-functionality-degree chain link, bifunctionality chain link, hydrolyzable groups and
Hydroxyl group, molal quantity of the entire infrastructure unit that a, b, c and d indicate to constitute tackifier when being 1mol shared by each chain link；
Wherein, R1For vinyl, phenyl, methyl, γ-glycidyl ether oxygen propyl, β-(3,4- epoxycyclohexyl) ethyls or
One kind in γ-methacryloxypropyl, R2For one kind in methyl, phenyl or vinyl, R3For phenyl, methyl,
One kind in γ-glycidyl ether oxygen propyl or γ-methacryloxypropyl, R4For in methoxyl group or ethyoxyl
One kind, a, b, c, d are the number more than zero and less than 1, and a+b+c+d=1.
2. a kind of preparation method of high refractive index LED liquid casting glue tackifier as described in claim 1, feature exist
In including the following steps：
(1) using the organosiloxane with hydrolyzable groups as monomer, under organic solvent dispersion, in hydrolyst and 30-80
Under the conditions of DEG C, deionized water cohydrolysis is added dropwise 3-5 hours, after hydrolyst is washed with deionized water, obtains a kind of colourless
Bright polymethyl-benzene base silicones oligomer；
(2) water white transparency polymethyl-benzene base silicones oligomer is heated to 75-100 DEG C, is passed through nitrogen and removes remaining moisture
Afterwards, band active function group silane coupling agent is added, under the action of catalyst for ester exchange reaction, it is small that 3-15 is reacted at 70-120 DEG C
Shi Hou is cooled to room temperature, after removing catalyst for ester exchange reaction, cold filtration, at 75-140 DEG C of material temperature, under vacuum
Removed under reduced pressure lower-molecular substance prepares the tackifier of suitable high refractive index LED liquid casting glues.
3. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature exist
In：The monomer is phenyltrimethoxysila,e, phenyl triethoxysilane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl
Diethoxy silane, dimethoxydiphenylsilane, methyl trimethoxy oxosilane, methyltriethoxysilane, methyl ethylene two
One or more in methoxy silane, dimethylformamide dimethyl oxosilane, dimethyl diethyl oxosilane combine in any proportion
Mixture.
4. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature exist
In：The organic solvent is at least one of hexamethylene, toluene, dimethylbenzene.
5. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature exist
In：The molal quantity of the deionized water is 0.8-1.5 times of the molal quantity of the hydrolyzable groups of the monomer.
6. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature exist
In：The hydrolyst is one kind in concentrated hydrochloric acid, trifluoromethane sulfonic acid, the concentrated sulfuric acid, phosphoric acid.
7. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature exist
In：The band active function group silane coupling agent is vinyltrimethoxysilane, vinyltriethoxysilane, γ-shrink
Glycerine ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-(methacryloxypropyl)
Propyl-triethoxysilicane, γ-glycidyl ether oxygen propyl methyl dimethoxysilane, γ-(methacryloxypropyl) propyl first
At least one of base dimethoxysilane, 2- (3,4- 7-oxa-bicyclo[4.1.0s) ethyl trimethoxy silane.
8. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature exist
In：The molal quantity with active function group silane coupling agent is 0.5-1.0 times of the total mole number of the monomer.
9. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature exist
In：The catalyst for ester exchange reaction is sodium hydroxide, sodium ethoxide, potassium hydroxide, potassium ethoxide, p-methyl benzenesulfonic acid, highly acid sun
One kind in ion exchange resin, alchlor, titanium tetrachloride.
10. a kind of preparation method of high refractive index LED liquid casting glue tackifier according to claim 2, feature
It is：The dosage of the catalyst for ester exchange reaction is the 20-500ppm of active function group silane coupling agent.
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| CN111205464B (en) * | 2020-02-27 | 2022-02-11 | 深圳市化讯半导体材料有限公司 | Silane coupling agent oligomer solution and preparation method and application thereof |
| CN111303820B (en) * | 2020-03-09 | 2021-03-26 | 杭州之江新材料有限公司 | Double-component polyurethane structural adhesive for bonding power battery and preparation method thereof |
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| CN102863799A (en) * | 2012-10-17 | 2013-01-09 | 东莞市贝特利新材料有限公司 | High-refractive-index organosilicon material for light-emitting diode (LED) packaging and preparation method of high-refractive-index organosilicon material |
| CN103739848A (en) * | 2013-12-25 | 2014-04-23 | 北京化工大学 | Tackifier for addition type organosilicone packaging glue and preparation method thereof |
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