CN106046380A - An LED encapsulating material, a preparing method thereof and application of the material - Google Patents
An LED encapsulating material, a preparing method thereof and application of the material Download PDFInfo
- Publication number
- CN106046380A CN106046380A CN201610290361.3A CN201610290361A CN106046380A CN 106046380 A CN106046380 A CN 106046380A CN 201610290361 A CN201610290361 A CN 201610290361A CN 106046380 A CN106046380 A CN 106046380A
- Authority
- CN
- China
- Prior art keywords
- reaction vessel
- reaction
- led encapsulation
- hydride
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
-
- 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
-
- 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
-
- 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
Abstract
The invention relates to an LED encapsulating material. The material is prepared from a vinyl compound A, a cyclohexyl methylsiloxane-carbonyl-platinum composite, 3,5-dimethyl-1-hexyn-3-ol, a hydride B and phenyl vinyl methylsilane. The chemical structural formula of the vinyl compound A is shown in the specification. The chemical structural formula of the hydride B is shown in the specification. The chemical structural formula of the material is shown in the specification, wherein x, y, u and v are not more than 2000 and not less than 0, Me represents methyl CH<3>- and Ph represents phenyl C<6>H<5>-. Compared with the prior art, the material has advantages of excellent transmissivity and refractive indexes in each waveband, excellent heat resistance, low optical performance degradation, good fluidity before heating and curing, convenience for effective encapsulating for light emitting diodes, a simple preparing method, and simple, convenient and efficient applications.
Description
Technical field
The invention belongs to technical field of semiconductors, particularly relate to a kind of LED encapsulation material and preparation method thereof, application.
Background technology
High brightness LED based on gallium nitride semiconductor material (LED) becomes with unit illumination along with the maturation of technology
This reduction, it is expected to replace traditional electric filament lamp and fluorescent lamp.In order to reduce the cost of light emitting diode unit illumination, high folding
The encapsulating material penetrating rate can more launch light from gallium nitride surface extraction, and this is due to when light is from high-refractive-index regions
When (gallium nitride is about 2.5) travels to region of low refractive index, there is whole inner reflection.Between encapsulating material and luminescent substance
There is refractive index not mate and cause extra light loss.The refractive index of major part encapsulating material is 1.5～1.7, although this can
Increase by the light output of 5%～10%, but the encapsulating material being applied to light emitting diode needs to meet heat stability height, light simultaneously
Flux stabilized, the integrated condition such as with low cost.
Most current light emitting diode is to reach encapsulation by the post-heating solidification that is uniformly dispersed liquid encapsulating material
Effect.It is solvent-free liquid formulation that the encapsulating material of light emitting diode requires, which has limited the material of major part high index of refraction
Being applied to LED package field, meanwhile, light-emitting diode packaging material also needs to have good light transmittance, thermally-stabilised
Property and light stability.
Existing light-emitting diode packaging material is at aspects such as material flowability, reliability, thermal insulation and optical property decay
Still suffer from a lot of problem, need badly and develop a kind of novel encapsulating material being applied to light emitting diode.
The present invention proposes a kind of encapsulating material based on Phenoxyphenyl silicone being applied to light emitting diode and system thereof
Preparation Method, application.
Summary of the invention
The technical problem to be solved in the present invention be to improve existing light-emitting diode packaging material material flowability, can
By the deficiency in terms of property, thermal insulation and optical property decay, it is an object of the invention to propose a kind of novel LED encapsulation material and
Its preparation method, application.
The present invention is by the following technical solutions: a kind of LED encapsulation material, and it is prepared from the following materials: vinylated
Compound A, ring ethyl-methyl siloxanes-carbonyl-platinum complexes, 3,5-dimethyl-1-hexin-3-alcohol, hydride B, phenylethylene
Butyldimethylsilyl, the chemical structural formula of described vinyl compound A isThe change of described hydride B
Structural formula isIts 0≤x, y, u, v≤2000, Me represents methyl CH3-, Ph represents phenyl
C6H5-。
As a further improvement on the present invention, the chemical structural formula of described encapsulating material is:
Wherein, 0≤x, y, u, v≤2000, Me represents methyl CH3-, Ph represents phenyl C6H5-。
Further, described encapsulating material can preserve at least 6 months under the conditions of less than 4 DEG C.
