CN105400446A - Tackifier for high-refractive index LED liquid casting glue and preparation method thereof - Google Patents
Tackifier for high-refractive index LED liquid casting glue and preparation method thereof Download PDFInfo
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- CN105400446A CN105400446A CN201510949866.1A CN201510949866A CN105400446A CN 105400446 A CN105400446 A CN 105400446A CN 201510949866 A CN201510949866 A CN 201510949866A CN 105400446 A CN105400446 A CN 105400446A
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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
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Abstract
The invention provides a tackifier for a high-refractive index LED liquid casting glue and a preparation method thereof. The preparation method comprises taking an organosiloxane with a hydrolysable alkoxy as a monomer, dispersing in an organic solvent, performing cohydrolysis condensation under the effect of a catalyst, and washing with water to obtain a colorless transparent polymerized methylphenyl silicone resin oligomer solution, then performing transesterification on the polymerized methylphenyl silicone resin oligomer solution and a silane coupling agent with an active functional group under the effect of a catalyst, and removing low-molecular substances in a reduced pressure environment after filtering is performed or the catalyst is neutralized, so as to prepare the tackifier for the high-refractive index LED liquid casting glue. The tackifier possesses the refractive index larger than or equal to 1.50, and possesses extremely good compatibility with the high-refractive index LED liquid casting glue. The preparation method comprises the advantages of simple technology, good repeatability, structure controllability and the like.i The tackifier gives play to important effect in the field of packaging of LED.
Description
Technical field
The present invention relates to tackifier technical field, particularly relate to a kind of high refractive index LED liquid joint sealant tackifier and preparation method thereof.
Background technology
It is low and can the advantage such as profound solidification that add-on type high refractive index LED liquid joint sealant not only has no coupling product in general add-on type liquid silicon rubber sulfidation, shrinking percentage, also there is transmittance high, specific refractory power is large, Heat stability is good, stress is little, the features such as water absorbability is low, are rapidly developed in LED industry recently.Equally, add-on type high refractive index LED liquid joint sealant also has low, poor with the adhesiveproperties of metal base (copper, aluminium, silver, gold and stainless steel etc.) and non-metallic substrate (PC, PBT, nylon and the pcb board etc.) problem of general liquid silastic surface energy after hardening.Consider that in practical application LED process, joint sealant is bonding higher to substrate bonding requirement, the exploitation of corresponding tackifier is study hotspot and the difficult point in this bonding field always.
At present, similar with usual silicone rubber, improving mainly containing of the method for the cementability of add-on type high refractive index LED liquid joint sealant and various material three kinds: one is adopt silane coupling agent to carry out pre-treatment to substrate surface, this method adds production process and production time, particularly can greatly reduce production efficiency when producing LED lamp bead in enormous quantities and increase Material Cost, silane coupling agent many uses flammable solvent, causes peril of transportation and environmental pollution simultaneously; Two be strengthen cementability by changing base xanthan molecule structure, but this method is due to immature in exploitation add-on type high refractive index LED liquid joint sealant technology, and actual production process is more complicated also, and cost is relatively high, at present not yet industrialization; Three is adopt the tackifier of general low-refraction to improve cementability by adding, and this method is easy to operate, but also exists and do not mate with high refractive index LED liquid embedding specific refractory power, poor compatibility, and catalyzer is the problem such as poisoning easily.It is good that desirable tackifier require with the main component consistency of add-on type high refractive index LED liquid joint sealant, and do not affect every physical and mechanical properties, electrical property and the resistance toheat after silica gel solid metallization processes and solidification.
Summary of the invention
The object of the invention is for above-mentioned deficiency of the prior art, provide a kind of high refractive index LED liquid joint sealant tackifier, this tackifier specific refractory power is more than or equal to 1.50, has good consistency with high refractive index LED liquid joint sealant.
Another object of the present invention is for above-mentioned deficiency of the prior art, a kind of preparation method of high refractive index LED liquid joint sealant tackifier is provided, with the organo-siloxane with hydrolyzable alkoxy grp for monomer, under non-polar solvent dilution, cohydrolysis polycondensation under catalyst action, obtain a kind of water white transparency polyphenylmethyl base silicone resin oligopolymer, then by polyphenylmethyl base silicone resin oligopolymer and band active function group silane coupling agent, under the effect of catalyzer, there is transesterification reaction, after filtering after desolvation, a kind of applicable high refractive index LED liquid joint sealant tackifier are prepared.The present invention has the advantages such as simple, the reproducible and structure-controllable of technique.
