CN106221237A - A kind of LED encapsulation organic silica gel and preparation method thereof - Google Patents
A kind of LED encapsulation organic silica gel and preparation method thereof Download PDFInfo
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- CN106221237A CN106221237A CN201610595790.1A CN201610595790A CN106221237A CN 106221237 A CN106221237 A CN 106221237A CN 201610595790 A CN201610595790 A CN 201610595790A CN 106221237 A CN106221237 A CN 106221237A
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
- G02B1/041—Lenses
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
Abstract
The present invention relates to a kind of LED encapsulation organic silica gel and preparation method thereof, this organic silica gel includes component A and B component, and wherein component A is prepared from by organic siliconresin 25 50 weight portion containing vinyl, catalyst 0.1 0.5 weight portion, viscosifier 13 weight portion；B component is by organic siliconresin 100 120 weight portion containing vinyl, hydrogeneous organic siliconresin 80 130 weight portion, and inhibitor 1 10 weight portion is prepared from.LED encapsulation organic silica gel water white transparency of the present invention, refractive index are high, cold-hot impact property is good, and its preparation method is easy, and decrease the output of spent acid, are of value to protection environment.It is poor that LED encapsulation organic silica gel of the present invention overcomes conventional encapsulant cold-hot impact, the shortcoming of easy xanthochromia, it is also possible to is adjusted the viscosity of silica gel, hardness, adhesive force according to the demand of application.
Description
Technical field
The present invention relates to a kind of organic silica gel, especially a kind of LED encapsulation organic silica gel and preparation method thereof.
Background technology
Light emitting diode is called for short LED, is the semiconductor device converting electrical energy into luminous energy.Owing to having, volume is little, the life-span
The advantages such as length, luminous efficiency height, environmental protection, are described as " green illumination light source ".It is widely used in illumination, traffic signal and face
The fields such as the room lighting of light source.
Generally LED encapsulation material mainly includes epoxy resin, thermosetting epoxy resin etc., along with LED power increasing and
The raising of brightness, these materials are bad because of thermostability, easy xanthochromia, it is impossible to meet power-type LED performance requirement.And organic siliconresin
There is color inhibition, cold-hot impact, light transmittance advantages of higher, it has also become the optimum selection of LED encapsulation material.The synthesis of silicones
Method can be divided into hydrolyzing chlorosilane method and alkoxy silane Hydrolyze method according to raw material sources.Hydrolyzing chlorosilane method is used to produce
Cheng Zhonghui produces substantial amounts of hydrogen chloride, and such as, Chinese invention patent application CN101619170A uses hydrolyzing chlorosilane to prepare LED
Encapsulation silica gel material, the method generates substantial amounts of hydrogen chloride, pollutes environment, and needs substantial amounts of washing to neutralize, prepared
Journey is loaded down with trivial details, and the transparency simultaneously causing organic silica gel is low.
Comparatively speaking, alkoxy silane Hydrolyze method more advantage, as CN 103881394 B uses high viscosity vinyl MQ
The synthesis self-forming packaging silicon rubber such as resin, vinyl silicone oil, thixotropic materials, but the method introduces thixotropic materials, is unfavorable for silicon
The long term storage of glue, and use high viscosity vinyl MQ resin to determine that as initiation material, the viscosity of raw material, it is impossible to flexibly
The viscosity of Requirements on Product according to application, hardness, adhesive force is adjusted.
Summary of the invention
Problem to be solved by this invention is the deficiency overcoming prior art to exist, it is provided that a kind of LED encapsulation organosilicon
Glue and preparation method thereof.
It is an object of the invention to prepare the LED that a kind of transparency is good, cold-hot impact is good, refractive index is high encapsulate with organic
Silica gel material, and overcome the pollution problem that hydrolyzing chlorosilane brings.LED encapsulation organic silica gel of the present invention overcomes
Conventional encapsulant poor heat resistance, the shortcoming such as easy xanthochromia, and condition of storage is easy, stores of long duration.Its preparation method letter
Just, decrease the output of spent acid, be of value to protection environment, it is also possible to according to the demand of application to the viscosity of resin, hardness, attachment
Power is adjusted.