Also propose the preparation method of a kind of LED encapsulation material, comprise the steps:
Step S1: in reaction vessel add vinyl compound A, sequentially add ring ethyl-methyl siloxanes-carbonyl-
Platinum complexes and 3,5-dimethyl-1-hexin-3-alcohol, vinyl compound A, ring ethyl-methyl siloxanes-carbonyl-platinum is combined
Thing, 3, the mass ratio of 5-dimethyl-1-hexin three kinds of materials of-3-alcohol is 30～50: 7～11: 1～3；
Step S2: reaction vessel under the conditions of 50 DEG C～70 DEG C, with the speed of 200RPM～400RPM continuously stirred 30～
60 minutes；
Step S3: hydride B and phenylethylene butyldimethylsilyl are added form mixture in reaction vessel successively, its
In, vinyl compound A, hydride B, the mass ratio of phenylethylene butyldimethylsilyl three are 30～50: 10～20: 3～5,
Under the conditions of reaction vessel is placed in 50 DEG C～70 DEG C, with continuously stirred 1～2 hour of the speed of 200RPM～400RPM；
Step S4: after reaction terminates, mixture is cooled to 25 DEG C of room temperatures, obtains encapsulating material.
Further, the preparation method of described vinyl compound A is as follows: comprise the following steps:
Step D1: 4-(Phenoxyphenyl) phenyidimethoxysilane is added in reaction vessel, then toward in reaction vessel
It is sequentially added into dimethoxydiphenylsilane, phenyl methyl vinyl methoxy silane, deionized water and 30wt%～50wt%
TBAH aqueous solution, 4-(Phenoxyphenyl) phenyidimethoxysilane, dimethoxydiphenylsilane, phenyl
Ethylene methacrylic methoxylsilane, deionized water, TBAH aqueous solution five kinds of materials of 30wt%～50wt%
Mass ratio is 210～230: 230～250: 30～50: 80～100: 13～15；
Step D2: reaction vessel is under the conditions of 70 DEG C～90 DEG C, with the speed of 200RPM～400RPM continuously stirred 5～7
Hour, in course of reaction, by-product carbinol is distilled out；
Step D3: after reaction terminates, the residue after being distilled, reaction vessel is cooled to 25 DEG C of room temperatures, toward reaction
Being sequentially added into toluene in container and deionized water obtains mixing liquid, toluene and deionized water volume ratio are 1～2: 1～2, will be mixed
Close after liquid addition separatory funnel shakes 60～120 seconds, stand to layering, discharge aqueous phase, retain organic facies；
Step D4: successively by the salt acid elution organic facies three times that wt/wt mass ratio is 4%～6%, be washed with deionized
Organic facies twice；
Step D5: organic facies filtered and passes through the toluene in rotary evaporation removing organic facies, obtaining vinyl compound
A。
Further, the preparation method of described 4-(Phenoxyphenyl) phenyidimethoxysilane is as follows: include as follows
Step:
Step L1: be sequentially added into ether, magnesium powder, iodomethane, ether, magnesium powder, three kinds of materials of iodomethane in reaction vessel a
Mass ratio be 400～600: 8～12: 0.2～0.3；
Step L2: reaction vessel a stirs 5～7 hours under 25 DEG C of room temperature, during stirring reaction, 4-dibromodiphenyl ether passes through
Dropping funnel was added dropwise in reaction vessel a in 5～7 hours, 4-dibromodiphenyl ether and the matter of the iodomethane of addition in step L1
Amount ratio is 80～120: 0.2～0.3；
Step L3: be sequentially added into phenyltrimethoxysila,e and absolute ether in reaction vessel b, mass ratio is 70～90
: 130～150, continue 1～2 hour 25 DEG C of stirring at normal temperature reactions；
Step L4: during stirring reaction, pipette solution in a certain amount of reaction vessel a with syringe, in 1～2 hour
Dropwise it is added drop-wise in reaction vessel b be formed mixed liquor, wherein, in the reaction vessel a that syringe pipettes in solution and reaction vessel b
The mass ratio of solution is 80～120: 200～230；
Step L5: after reaction terminates, the mixed liquor in reaction vessel b is filtrated to get diethyl ether solution, then that ether is molten
Liquid is dried by anhydrous magnesium sulfate, finally will filter except the diethyl ether solution after water, rotary evaporation, obtains crude product；
Step L6: crude product step L5 obtained is removed by distillation low boiling impurity and obtains pure 4-(phenoxy group
Phenyl) phenyidimethoxysilane.