Object of the present invention is achieved through the following technical solutions.
A kind of high refractive index LED liquid joint sealant tackifier, the general structure of these tackifier is (R
1siO
3/2) a (R
2r
3siO
2/2) b (R
4) c (OH) d,
Wherein, R
1siO
3/2, R
2r
3siO
2/2, R
4represent three-functionality-degree chain link, difunctionality chain link, hydrolysable group and oh group respectively with OH, a, b, c and d all represent that the entire infrastructure unit forming tackifier is mole number during 1mol shared by each chain link;
Wherein, R
1for the one in vinyl, phenyl, methyl, γ-glycidyl ether oxygen propyl, β-(3,4-epoxycyclohexyl) ethyl or γ-methacryloxypropyl, R
2for the one in methyl, phenyl or vinyl, R
3for the one in phenyl, methyl, γ-glycidyl ether oxygen propyl or γ-methacryloxypropyl, R
4for the one in methoxyl group or oxyethyl group, a, b, c, d be greater than zero and be less than 1 number, and a+b+c+d=1.
Preferably, a, b are 0.1-0.5, c, d is 0.5-0.9.
A preparation method for high refractive index LED liquid joint sealant tackifier, comprises the following steps:
(1) with the organo-siloxane of the hydrolysable group with different functionality for monomer, under organic solvent dispersion, under hydrolyst and 30-80 DEG C of condition, drip appropriate deionized water cohydrolysis 3-5 hour, after washing away hydrolyst with deionized water, obtain a kind of water white transparency polyphenylmethyl base silicone resin oligopolymer; Preferably, the organo-siloxane of described hydrolysable group is the phenyl siloxane of hydrolyzable alkoxy base.Preferably, hydrolysis temperature is 40-60 DEG C, and hydrolysis time is 3.5-4.5 hour.
(2) water white transparency polyphenylmethyl base silicone resin oligopolymer is heated to 75-100 DEG C, after passing into the residual moisture of nitrogen removing, add band active function group silane coupling agent, under the effect of catalyst for ester exchange reaction, 70-120 DEG C of reaction after 3-15 hour, be cooled to room temperature, after removing catalyzer, cold filtration, at material temperature 75-140 DEG C, removed under reduced pressure lower-molecular substance (lower-molecular substance comprises described organic solvent) under vacuum, prepares the tackifier of applicable high refractive index LED liquid joint sealant.
Particularly, preferably, the material temperature removing organic solvent described in is 75-130 DEG C.The described vacuum tightness removing organic solvent is 10-80mmHg.
Wherein, described monomer (i.e. organo-siloxane monomer) be phenyltrimethoxysila,e, one or more mixtures combined in any proportion in phenyl triethoxysilane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, methyl trimethoxy oxosilane, Union carbide A-162, methylvinyldimethoxysilane, dimethylformamide dimethyl oxosilane, dimethyl diethoxy silane.
Preferably, described monomer be in phenyltrimethoxysila,e, phenyl triethoxysilane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, methyl trimethoxy oxosilane, Union carbide A-162, methylvinyldimethoxysilane, dimethylformamide dimethyl oxosilane, dimethyl diethoxy silane any two kinds be in mass ratio 1:1 combination mixture.
More preferably, the mixture that described monomer is phenyltrimethoxysila,e, phenyl triethoxysilane, methyl trimethoxy oxosilane and Union carbide A-162 take mass ratio as 2:2:1:1, or the mixture that described monomer is aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane take mass ratio as 1:1:1, or described monomer be methylvinyldimethoxysilane, dimethylformamide dimethyl oxosilane, dimethyl diethoxy silane take mass ratio as the mixture of 1:1:1.
Wherein, described organic solvent is at least one in hexanaphthene, toluene, dimethylbenzene.Preferably, the mixture of described machine solvent to be hexanaphthene, toluene, dimethylbenzene with mass ratio be 3:1:1.The consumption of described organic solvent is 2-4 times of the quality having described monomer, is preferably 3 times.
Wherein, the mole number of described deionized water is 0.8-1.5 times of the mole number of the hydrolysable group of described monomer, is preferably 1-1.2 doubly.
Wherein, described hydrolyst is the one in concentrated hydrochloric acid, trifluoromethane sulfonic acid, the vitriol oil, phosphoric acid.Particularly, the mass concentration of described concentrated hydrochloric acid is 37%, and the mass concentration of the described vitriol oil is 98%, and the mass concentration of described phosphoric acid is 85%.Preferably, the mass ratio of described hydrolyst and deionized water is 0.05:99.5-5:95.