Organic containing vinyl in LED organic silica-gel material for encapsulating of the present invention, in described component A and B component
Silicones molecular formula is (ViMe2SiO1/2)x(Ph2SiO)y(PhSiO3/2) z, wherein Vi is vinyl, and Ph is phenyl, x+y+z=
1, x:z=1:3-5.It is 3000-55000mPa s the viscosity of 25 DEG C.
In LED organic silica-gel material for encapsulating of the present invention, in described component A, catalyst is to be catalyzed Si-H addition reaction
The platinum of reaction, the compound of palladium, preferably chloroplatinic acid, its consumption is 0.1-0.5 weight portion.
In LED organic silica-gel material for encapsulating of the present invention, in described B component, hydrogeneous organic siliconresin at least contains two
Individual or plural si-h bond, it is 50-500mPa s the viscosity of 25 DEG C.
In LED organic silica-gel material for encapsulating of the present invention, in described B component, inhibitor is suppression hydrosilylation
1-acetenyl-1-Hexalin, one in 2-methyl-3-butyne-2-alcohol.It is preferably 1-acetenyl-1-Hexalin.Its consumption
It is the 0.001-5% of A, B mixing total amount.
In LED organic silica-gel material for encapsulating of the present invention, in described component A, viscosifier are silane coupler, as γ-
(2,3-glycidyl) propyl trimethoxy silicane.
The preparation method of LED organic silica-gel material for encapsulating of the present invention, wherein A, B component preparation method as follows:
The preparation process of component A: take the water of 5-15 weight portion, the effect of water is complete for silane hydrolyzate, and its consumption is
Preferably calculate according to the amount of added silane, according to water: silane=2.5-3:1 (mol ratio), it is ensured that it reacts completely,
Silane described here refers to all silane compounds that hydrolysis can occur that reaction adds, including phenyltrimethoxysila,e
With dimethoxydiphenylsilane consumption summation.Add the hydrolyst hydrochloric acid of 0.1 weight portion afterwards, mix in reactor,
Taking the tetramethyl divinyl disiloxane of 3-5 weight portion, the amount added affects the viscosity of products therefrom, and its addition is the most,
The viscosity of product is the least, and practical operation can determine addition according to product to the demand of viscosity；The phenyl three of 20-50 weight portion
Methoxy silane, its addition is the most, and the viscosity of product is the biggest, according to product, the demand of viscosity can be adjusted consumption；With 4-8 weight
The dimethoxydiphenylsilane mix homogeneously of part is added dropwise to reactor under 65 DEG C of stirring conditions, reacts 3 little after dropping
Time, then divide water, decompression to steam solvent and unreacted monomer, obtain the organic siliconresin containing vinyl；Take 25-50 weight portion
The obtained organic siliconresin containing vinyl, the catalyst of 0.1-0.5 weight portion, 1-3 weight portion viscosifier mixing all
Even, it is thus achieved that component A；
The preparation process of B component: take the water of 5-15 weight portion, the effect of water is complete for silane hydrolyzate, and its consumption is
Preferably calculate according to the amount of added silane, according to water: silane=2.5-3:1 (mol ratio), it is ensured that it reacts completely,
Silane described here refers to all silane compounds that hydrolysis can occur that reaction adds, including phenyltrimethoxysila,e
With dimethoxydiphenylsilane consumption summation.Add the hydrolyst hydrochloric acid of 0.1 weight portion afterwards, mixed in reactor
Close, take 4-8 weight portion tetramethyldihydrogendisiloxane, the amount added affect the viscosity of products therefrom, its add get over
Many, the viscosity of product is the least, and practical operation can determine addition according to product to the demand of viscosity；The benzene of 15-25 weight portion
Base trimethoxy silane, its addition is the most, and the viscosity of product is the biggest, according to product, the demand of viscosity can be adjusted consumption；And 4-8
The dimethoxydiphenylsilane mix homogeneously of weight portion is added dropwise to reactor under 65 DEG C of stirring conditions, reacts after dropping
3 hours, water, decompression is then divided to steam solvent and unreacted monomer, obtain hydrogeneous organic siliconresin；Taking obtained hydrogeneous has
Machine silicones 80-130 weight portion, component A preparation process in the obtained organic siliconresin 100-120 weight containing vinyl
Part, inhibitor 1-10 weight portion, mix homogeneously, it is thus achieved that B component.