Further, described hydride B is prepared from by following preparation method: comprise the steps:
Step N1: by dimethoxydiphenylsilane, methyl-hydrogen-annular siloxane, deionized water, the concentrated sulphuric acid of 98%
Adding in reaction vessel, four kinds of material mass ratios are 280～300: 100～120: 70～90: 20～40；
Step N2: reaction vessel is under the conditions of 70 DEG C～90 DEG C, with the speed of 200RPM～400RPM continuously stirred 3～6
Hour, in course of reaction, by-product carbinol is distilled out；
Step N3: reaction terminate after, reaction vessel is cooled to 25 DEG C of room temperatures, be sequentially added into toward reaction vessel in toluene with
Deionized water, toluene and deionized water volume ratio are 1～2: 1～2, and mixing liquid is added shake 60～120 in separatory funnel
After Miao, stand to layering, discharge aqueous phase, retain organic facies；
Step N4: organic facies is washed 4 times, by organic facies mistake with saturated sodium bicarbonate solution washing 1 time, deionization successively
Filter and pass through rotary evaporation and remove toluene, obtain hydride B.
Further, the chemical structural formula of described 4-(Phenoxyphenyl) phenyidimethoxysilane is
The application of a kind of LED encapsulation material, adds encapsulating material in LED device, at 130 DEG C～150 DEG C
Heat 2～4 hours so that it is be heating and curing formation cross linked polymer further, to complete the encapsulation to light emitting diode.
The present invention compared with the existing technology, provides the benefit that: all show absorbance and the refraction of excellence in each wavelength period
Rate；Good Heat-resistance, optical property decay is low；Good fluidity before being heating and curing, it is simple to light emitting diode is effectively encapsulated；
Preparation method is simple, applies simple and effective.
Detailed description of the invention
In order to make those skilled in the art be more fully understood that technical scheme, and make the present invention features described above,
Purpose and advantage become apparent from understandable, it is to be appreciated that embodiment is merely to illustrate the present invention rather than limits the present invention
Scope.
Product embodiments 1
The present embodiment one LED encapsulation material is prepared from the following materials: vinyl compound A, ring ethyl-methyl silicon
Oxygen alkane-carbonyl-platinum complexes, 3,5-dimethyl-1-hexin-3-alcohol, hydride B, phenylethylene butyldimethylsilyl, vinylated
The chemical structural formula of compound A isThe chemical structural formula of hydride B isIts 0≤x, y, u, v≤2000, Me represents methyl CH3-, Ph represents phenyl C6H5-。
The chemical structural formula of above-mentioned encapsulating material is:Wherein,
0≤x, y, u, v≤2000, Me represents methyl CH3-, Ph represents phenyl C6H5-, this encapsulating material can be protected under the conditions of less than 4 DEG C
Deposit at least 6 months.
Embodiment of the method
The said goods embodiment can prepare according to following preparation method, the preparation method of a kind of LED encapsulation material, including
Following steps:
Step S1: add 43.25g vinyl compound A in round-bottomed flask, sequentially add 8.8uL ring ethyl-methyl
Siloxanes-carbonyl-platinum complexes and 1.8uL3,5-dimethyl-1-hexin-3-alcohol；
Step S2: round-bottomed flask was under the conditions of 60 DEG C, with continuously stirred 45 minutes of the speed of 300RPM；
Step S3: 16.33g hydride B and 3.62g phenylethylene butyldimethylsilyl are added in round-bottomed flask formed successively
Mixture, wherein, under the conditions of reaction vessel is placed in 60 DEG C, with continuously stirred 1.5 hours of the speed of 250RPM；
Step S4: after reaction terminates, mixture is cooled to 25 DEG C of room temperatures, obtains encapsulating material.