Wherein, described band active function group silane coupling agent is at least one in vinyltrimethoxy silane, vinyltriethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl-triethoxysilicane, γ-glycidyl ether oxygen propyl methyl dimethoxysilane, γ-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane, 2-(3,4-epoxy cyclohexane) ethyl trimethoxy silane.
Preferably, described band active function group silane coupling agent is vinyltrimethoxy silane, vinyltriethoxysilane, 2-(3, 4-epoxy cyclohexane) ethyl trimethoxy silane take mass ratio as the mixture of 2:2:1, or described band active function group silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl-triethoxysilicane is with the mixture of equal-quality ratio, or, described band active function group silane coupling agent is γ-glycidyl ether oxygen propyl methyl dimethoxysilane, γ-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane take mass ratio as the mixture of 2:1.
Wherein, the mole number of described active function group silane coupling agent is 0.5-1.0 times of the total mole number of described monomer, is preferably 0.6-0.8 doubly.
Wherein, described transesterification catalyst is the one in sodium hydroxide, sodium ethylate, potassium hydroxide, potassium ethylate, tosic acid, storng-acid cation exchange resin, aluminum chloride, titanium tetrachloride.
Wherein, the consumption of described transesterification catalyst is the 20-500ppm of active function group silane coupling agent, is preferably 80-350ppm, ppm and mg/L.
The invention has the beneficial effects as follows:
(1) the present invention with the organo-siloxane with hydrolyzable alkoxy grp for monomer, under non-polar solvent dilution, cohydrolysis polycondensation under catalyst action, obtain a kind of water white transparency polyphenylmethyl base silicone resin oligopolymer, then by polyphenylmethyl base silicone resin oligopolymer and band active function group silane coupling agent, under the effect of catalyzer, there is transesterify.
(2) specific refractory power of tackifier of the present invention is more than or equal to 1.50, and be preferably 1.50-1.53, these tackifier and high refractive index LED liquid joint sealant have good consistency.
(3) with the tackifier that preparation method of the present invention obtains, directly join in additional organosilicon glue, can improve the cementability of silica gel and base material, and the method raw material is easy to get, reaction conditions gentle, technique is simple, workable, is easy to suitability for industrialized production.
(4) preparation method of the present invention has the advantages such as simple, the reproducible and structure-controllable of technique.Adding tackifier of the present invention can make high refractive index LED liquid joint sealant and LED lamp bead timbering material polyphthalamide be greater than 90% cohesive failure degree, greatly improve sticking power, strengthen the resistance to air loss of LED chip encapsulation, extend the work-ing life of LED lamp bead.The tackifier of high refractive index LED liquid joint sealant of the present invention can play an important role in the encapsulation of LED photodiode.
Embodiment
The invention will be further described with the following Examples.
embodiment 1
With condensing works, the 1L four-hole bottle of thermometer and agitator, add 297.5g(1.5mol) phenyltrimethoxysila,e, 446.2g dimethylbenzene, 0.38g trifluoromethane sulfonic acid, to be mixed evenly after, be heated to 50 DEG C, then slowly 81g(4.5mol was dripped through 1 hour) deionized water, after dropwising rear reaction 3h, be washed to neutrality, separate organic layer, obtain water white transparency polyphenylmethyl base silicone resin oligopolymer, then put up water trap stirring and be warming up to 90 DEG C of moisture passing into nitrogen removing and remain, to water trap distillates without water droplet, then 59.0g(0.25mol is added) γ-glycidyl ether oxygen propyl trimethoxy silicane and 110.0g(0.50mol) γ-glycidyl ether oxygen propyl methyl dimethoxysilane, adding the reaction of 125 DEG C, 0.2g sodium hydroxide continues after reaction 3h question response terminates, stirring is cooled to room temperature, add in 0.3g glacial acetic acid and remaining hydrogen sodium oxide, after filtration, last at 130 DEG C, vacuum tightness is the thick tackifier that 20mmHg obtains that outward appearance is micro-Huang, at 25 DEG C, record its specific refractory power is 1.50.