Component A, B are mixed by weight for 1:4, obtains a kind of water white transparency, cold-hot impact is good, refractive index is high
LED encapsulation organic silica gel.
LED encapsulation organic silica gel of the present invention can be used for the making field of optical lens.
Concrete scheme is as follows:
A kind of LED encapsulation organic silica gel, the weight ratio including component A and B component, component A and B component is 1:4,
Described component A is prepared by the raw material of following weight portion:
Organic siliconresin containing vinyl: 25-50 part
Catalyst: 0.1-0.5 part
Viscosifier: 1-3 part；
Described B component is prepared by the raw material of following weight portion:
Organic siliconresin containing vinyl: 100-120 part
Hydrogeneous organic siliconresin: 80-130 part
Inhibitor: 1-10 part.
Further, the molecular formula of the described organic siliconresin containing vinyl is (ViMe2SiO1/2)x(Ph2SiO)y
(PhSiO3/2) z, wherein Vi is vinyl, and Ph is phenyl, x+y+z=1, x:z=1:3-5.
Further, described catalyst is the compound of platiniferous or palladium.
Further, described viscosifier are silane coupler；
Optional, described viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane.
Further, the molecular formula of described hydrogeneous organic siliconresin is (HMe2SiO1/2)x(Ph2SiO)y(PhSiO3/2)
Z, wherein Ph is phenyl, x+y+z=1, x:z=1:2-3.
Further, described inhibitor is in alkynol compound, many vinyl polysiloxane or amide compound
Any one；
Optional, described inhibitor is 1-acetenyl-1-Hexalin or 2-methyl-3-butyne-2-alcohol.
The application in making LED lamp bar or optical lens of the LED encapsulation organic silica gel.
The preparation method of LED encapsulation organic silica gel, including preparation process and the preparation process of B component of component A；Its
In,
The preparation process of component A: by the water of 5-15 weight portion, the hydrolyst hydrochloric acid of 0.1 weight portion adds reactor
Mixing, described hydrochloric acid be mass fraction be the aqueous hydrochloric acid solution of 20%, take tetramethyl divinyl two silica of 3-5 weight portion
The dimethoxydiphenylsilane mix homogeneously of alkane, the phenyltrimethoxysila,e of 20-50 weight portion, and 4-8 weight portion is in 65
It is added dropwise to reactor under DEG C stirring condition, reacts 3 hours after dropping, then divide water, decompression to steam solvent with unreacted
Monomer, obtains the organic siliconresin containing vinyl；Take 25-50 weight portion the obtained organic siliconresin containing vinyl,
The catalyst of 0.1-0.5 weight portion, the viscosifier mix homogeneously of 1-3 weight portion, it is thus achieved that component A；
The preparation process of B component: the hydrolyst hydrochloric acid of the water of 5-15 weight portion, 0.1 weight portion is added reaction
Still mix, described hydrochloric acid be mass fraction be the aqueous hydrochloric acid solution of 20%, take 4-8 weight portion tetramethyl dihydro two silica
The dimethoxydiphenylsilane mix homogeneously of alkane, the phenyltrimethoxysila,e of 15-25 weight portion, and 4-8 weight portion is in 65
It is added dropwise to reactor under DEG C stirring condition, reacts 3 hours after dropping, then divide water, decompression to steam solvent with unreacted
Monomer, obtains hydrogeneous organic siliconresin；Take obtained hydrogeneous organic siliconresin 80-130 weight portion, the preparation process of component A
The organic siliconresin 100-120 weight portion containing vinyl obtained by, inhibitor 1-10 weight portion, mix homogeneously, it is thus achieved that B group
Point.