In other embodiments, the vinyl compound A in step S1, ring ethyl-methyl siloxanes-carbonyl-platinum are combined
Thing, 3, in the range of the mass ratio of 5-dimethyl-1-hexin three kinds of materials of-3-alcohol remains 30～50: 7～11: 1～3；On
Stating in step S2, round-bottomed flask is under the conditions of 50 DEG C～70 DEG C, with continuously stirred 30～60 points of the speed of 200RPM～400RPM
Clock；In above-mentioned steps S3, vinyl compound A, hydride B, the mass ratio of phenylethylene butyldimethylsilyl three are 30
～50: 10～20: 3～5, under the conditions of round-bottomed flask is placed in 50 DEG C～70 DEG C, hold with the speed of 200RPM～400RPM
Continuous stirring 1～2 hour.
The preparation method of above-mentioned vinyl compound A is as follows: comprise the following steps:
Step D1: 220.38g 4-(Phenoxyphenyl) phenyidimethoxysilane is added in three neck round bottom flask, then
243.28g dimethoxydiphenylsilane, 44.38g phenyl methyl ethenylmethoxy it is sequentially added in three neck round bottom flask
The TBAH aqueous solution of silane, 93.73g deionized water and 14.79g 40wt%；
Step D2: three neck round bottom flask is under the conditions of 80 DEG C, with continuously stirred 6 hours of the speed of 300RPM, course of reaction
In, by-product carbinol is distilled out in the three neck round bottom flask using 1L builds the distilling apparatus of formation with condensing tube；
Step D3: after reaction terminates, the residue after being distilled, treat that the residue in three neck round bottom flask is cooled to 25
DEG C room temperature, in three neck round bottom flask, 450mL toluene and 400mL deionized water obtain mixing liquid, are added point by mixing liquid
After liquid funnel shakes 80 seconds, stand to layering, discharge aqueous phase, retain organic facies；
Step D4: successively by the salt acid elution organic facies three times that 800mL mass ratio is 5%, use 800mL deionized water wash
Organic facies twice；
Step D5: organic facies filtered and passes through the toluene in rotary evaporation removing organic facies, obtaining 418.68g vinyl
Compound A.
In other embodiments, 4-(Phenoxyphenyl) phenyidimethoxysilane, diphenyl dimethoxy in step D1
Silane, phenyl methyl vinyl methoxy silane, deionized water, the TBAH aqueous solution five of 30wt%～50wt%
In the mass ratio of kind material is maintained at 210～230: 230～250: 30～50: 80～100: 13～15；In step D2 three
Mouthful round-bottomed flask was under the conditions of 70 DEG C～90 DEG C, with continuously stirred 5～7 hours of the speed of 200RPM～400RPM；Step
In D3, toluene and deionized water volume ratio are 1～2: 1～2, and mixing liquid is added shake 60～120 seconds in separatory funnel
?.
Being applied to 4-(Phenoxyphenyl) phenyidimethoxysilane in above-mentioned preparation method, its chemical structural formula is:The synthesis of 4-(Phenoxyphenyl) phenyidimethoxysilane is carried out in glove box, including as follows
Step:
Step L1: be sequentially added into 800mL ether, 10g magnesium powder, 0.1mL iodomethane in round-bottomed flask a；
Step L2: round-bottomed flask a stirs 6 hours under 25 DEG C of room temperature, during stirring reaction, by 100g 4-dibromodiphenyl ether
It is added dropwise in round-bottomed flask a in 6 hours by Dropping funnel；
Step L3: be sequentially added into 87.6g phenyltrimethoxysila,e and 200mL absolute ether in round-bottomed flask b, 25
The reaction of DEG C stirring at normal temperature continues 1～2 hour；
Step L4: during stirring reaction, pipette solution 100mL in round-bottomed flask a with syringe, dropwise dripped in 1 hour
It is added in round-bottomed flask b；
Step L5: after reaction terminates, the mixed liquor in round-bottomed flask b is filtrated to get diethyl ether solution, then that ether is molten
Liquid is dried by anhydrous magnesium sulfate, finally will filter except the diethyl ether solution after water, rotary evaporation, obtains 129.1g crude product；
Step L6: 129.1g crude product step L5 obtained is removed by distillation low boiling impurity, and to obtain 121.6g pure
4-(Phenoxyphenyl) phenyidimethoxysilane.