embodiment 2
With condensing works, the 2L four-hole bottle of thermometer and agitator, add 297.5g(1.5mol) phenyltrimethoxysila,e, 244g(1.0mol) diphenyl dimethoxy, 600g dimethylbenzene, 0.5g trifluoromethane sulfonic acid, to be mixed evenly after, be heated to 70 DEG C, then slowly 93.6(5.2mol was dripped through 1 hour) deionized water, after dropwising rear reaction 3h, be washed to neutrality, separate organic layer, water white transparency polyphenylmethyl base silicone resin oligopolymer, then put up water trap stirring and be warming up to 90 DEG C of moisture passing into nitrogen removing and remain, to water trap distillates without water droplet, then 59.0g(0.25mol is added) γ-glycidyl ether oxygen propyl trimethoxy silicane and 110.0g(0.50mol) γ-glycidyl ether oxygen propyl methyl dimethoxysilane, adding the reaction of 125 DEG C, 0.2g sodium hydroxide continues after reaction 3h question response terminates, stirring is cooled to room temperature, add in 0.3g glacial acetic acid and remaining hydrogen sodium oxide, after filtration, last at 130 DEG C, vacuum tightness is that 20mmHg obtains thick tackifier, at 25 DEG C, record specific refractory power is 1.53.
embodiment 3
With condensing works, the 2L four-hole bottle of thermometer and agitator, add 297.5g(1.5mol) phenyltrimethoxysila,e, 244g(1.0mol) diphenyl dimethoxy, 600g toluene, 0.5g trifluoromethane sulfonic acid, to be mixed evenly after, be heated to 70 DEG C, then slowly 93.6(5.2mol was dripped through 1 hour) deionized water, after dropwising rear reaction 3h, be washed to neutrality, separate organic layer, water white transparency polyphenylmethyl base silicone resin oligopolymer, then put up water trap stirring and be warming up to 90 DEG C of moisture passing into nitrogen removing and remain, to water trap distillates without water droplet, then 62.14g(0.25mol is added) γ-(methacryloxypropyl) propyl trimethoxy silicane and 116.17g(0.50mol) γ-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane, add the reaction of 85 DEG C, 0.2g sodium hydroxide and continue reaction 12 hours, after question response terminates, stirring is cooled to room temperature, add in 0.3g glacial acetic acid and remaining hydrogen sodium oxide, after filtration, last at 80 DEG C, vacuum tightness is that 10mmHg obtains colorless viscous shape tackifier, at 25 DEG C, record specific refractory power is 1.52.
embodiment 4
With condensing works, the 2L four-hole bottle of thermometer and agitator, add 297.5g(1.5mol) phenyltrimethoxysila,e, 244g(1.0mol) diphenyl dimethoxy, 600g toluene, 0.5g trifluoromethane sulfonic acid, to be mixed evenly after, be heated to 70 DEG C, then slowly 93.6(5.2mol was dripped through 1 hour) deionized water, after dropwising rear reaction 3h, be washed to neutrality, separate organic layer, water white transparency polyphenylmethyl base silicone resin oligopolymer, then put up water trap stirring and be warming up to 90 DEG C of moisture passing into nitrogen removing and remain, to water trap distillates without water droplet, then 58.09(0.25mol is added) γ-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane and 124.28(0.50mol), add the reaction of 85 DEG C, 0.2g sodium hydroxide and continue reaction 12 hours, after question response terminates, stirring is cooled to room temperature, add in 0.3g glacial acetic acid and remaining hydrogen sodium oxide, after filtration, last at 80 DEG C, vacuum tightness is that 10mmHg obtains colorless viscous shape tackifier, at 25 DEG C, record specific refractory power is 1.52.
embodiment 5
With condensing works, the 2L four-hole bottle of thermometer and agitator, add 297.5g(1.5mol) phenyltrimethoxysila,e, 122g(0.5mol) diphenyl dimethoxy and 60.11g(0.5mol) dimethylformamide dimethyl oxygen base, 600g dimethylbenzene, 0.5g trifluoromethane sulfonic acid, to be mixed evenly after, be heated to 70 DEG C, then slowly 93.6(5.2mol was dripped through 1 hour) deionized water, after dropwising rear reaction 3h, be washed to neutrality, separate organic layer, water white transparency polyphenylmethyl base silicone resin oligopolymer, then put up water trap stirring and be warming up to 90 DEG C of moisture passing into nitrogen removing and remain, to water trap distillates without water droplet, then 177.0g(0.75mol is added) after γ-glycidyl ether oxygen propyl trimethoxy silicane bundle, stirring is cooled to room temperature, add in 0.3g glacial acetic acid and remaining hydrogen sodium oxide, after filtration, last at 130 DEG C, vacuum tightness is that 20mmHg obtains thick tackifier, at 25 DEG C, record specific refractory power is 1.51.