Beneficial effect: LED encapsulation organic silica gel water white transparency of the present invention, cold-hot impact is good, refractive index is high,
Its preparation method is easy, and decreases the output of spent acid, is of value to protection environment.LED encapsulation organosilicon of the present invention
Glue overcomes conventional encapsulant poor heat resistance, the shortcoming of easy xanthochromia, it is also possible to according to the demand of application to the viscosity of silica gel, hard
Degree, adhesive force are adjusted.
Detailed description of the invention
Below in conjunction with embodiment, technical solution of the present invention is further elaborated.Unreceipted concrete technology or bar in embodiment
Part person, according to the technology described by the document in this area or condition or is carried out according to product description.Agents useful for same or instrument
Device unreceipted production firm person, be can by city available from conventional products.
Embodiment 1: synthetic sample 1
In the present embodiment hydrolyst be mass fraction be the aqueous hydrochloric acid solution of 20%, silicon hydrogen reaction catalyst for containing
Platinum catalyst, its platinum content is 0.37%, and viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane, and inhibitor is
1-acetenyl-1-Hexalin.
The preparation method of the organic siliconresin containing vinyl in component A is:
First weigh the water of 7.2 kilograms and the hydrolyst hydrochloric acid of 0.1 kilogram is poured in reactor and mixed, then
Weigh the tetramethyl divinyl disiloxane of 3.7 kilograms, the phenyltrimethoxysila,e of 23.8 kilograms and the hexichol of 4.9 kilograms
Base dimethoxysilane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is delayed
Slowly it is added drop-wise in reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain
Organic siliconresin containing vinyl.The organosilicon containing vinyl of different viscosities wherein can be obtained according to the mass ratio that silane is different
Resin.
Wherein in B component, the preparation method of hydrogeneous organic siliconresin is:
First weigh the water of 6.1 kilograms and the hydrolyst hydrochloric acid of 0.1 kilogram is poured in reactor and mixed, then
Weigh the diphenyl two of the tetramethyldihydrogendisiloxane of 5.4 kilograms, the phenyltrimethoxysila,e of 19.8 kilograms and 4.9 kilograms
Methoxy silane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dripped
It is added in reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain hydrogeneous
Organic siliconresin.The hydrogeneous organic siliconresin of different viscosities wherein can be obtained according to the mass ratio that silane is different.
By 485.6 kilograms of platinum catalysts with 1 kilogram of the organic siliconresin containing vinyl, mix all with 24 kilograms of viscosifier
Even preparation component A, by the organic siliconresin containing vinyl 1164.4 kilograms, hydrogeneous organic siliconresin 850 kilograms and inhibitor 32
Kilogram mix homogeneously prepares B component.A, B component 1:4 in proportion is mixed, obtain a kind of water white transparency, cold-hot impact good,
The LED encapsulation organic silica gel that refractive index is high.
Embodiment 2: synthetic sample 2
In the present embodiment hydrolyst be mass fraction be the aqueous hydrochloric acid solution of 20%, silicon hydrogen reaction catalyst for containing
Palladium catalyst, its palladium content is 0.37%, and viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane, and inhibitor is
2-methyl-3-butyne-2-alcohol.
The preparation method of the organic siliconresin containing vinyl in component A is:
First weigh the water of 9.9 kilograms and the hydrolyst of 0.1 kilogram is poured in reactor and mixed, then weigh
The diphenyl two of the tetramethyl divinyl disiloxane of 3.7 kilograms, the phenyltrimethoxysila,e of 33.7 kilograms and 4.9 kilograms
Methoxy silane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dripped
It is added in reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain containing second
The organic siliconresin of thiazolinyl.The organosilicon tree containing vinyl of different viscosities wherein can be obtained according to the mass ratio that silane is different
Fat.