In other embodiments, in step L1, ether, magnesium powder, the mass ratio of three kinds of materials of iodomethane remain 400～600
: 8～12: 0.2～0.3；In step L2, round-bottomed flask a stirs 5～7 hours, correspondingly, 4-under 25 DEG C of room temperature
Dibromodiphenyl ether was added dropwise in round-bottomed flask a by Dropping funnel in 5～7 hours, 4-dibromodiphenyl ether and the iodomethane of addition
Mass ratio be 80～120: 0.2～0.3；In step L3, the mass ratio of phenyltrimethoxysila,e and absolute ether keeps
It is 70～90: 130～150, continues 1～2 hour 25 DEG C of stirring at normal temperature reactions；The round bottom that in step L4, syringe pipettes
In flask a, solution is 80～120: 200～230 with the mass ratio of solution in round-bottomed flask b, and dropping completed i.e. in 1～2 hour
Can；
Above-mentioned hydride B is prepared from by following preparation method: comprise the steps:
Step N1: 293.3g dimethoxydiphenylsilane, 108.0g methyl-hydrogen-annular siloxane, 81.0g are gone from
Sub-water, the concentrated sulphuric acid of 29.42g 98% add in round-bottomed flask；
Step N2: round-bottomed flask is under the conditions of 80 DEG C, with continuously stirred 4.5 hours of the speed of 250RPM, in course of reaction,
By-product carbinol is distilled out；
Step N3: after reaction terminates, round-bottomed flask is cooled to 25 DEG C of room temperatures, is sequentially added into 200mL first in round-bottomed bottle
Benzene and 200mL deionized water, will mix after shaking 90 seconds in liquid addition separatory funnel, stand to being layered, discharge aqueous phase, retain
Organic facies；
Step N4: organic facies is washed 4 times, by organic facies mistake with saturated sodium bicarbonate solution washing 1 time, deionization successively
Filter and pass through rotary evaporation and remove toluene, obtain 337.14g hydride B.
In other embodiments, the mass ratio keeping four kinds of materials in step N1 is 280～300: 100～120: 70～90
: 20～40；In step N2, round-bottomed flask is under the conditions of 70 DEG C～90 DEG C, and the speed with 200RPM～400RPM is continuously stirred
3～6 hours；In step N3, toluene and deionized water volume ratio remain 1～2: 1～2, and mixing liquid is added separatory leakage
Bucket shakes 60～120 seconds.
The LED encapsulation material of excellent is got final product by above step.
Application Example
The encapsulating material prepared according to the method described above is added in LED, heats 3 hours at 140 DEG C so that it is enter one
Walk the formation cross linked polymer that is heating and curing, to complete the encapsulation to LED；After encapsulating material adds LED in other embodiments,
At 130 DEG C～150 DEG C, heating also may be used for 2～4 hours.
Ultraviolet-visible spectrum degradation: take above-mentioned encapsulating material 0.5g and be applied on the piezoid of 1 square inch, 150
Heat 3 hours at DEG C, make material be heating and curing；Under air atmosphere, the high temperature furnace of 200 DEG C stores respectively 12 days, 24 days, 42
It and 70 days, the absorbance of test encapsulating material, absorbance ageing test result shows, preparation-obtained encapsulating material is being grown
Maintain higher absorbance in each wavelength period under time high temperature storage, show good heat-resisting, ageing-resistant performance.
Ultraviolet-visible spectrum refractive index is tested: takes encapsulating material 0.5g and is applied on the piezoid of 1 square inch, at 150 DEG C
Lower heating 3 hours, makes material be heating and curing, and ultraviolet-visible spectrum test shows, encapsulating material shows higher in each wavelength period
Refractive index.
In sum, the present invention compared with the existing technology, has the advantage that and all shows the saturating of excellence in each wavelength period
Penetrate rate and refractive index；Good Heat-resistance, optical property decay is low；Good fluidity before being heating and curing, it is simple to light emitting diode is entered
Row effectively encapsulation；Preparation method is simple, applies simple and effective.