Finally should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention; but not limiting the scope of the invention; although done to explain to the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (10)
1. high refractive index LED liquid joint sealant tackifier, is characterized in that: the general structure of these tackifier is (R
1siO
3/2) a (R
2r
3siO
2/2) b (R
4) c (OH) d,
Wherein, R
1siO
3/2, R
2r
3siO
2/2, R
4represent three-functionality-degree chain link, difunctionality chain link, hydrolysable group and oh group respectively with OH, a, b, c and d all represent that the entire infrastructure unit forming tackifier is mole number during 1mol shared by each chain link;
Wherein, R
1for the one in vinyl, phenyl, methyl, γ-glycidyl ether oxygen propyl, β-(3,4-epoxycyclohexyl) ethyl or γ-methacryloxypropyl, R
2for the one in methyl, phenyl or vinyl, R
3for the one in phenyl, methyl, γ-glycidyl ether oxygen propyl or γ-methacryloxypropyl, R
4for the one in methoxyl group or oxyethyl group, a, b, c, d be greater than zero and be less than 1 number, and a+b+c+d=1.
2. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier as claimed in claim 1, is characterized in that, comprise the following steps:
(1) with the organo-siloxane with hydrolysable group for monomer, under organic solvent dispersion, under hydrolyst and 30-80 DEG C of condition, drip deionized water cohydrolysis 3-5 hour, after washing away hydrolyst with deionized water, obtain a kind of water white transparency polyphenylmethyl base silicone resin oligopolymer;
(2) water white transparency polyphenylmethyl base silicone resin oligopolymer is heated to 75-100 DEG C, after passing into the residual moisture of nitrogen removing, add band active function group silane coupling agent, under the effect of catalyst for ester exchange reaction, 70-120 DEG C of reaction after 3-15 hour, be cooled to room temperature, after removing catalyzer, cold filtration, at material temperature 75-140 DEG C, removed under reduced pressure lower-molecular substance under vacuum, prepares the tackifier of applicable high refractive index LED liquid joint sealant.
3. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, is characterized in that: described monomer is one or more mixtures combined in any proportion in phenyltrimethoxysila,e, phenyl triethoxysilane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane, dimethoxydiphenylsilane, methyl trimethoxy oxosilane, Union carbide A-162, methylvinyldimethoxysilane, dimethylformamide dimethyl oxosilane, dimethyl diethoxy silane.
4. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, is characterized in that: described organic solvent is at least one in hexanaphthene, toluene, dimethylbenzene.
5. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, is characterized in that: the mole number of described deionized water is 0.8-1.5 times of the mole number of the hydrolysable group of described monomer.
6. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, is characterized in that: described hydrolyst is the one in concentrated hydrochloric acid, trifluoromethane sulfonic acid, the vitriol oil, phosphoric acid.
7. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, it is characterized in that: described band active function group silane coupling agent is vinyltrimethoxy silane, vinyltriethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl-triethoxysilicane, γ-glycidyl ether oxygen propyl methyl dimethoxysilane, γ-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane, 2-(3, 4-epoxy cyclohexane) at least one in ethyl trimethoxy silane.
8. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, is characterized in that: the mole number of described band active function group silane coupling agent is 0.5-1.0 times of the total mole number of described monomer.
9. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, is characterized in that: described transesterification catalyst is the one in sodium hydroxide, sodium ethylate, potassium hydroxide, potassium ethylate, tosic acid, storng-acid cation exchange resin, aluminum chloride, titanium tetrachloride.
10. the preparation method of a kind of high refractive index LED liquid joint sealant tackifier according to claim 2, is characterized in that: the consumption of described transesterification catalyst is the 20-500ppm of active function group silane coupling agent.
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| CN108239284A (en) * | 2016-12-27 | 2018-07-03 | 中昊晨光化工研究院有限公司 | A kind of add-on type liquid silicon rubber tackifier and preparation method thereof |
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| CN110256676A (en) * | 2019-05-24 | 2019-09-20 | 中山大学 | A kind of phenyl hydrogen-containing siloxane resin, high refractive index LED encapsulation silicon resin composition and preparation method thereof |
| CN110591635A (en) * | 2019-07-05 | 2019-12-20 | 惠州瑞德新材料科技股份有限公司 | Sealant and preparation method thereof |
| CN111205464A (en) * | 2020-02-27 | 2020-05-29 | 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 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2015
- 2015-12-18 CN CN201510949866.1A patent/CN105400446B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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