Wherein in B component, the preparation method of hydrogeneous organic siliconresin is:
First weigh the water of 8.8 kilograms and the hydrolyst of 0.1 kilogram is poured in reactor and mixed, then weigh
The diphenyl dimethoxy of the tetramethyldihydrogendisiloxane of 5.4 kilograms, the phenyltrimethoxysila,e of 29.7 kilograms and 4.9 kilograms
Base silane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dropped to
In reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain hydrogeneous organic
Silicones.The hydrogeneous organic siliconresin of different viscosities wherein can be obtained according to the mass ratio that silane is different.
By 485.6 kilograms of platinum catalysts with 1 kilogram of the organic siliconresin containing vinyl, the viscosifier with 25 kilograms mix
Uniformly preparation component A, by the organic siliconresin containing vinyl 1164.4 kilograms, hydrogeneous organic siliconresin 850 kilograms and inhibitor
32 kilograms of mix homogeneously prepare B component.A, B component 1:4 in proportion is mixed, obtains a kind of water white transparency, cold-hot impact
The LED encapsulation organic silica gel good, refractive index is high.
Embodiment 3: synthetic sample 3
In the present embodiment hydrolyst be mass fraction be the aqueous hydrochloric acid solution of 20%, silicon hydrogen reaction catalyst for containing
Platinum catalyst, its platinum content is 0.37%, and viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane, and inhibitor is
Amide compound, specially DMF.
The preparation method of the organic siliconresin containing vinyl in component A is:
First weigh the water of 12.6 kilograms and the hydrolyst of 0.1 kilogram is poured in reactor and mixed, then claim
Take the tetramethyl divinyl disiloxane of 3.7 kilograms, the phenyltrimethoxysila,e of 43.6 kilograms and the diphenyl of 4.9 kilograms
Dimethoxysilane mix homogeneously is placed in Dropping funnel.Then under the conditions of 65 DEG C, while stirring that mixed solution is slow
It is added drop-wise in reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, contained
The organic siliconresin of vinyl.The organosilicon tree containing vinyl of different viscosities wherein can be obtained according to the mass ratio that silane is different
Fat.
Wherein in B component, the preparation method of hydrogeneous organic siliconresin is:
First weigh the water of 11.5 kilograms and the hydrolyst of 0.1 kilogram is poured in reactor and mixed, then claim
Take the diphenyl diformazan of the tetramethyldihydrogendisiloxane of 5.4 kilograms, the phenyltrimethoxysila,e of 39.7 kilograms and 4.9 kilograms
TMOS mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly added dropwise
In reactor.Reacting 3 hours after dropping, then divide water, decompression steams solvent and unreacted monomer, obtains hydrogeneous having
Machine silicones.The hydrogeneous organic siliconresin of different viscosities wherein can be obtained according to the mass ratio that silane is different.
The viscosifier of 485.6 kilograms of platinum catalysts with 1 kilogram of the organic siliconresin containing vinyl and 25 kilograms are mixed
Uniformly preparation component A, by the organic siliconresin containing vinyl 1164.4 kilograms, hydrogeneous organic siliconresin 850 kilograms and inhibitor
32 kilograms of mix homogeneously prepare B component.A, B component 1:4 in proportion is mixed, obtains a kind of water white transparency, cold-hot impact
The LED encapsulation organic silica gel good, refractive index is high.
Embodiment 4: synthetic sample 4
In the present embodiment hydrolyst be mass fraction be the aqueous hydrochloric acid solution of 20%, silicon hydrogen reaction catalyst for containing
Platinum catalyst, its platinum content is 0.37%, and viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane, and inhibitor is
Many vinyl polysiloxane, the double phenyl polysiloxane of the most vinyls.
The preparation method of the organic siliconresin containing vinyl in component A is:
First weigh the water of 7.9 kilograms and the hydrolyst of 0.1 kilogram is poured in reactor and mixed, then weigh
The diphenyl two of the tetramethyl divinyl disiloxane of 3.7 kilograms, the phenyltrimethoxysila,e of 23.8 kilograms and 9.8 kilograms
Methoxy silane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dripped
It is added in reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain containing second
The organic siliconresin of thiazolinyl.The organosilicon tree containing vinyl of different viscosities wherein can be obtained according to the mass ratio that silane is different
Fat.