Above-mentioned embodiment is used for illustrative purposes only, and is not limitation of the present invention, relevant technical field
Those of ordinary skill, without departing from the spirit and scope of the present invention, it is also possible to various changes can be made and modification, therefore institute
The technical scheme having equivalent also should belong to scope of the invention.
Claims (9)
1. a LED encapsulation material, it is characterised in that: described encapsulating material is prepared from the following materials: vinyl compound
A, ring ethyl-methyl siloxanes-carbonyl-platinum complexes, 3,5-dimethyl-1-hexin-3-alcohol, hydride B, phenyl vinyl first
Base silane, the chemical structural formula of described vinyl compound A isDescribed hydride B
Chemical structural formula beIts 0≤x, y, u, v≤2000, Me represents methyl CH3-, Ph represents benzene
Base C6H5-。
A kind of LED encapsulation material the most according to claim 1, it is characterised in that: the chemical structural formula of described encapsulating material
For:Wherein, 0≤x, y, u, v≤2000, Me generation
Table methyl CH3-, Ph represents phenyl C6H5-。
A kind of LED encapsulation material the most according to claim 2, it is characterised in that: described encapsulating material is less than 4 DEG C of conditions
Under can preserve at least 6 months.
4. according to the preparation method of the arbitrary described a kind of LED encapsulation material of claim 1-3, it is characterised in that: include as follows
Step:
Step S1: add vinyl compound A in reaction vessel, sequentially add ring ethyl-methyl siloxanes-carbonyl-platinum multiple
Compound and 3,5-dimethyl-1-hexin-3-alcohol, vinyl compound A, ring ethyl-methyl siloxanes-carbonyl-platinum complexes, 3,
The mass ratio of 5-dimethyl-1-hexin three kinds of materials of-3-alcohol is 30～50: 7～11: 1～3；
Step S2: reaction vessel is under the conditions of 50 DEG C～70 DEG C, with continuously stirred 30～60 points of the speed of 200RPM～400RPM
Clock；
Step S3: hydride B and phenylethylene butyldimethylsilyl are added form mixture, wherein, second in reaction vessel successively
Alkenyl compound A, hydride B, the mass ratio of phenylethylene butyldimethylsilyl three are 30～50: 10～20: 3～5, will reaction
Under the conditions of container is placed in 50 DEG C～70 DEG C, with continuously stirred 1～2 hour of the speed of 200RPM～400RPM；
Step S4: after reaction terminates, mixture is cooled to 25 DEG C of room temperatures, obtains encapsulating material.
The preparation method of a kind of LED encapsulation material the most according to claim 3, it is characterised in that: described vinyl chemical combination
The preparation method of thing A is as follows: comprise the following steps:
Step D1: 4-(Phenoxyphenyl) phenyidimethoxysilane is added in reaction vessel, then toward in reaction vessel successively
Add dimethoxydiphenylsilane, phenyl methyl vinyl methoxy silane, deionized water and the four of 30wt%～50wt%
Butyl ammonium hydroxide aqueous solution, 4-(Phenoxyphenyl) phenyidimethoxysilane, dimethoxydiphenylsilane, phenyl methyl
Vinyl methoxy silane, deionized water, the quality of five kinds of materials of TBAH aqueous solution of 30wt%～50wt%
Ratio is 210～230: 230～250: 30～50: 80～100: 13～15；
Step D2: reaction vessel is under the conditions of 70 DEG C～90 DEG C, with continuously stirred 5～7 hours of the speed of 200RPM～400RPM,
In course of reaction, by-product carbinol is distilled out；
Step D3: after reaction terminates, the residue after being distilled, reaction vessel is cooled to 25 DEG C of room temperatures, toward reaction vessel
In be sequentially added into toluene and deionized water obtains mixing liquid, toluene and deionized water volume ratio are 1～2: 1～2, by mixed liquor
After body addition separatory funnel shakes 60～120 seconds, stand to layering, discharge aqueous phase, retain organic facies；
Step D4: successively by the salt acid elution organic facies three times that mass ratio is 4%～6%, be washed with deionized organic facies two
Secondary；
Step D5: organic facies filtered and passes through the toluene in rotary evaporation removing organic facies, obtaining vinyl compound A.
The preparation method of a kind of LED encapsulation material the most according to claim 4, it is characterised in that: described 4-(phenoxy group benzene
Base) preparation method of phenyidimethoxysilane is as follows: comprises the steps:
Step L1: be sequentially added into ether, magnesium powder, iodomethane, ether, magnesium powder, the matter of three kinds of materials of iodomethane in reaction vessel a
Amount ratio is 400～600: 8～12: 0.2～0.3；
Step L2: reaction vessel a stirs 5～7 hours under 25 DEG C of room temperature, during stirring reaction, 4-dibromodiphenyl ether passes through dropping liquid
Funnel was added dropwise in reaction vessel a in 5～7 hours, 4-dibromodiphenyl ether and the mass ratio of the iodomethane of addition in step L1
It is 80～120: 0.2～0.3；
Step L3: be sequentially added into phenyltrimethoxysila,e and absolute ether in reaction vessel b, mass ratio is 70～90: 130
～150, continue 1～2 hour 25 DEG C of stirring at normal temperature reactions；
Step L4: during stirring reaction, pipette solution in a certain amount of reaction vessel a with syringe, in 1～2 hour dropwise
Being added drop-wise in reaction vessel b form mixed liquor, wherein, in the reaction vessel a that syringe pipettes, solution is molten with reaction vessel b
The mass ratio of liquid is 80～120: 200～230；
Step L5: after reaction terminates, the mixed liquor in reaction vessel b is filtrated to get diethyl ether solution, then diethyl ether solution is led to
Cross anhydrous magnesium sulfate to be dried, finally will filter except the diethyl ether solution after water, rotary evaporation, obtain crude product；
Step L6: crude product step L5 obtained is removed by distillation low boiling impurity and obtains pure 4-(Phenoxyphenyl)
Phenyidimethoxysilane.
The preparation method of a kind of LED encapsulation material the most according to claim 5, it is characterised in that: described hydride B by with
Lower preparation method is prepared from: comprise the steps:
Step N1: dimethoxydiphenylsilane, methyl-hydrogen-annular siloxane, deionized water, the concentrated sulphuric acid of 98% are added
In reaction vessel, four kinds of material mass ratios are 280～300: 100～120: 70～90: 20～40；
Step N2: reaction vessel is under the conditions of 70 DEG C～90 DEG C, with continuously stirred 3～6 hours of the speed of 200RPM～400RPM,
In course of reaction, by-product carbinol is distilled out；
Step N3: reaction terminate after, reaction vessel is cooled to 25 DEG C of room temperatures, be sequentially added into toward reaction vessel in toluene with go from
Sub-water, toluene and deionized water volume ratio are 1～2: 1～2, will mix after shaking 60～120 seconds in liquid addition separatory funnel,
Stand to layering, discharge aqueous phase, retain organic facies；
Step N4: organic facies is washed 4 times with saturated sodium bicarbonate solution washing 1 time, deionization successively, organic facies is filtered also
Remove toluene by rotary evaporation, obtain hydride B.