Wherein in B component, the preparation method of hydrogeneous organic siliconresin is:
First weigh the water of 6.8 kilograms and the hydrolyst of 0.1 kilogram is poured in reactor and mixed, then weigh
The diphenyl dimethoxy of the tetramethyldihydrogendisiloxane of 5.4 kilograms, the phenyltrimethoxysila,e of 19.8 kilograms and 9.8 kilograms
Base silane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dropped to
In reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain hydrogeneous organic
Silicones.The hydrogeneous organic siliconresin of different viscosities wherein can be obtained according to the mass ratio that silane is different.
The viscosifier of 485.6 kilograms of platinum catalysts with 1 kilogram of the organic siliconresin containing vinyl and 25 kilograms are mixed
Uniformly preparation component A, by the organic siliconresin containing vinyl 1164.4 kilograms, hydrogeneous organic siliconresin 850 kilograms and 32 kilograms
Inhibitor mixed uniformly prepares B component.A, B component 1:4 in proportion is mixed, obtains a kind of water white transparency, cold-hot impact
The LED encapsulation organic silica gel good, refractive index is high.
Embodiment 5: performance characterization
Sample 1-4 obtained by embodiment 1-4 is carried out performance characterization:
1) light transmittance: use ultraviolet-visible spectrophotometer, measuring thickness is 1cm colloid printing opacity at 450-800nm
Rate, averages.
2) viscosity: use NDJ-79 rotating cylinder viscometer, test viscosity of colloid under the conditions of 25 DEG C.
3) hardness: use LX-D type Shore durometer, by hot-air-circulation oven, heats 1 little at 100 DEG C
Time, heat 4 hours at 150 DEG C, it is thus achieved that firming body, be down to room temperature, use the hardness of Shore durometer test solidfied material.
4) refractive index: use W type Abbe refractometer, test passes the refractive index of uncured colloid at 25 DEG C.
5) thermal shock test: use two slot type thermal shock test chambers, tests solidfied material 30min at 100 DEG C, and-40
30min at DEG C, circulates 100 times.Carrying out lighting test, calculating fraction defective, determine the qualification of product.Experimental result such as following table
Shown in,
Table 1 properties of sample test result table
The test result listed from table 1, prepared sample all meets city in the face of the general test requirement of organic silica gel.
The refractive index of the organic silica gel of 50% is about 1.53 the most on the market, and the organic silica gel refractive index of 30% is higher than 1.54, this
In bright prepared embodiment sample, the refractive index of organic silica gel is all more than 1.54, and light transmittance is up to 98%, and hardness is
D50.The most typically requiring in thermal shock test that 100 fraction defectives are 0 to be considered as qualified, wherein, sample 1 tests 150 times not
Yield is 0, and sample 2 has adhered to just occurring bad 150 times, it is seen that sample 1 and 2 fully meets requirement；105 ability tested by sample 3
Occurring bad, it is bad that 103 appearance tested by sample 4, it is seen that sample 3 and 4 also substantially meets Eligibility requirements.
LED encapsulation organic silica gel of the present invention prepares simplicity, and environmental pollution is little, has from performance detection
The mechanical performance that high refractive index, light transmittance are high and strong, overcomes conventional encapsulant poor heat resistance, the shortcoming of easy xanthochromia, goes back
According to the demand of application, the viscosity of silica gel, hardness, adhesive force can be adjusted, excellent performance.
Embodiment 6
In the present embodiment hydrolyst be mass fraction be the aqueous hydrochloric acid solution of 20%, silicon hydrogen reaction catalyst for containing
Platinum catalyst, its platinum content is 0.37%, and viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane, and inhibitor is
1-acetenyl-1-Hexalin.
The preparation method of the organic siliconresin containing vinyl in component A is:
First weigh the water of 5 kilograms and the hydrolyst hydrochloric acid of 0.1 kilogram is poured in reactor and mixed, then claim
Take the diphenyl dimethoxy of the tetramethyl divinyl disiloxane of 3 kilograms, the phenyltrimethoxysila,e of 20 kilograms and 4 kilograms
Base silane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dropped to
In reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain containing vinyl
Organic siliconresin.The organic siliconresin containing vinyl of different viscosities wherein can be obtained according to the mass ratio that silane is different.
Wherein in B component, the preparation method of hydrogeneous organic siliconresin is:
First weigh the water of 5 kilograms and the hydrolyst hydrochloric acid of 0.1 kilogram is poured in reactor and mixed, then claim
Take the diphenyl dimethoxy silicon of the tetramethyldihydrogendisiloxane of 4 kilograms, the phenyltrimethoxysila,e of 15 kilograms and 4 kilograms
Alkane mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dropped to reaction
In still.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain hydrogeneous organosilicon tree
Fat.The hydrogeneous organic siliconresin of different viscosities wherein can be obtained according to the mass ratio that silane is different.
By 25 kilograms of platinum catalysts with 0.1 kilogram of the organic siliconresin containing vinyl, mix homogeneously with 1 kilogram of viscosifier
Preparation component A, mixes the organic siliconresin containing vinyl 100 kilograms, hydrogeneous organic siliconresin 80 kilograms with inhibitor 1 kilogram
Uniformly prepare B component.A, B component 1:4 in proportion is mixed, obtains a kind of water white transparency, cold-hot impact is good, refractive index is high
LED encapsulation organic silica gel.
Embodiment 7
In the present embodiment hydrolyst be mass fraction be the aqueous hydrochloric acid solution of 20%, silicon hydrogen reaction catalyst for containing
Platinum catalyst, its platinum content is 0.37%, and viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane, and inhibitor is
1-acetenyl-1-Hexalin.
The preparation method of the organic siliconresin containing vinyl in component A is:
First weigh the water of 15 kilograms and the hydrolyst hydrochloric acid of 0.1 kilogram is poured in reactor and mixed, then
Weigh the diphenyl diformazan of the tetramethyl divinyl disiloxane of 5 kilograms, the phenyltrimethoxysila,e of 50 kilograms and 8 kilograms
TMOS mix homogeneously is placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly added dropwise
In reactor.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain containing ethylene
The organic siliconresin of base.The organic siliconresin containing vinyl of different viscosities wherein can be obtained according to the mass ratio that silane is different.
Wherein in B component, the preparation method of hydrogeneous organic siliconresin is:
First weigh the water of 15 kilograms and the hydrolyst hydrochloric acid of 0.1 kilogram is poured in reactor and mixed, then
Weigh the tetramethyldihydrogendisiloxane of 8 kilograms, the phenyltrimethoxysila,e of 25 kilograms and the diphenyl dimethoxy of 8 kilograms
Silane mixture is uniformly placed in Dropping funnel.Then, under the conditions of 65 DEG C, while stirring mixed solution is slowly dropped to instead
Answer in still.React 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer, obtain hydrogeneous organosilicon
Resin.The hydrogeneous organic siliconresin of different viscosities wherein can be obtained according to the mass ratio that silane is different.
By 50 kilograms of platinum catalysts with 0.5 kilogram of the organic siliconresin containing vinyl, mix homogeneously with 3 kilograms of viscosifier
Preparation component A, mixes the organic siliconresin 120 kg containing vinyl, hydrogeneous organic siliconresin 130 kilograms with inhibitor 10 kilograms
Close and uniformly prepare B component.A, B component 1:4 in proportion is mixed, obtains that a kind of water white transparency, cold-hot impact be good, refractive index
High LED encapsulation organic silica gel.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is example
Property, it is impossible to be interpreted as limitation of the present invention, those of ordinary skill in the art is without departing from the principle of the present invention and objective
In the case of above-described embodiment can be changed within the scope of the invention, revise, replace and modification.