The preparation method of a kind of LED encapsulation material the most according to claim 5, it is characterised in that: described 4-(phenoxy group benzene
Base) chemical structural formula of phenyidimethoxysilane is
9. the application of a LED encapsulation material, it is characterised in that: arbitrary for claim 1-3 described encapsulating material is added LED
In, heat 2～4 hours at 130 DEG C～150 DEG C so that it is be heating and curing formation cross linked polymer further, to complete LED
Encapsulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610290361.3A CN106046380A (en) | 2016-04-27 | 2016-04-27 | An LED encapsulating material, a preparing method thereof and application of the material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610290361.3A CN106046380A (en) | 2016-04-27 | 2016-04-27 | An LED encapsulating material, a preparing method thereof and application of the material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106046380A true CN106046380A (en) | 2016-10-26 |
Family
ID=57176708
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610290361.3A Pending CN106046380A (en) | 2016-04-27 | 2016-04-27 | An LED encapsulating material, a preparing method thereof and application of the material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106046380A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286899A (en) * | 2017-05-19 | 2017-10-24 | 合肥市惠科精密模具有限公司 | A kind of Micro LED screens are encapsulated with high-strength anti-aging silica gel |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319090A (en) * | 2006-12-01 | 2008-12-10 | 罗门哈斯公司 | Aryl(thio)ether aryl polysiloxane composition and methods for making and using same |
| US20090146324A1 (en) * | 2007-12-06 | 2009-06-11 | Rohm And Haas Company | Phenoxyphenyl polysiloxane composition and method for making and using same |
| CN102790141A (en) * | 2011-05-17 | 2012-11-21 | 罗门哈斯电子材料有限公司 | Method of making light emitting diodes |
-
2016
- 2016-04-27 CN CN201610290361.3A patent/CN106046380A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319090A (en) * | 2006-12-01 | 2008-12-10 | 罗门哈斯公司 | Aryl(thio)ether aryl polysiloxane composition and methods for making and using same |
| US20090146324A1 (en) * | 2007-12-06 | 2009-06-11 | Rohm And Haas Company | Phenoxyphenyl polysiloxane composition and method for making and using same |
| CN102790141A (en) * | 2011-05-17 | 2012-11-21 | 罗门哈斯电子材料有限公司 | Method of making light emitting diodes |
Non-Patent Citations (1)
| Title |
|---|
| DAVID W. MOSLEY ER AL.: "High refractive index thermally stable phenoxyphenyl and phenylthiophenyl silicones for light‐emitting diode applications", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286899A (en) * | 2017-05-19 | 2017-10-24 | 合肥市惠科精密模具有限公司 | A kind of Micro LED screens are encapsulated with high-strength anti-aging silica gel |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101509648B1 (en) | Nanocrystal doped matrixes | |
| CN105358615B (en) | Additive for organosilicon encapsulating material | |
| CN103012797B (en) | Preparation method of methyl phenyl vinyl silicone oil | |
| TWI547541B (en) | Transformative wavelength conversion medium | |
| KR20120035152A (en) | Functionalized matrixes for dispersion of nanostructures | |
| CN104487520B (en) | The condensation catalyst of curable organopolysiloxane composition, its manufacture method, the manufacture method of organopolysiloxane solidfied material, the method for condensing of organopolysiloxane, optical semiconductor sealing body and organopolysiloxane | |
| US8637627B2 (en) | Phenoxyphenyl polysiloxane composition and method for making and using same | |
| CN104151834B (en) | Hardening resin composition, its solidfied material and luminescent semiconductor device | |
| WO2004107458A2 (en) | Encapsulating composition for led | |
| TW200906886A (en) | Sealing agent for optical semiconductor element, and optical semiconductor element | |
| CN107057702B (en) | A kind of red fluorescence powder, preparation method and its made light emitting device | |
| CN104066794B (en) | Curable compositions | |
| CN105017773B (en) | LED package organopolysiloxane composition | |
| JP6086396B2 (en) | Curable composition and method for producing the same | |
| CN104733595B (en) | Variability wavelength-conversion media | |
| EP2784104B1 (en) | Production method of an organopolysiloxane | |
| Kang et al. | Enhancement of the optical properties of CsPbBr 3 perovskite nanocrystals using three different solvents | |
| CN106046380A (en) | An LED encapsulating material, a preparing method thereof and application of the material | |
| Yang et al. | Single 395 nm excitation warm WLED with a luminous efficiency of 104.86 lm/W and a color rendering index of 90.7 | |
| EP3101052B1 (en) | Cured product | |
| CN108336196A (en) | A kind of preparation method of UV LED chip | |
| Wang et al. | Tunable white light emission of an anti-ultraviolet rare-earth polysiloxane phosphors based on near UV chips | |
| CN106085344A (en) | Ultraviolet leds lamp bead encapsulation glue and preparation method thereof | |
| CN103588972A (en) | Phenyl vinyl silicone oil with high refractive index and high light transmittance and preparation method thereof | |
| CN104004362A (en) | Phenylene-phenylene ether organosilicon material for power type LED packaging and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161026 |
|
| RJ01 | Rejection of invention patent application after publication |