Claims (8)
1. a LED encapsulation organic silica gel, it is characterised in that: include the weight ratio of component A and B component, component A and B component
For 1:4,
Described component A is prepared by the raw material of following weight portion:
Organic siliconresin containing vinyl: 25-50 part
Catalyst: 0.1-0.5 part
Viscosifier: 1-3 part；
Described B component is prepared by the raw material of following weight portion:
Organic siliconresin containing vinyl: 100-120 part
Hydrogeneous organic siliconresin: 80-130 part
Inhibitor: 1-10 part.
LED encapsulation organic silica gel the most according to claim 1, it is characterised in that: the described organosilicon containing vinyl
The molecular formula of resin is (ViMe2SiO1/2)x(Ph2SiO)y(PhSiO3/2) z, wherein Vi is vinyl, and Ph is phenyl, x+y+z=
1, x:z=1:3-5.
LED encapsulation organic silica gel the most according to claim 1, it is characterised in that: described catalyst be platiniferous or
The compound of palladium.
LED encapsulation organic silica gel the most according to claim 1, it is characterised in that: described viscosifier are silane coupled
Agent；
Optional, described viscosifier are γ-(2,3-glycidyl) propyl trimethoxy silicane.
LED encapsulation organic silica gel the most according to claim 1, it is characterised in that: described hydrogeneous organic siliconresin
Molecular formula is (HMe2SiO1/2)x(Ph2SiO)y(PhSiO3/2) z, wherein Ph is phenyl, x+y+z=1, x:z=1:2-3.
LED encapsulation organic silica gel the most according to claim 1, it is characterised in that: described inhibitor is alkynol class
Any one in compound, many vinyl polysiloxane or amide compound；
Optional, described inhibitor is 1-acetenyl-1-Hexalin or 2-methyl-3-butyne-2-alcohol.
7. in claim 1 to 6 LED encapsulation organic silica gel described in any one in making LED lamp bar or optical lens
Application.
8. the preparation method of LED encapsulation organic silica gel described in any one in claim 1 to 6, including the preparation of component A
Step and the preparation process of B component；Wherein,
The preparation process of component A: by the water of 5-15 weight portion, the hydrolyst hydrochloric acid of 0.1 weight portion adds reactor mixing,
Described hydrochloric acid be mass fraction be the aqueous hydrochloric acid solution of 20%, take the tetramethyl divinyl disiloxane of 3-5 weight portion,
The phenyltrimethoxysila,e of 20-50 weight portion, and the dimethoxydiphenylsilane mix homogeneously of 4-8 weight portion stirs in 65 DEG C
It is added dropwise to reactor under the conditions of mixing, reacts 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer,
Obtain the organic siliconresin containing vinyl；Take the obtained organic siliconresin containing vinyl of 25-50 weight portion, 0.1-0.5
Catalyst described in the claim 3 of weight portion, 1-3 weight portion claim 4 described in viscosifier mix homogeneously, obtain
Obtain component A；
The preparation process of B component: the hydrolyst hydrochloric acid of the water of 5-15 weight portion, 0.1 weight portion is added reactor and mixes
Close, described hydrochloric acid be mass fraction be the aqueous hydrochloric acid solution of 20%, take 4-8 weight portion tetramethyldihydrogendisiloxane,
The phenyltrimethoxysila,e of 15-25 weight portion, and the dimethoxydiphenylsilane mix homogeneously of 4-8 weight portion stirs in 65 DEG C
It is added dropwise to reactor under the conditions of mixing, reacts 3 hours after dropping, then divide water, decompression to steam solvent and unreacted monomer,
Obtain hydrogeneous organic siliconresin；Take in the preparation process of obtained hydrogeneous organic siliconresin 80-130 weight portion, component A made
The organic siliconresin 100-120 weight portion containing vinyl, the inhibitor 1-10 weight portion described in claim 6, mixing
Uniformly, it is thus achieved that B component.
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