CN106543440A - Annular oligomeric silsesquioxanes, its modified organic silicon packaging plastic and preparation method thereof - Google Patents
Annular oligomeric silsesquioxanes, its modified organic silicon packaging plastic and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
The present invention relates to a kind of annular oligomeric silsesquioxanes, its modified organic silicon packaging plastic and preparation method thereof.The annular oligomeric silsesquioxanes of present invention synthesis（MOSS）（Component A）, synthesis terminal hydroxy ethylene polysiloxanes（Component B）, then A, B component is according to 1：The mass ratio mixing of (1 ~ 5), recycles chloroplatinic acid catalyst to carry out Si―H addition reaction solidification and prepares LED encapsulation MOSS modified organic silicon packaging plastics.Preparation process is simple of the present invention, synthetic yield are high；The packaging plastic has good heat stability and higher refractive index, and light transmission preferably, can solidify at a lower temperature.The MOSS modified organic silicons packaging plastic of preparation 500 nm wavelength light transmittance more than 90%, refractive index at a temperature of 25 DEG C is 1.535, thermal gravimetric analysis results show that the heat decomposition temperature of the packaging plastic is 416 DEG C, it is 57% in 700 DEG C of residual rates, show preferable heat resistance, the tensile strength and elongation at break of the packaging plastic is respectively 1.88 MPa and 157%, Shore A hardness 36.
Description
Technical field
The present invention relates to a kind of annular oligomeric silsesquioxanes, its modified organic silicon packaging plastic and preparation method thereof.
Background technology
Light emitting diode (Lighting-Emitting Diode, LED) is because have efficient, environmental protection, life-span length etc. excellent
Point, the application prospect in fields such as illumination, display, electronic equipment backlight, and decorations get most of the attention, and LED has become the whole world
The trend and trend of change.The fast development of LED technology, luminous efficiency are stepped up.With LED towards high brightness, high-weatherability,
The directions such as high uniformity of luminance, high reliability are developed, and it is also proposed higher performance to the macromolecular material for LED encapsulation will
Ask.The encapsulating material of great power LED must possess high index of refraction, high transmission rate, preferable heat resistance, sealing property and good
Good mechanical property and adhesive property.China encapsulates big country as LED, during the LED component encapsulation in the whole world 80% is all concentrated on
State.But China but lags far behind the major countries such as the U.S., Japan, power type LED encapsulation in the research of LED encapsulation material
Material market is captured by Japan and U.S.'s product completely so that our product cost is raised, and profit margin is little, more crucial
It is that development is seriously restricted.
The LED encapsulation material being widely used at present mainly has epoxy resin and organic siliconresin.Wherein, epoxy resin is present
The defect that crosslink density is excessive after solidification, toughness of material is poor, in addition, aging xanthochromia easily occurs in epoxy encapsulation glue asking
Topic, causes light transmittance and luminance-reduction, reduction of service life；Although traditional organic siliconresin packaging plastic refractive index and light transmittance
It is higher, but it is difficult to the defect for overcoming its mechanical property not enough.And add nanometer particle-modified organo-mineral complexing packaging plastic, though
Can so have at a relatively high refractive index, while can also improve the heat-resisting and mechanical performance of packaging plastic, but encapsulating material can be affected
The transparency, cause light output efficiency to decline.
The content of the invention
In order to solve problems of the prior art, an object of the present invention is to provide a kind of New Ring-like Type oligomerisation
Silsesquioxane (MOSS).
The second object of the present invention is organic silica gel to be modified by annular oligomeric silsesquioxanes (MOSS), system
A kind of new MOSS modified organic silicon packaging plastics were obtained, the refractive index of the packaging plastic is up to 1.535, and light transmittance is more than 90%,
Heat decomposition temperature is 415 DEG C, and elongation at break is 160%, and solidification temperature is low, packaging plastic and commercially available phase obtained in the present invention
Close product and compare and have the advantages that high folding, heat-resisting, preferable mechanical property and solidification temperature are low.
The third object of the present invention is the preparation method for providing the packaging plastic.
For achieving the above object, the present invention adopts following mechanism：
A. the synthetic method of annular oligomeric silsesquioxanes (MOSS)：The method referred to as metal inducement is self-assembled into around-France.
It is characterized in that the polysiloxanes complexation of the hydrolyzed trialkoxysilanes generation metal ion under transition metal and alkali metal induction
Then the complex and a chlorosilane are reacted, are peeled off in complex by the metal of thing --- three-dimensional oligomerisation-polysiloxanes complex
Metal ion, finally give MOSS.It is PhSi (OR) first in course of reaction3, NaOH, water, alcohol cohydrolysis have obtained saddle
The crystalline complex of shape.The crystalline complex outer layer is phenyl ring-type silicone layer, their negative charge by internal layer copper from
Son and sodium ion neutralization, also contain alcohol and water molecule in crystalline complex.Crystal is reacted with chlorosilane, by copper ion and sodium ion
Peel off and generate CuCl2And NaCl, while generating MOSS.
B. the synthetic method of terminal hydroxy ethylene polysiloxanes：The synthetic method is characterized in that selection potassium hydroxide as anti-
The catalyst answered, from toluene as reaction dissolvent, octamethylcy-clotetrasiloxane D4Enter with methylvinyldimethoxysilane
Row open loop condensation reaction, prepares terminal hydroxy ethylene polysiloxanes.
The curing of c.MOSS modified organic silicon packaging plastics：The method is by silicon hydrogen component annular oligomeric silsesquioxanes
Si―H addition reaction curing reaction between MOSS and vinyl component terminal hydroxy ethylene polysiloxanes, prepares MOSS modified organic silicons
Packaging plastic.
According to above-mentioned reaction mechanism, the present invention is adopted the following technical scheme that：
A kind of annular oligomeric silsesquioxanes, it is characterised in that the structural formula of annular oligomeric silsesquioxanes MOSS is：
A kind of LED encapsulation MOSS modified organic silicon packaging plastics, the packaging plastic is double-component, it is characterised in that described group
A is divided to adopt above-mentioned annular oligomeric silsesquioxanes MOSS, component B is terminal hydroxy ethylene polysiloxanes, during use, by component
A and component B are according to 1:The mass ratio of (1～5) is sufficiently mixed uniformly, and adds chloroplatinic acid catalyst, and its addition is mixed for reaction
The 0.1%～0.3% of compound gross mass, after excluding bubble, solidifies 1～2h at a temperature of 60 DEG C～80 DEG C, or in room temperature
48～72h of lower solidification, can obtain the LED encapsulation MOSS modified organic silicon packaging plastics for solidifying.
The structural formula of above-mentioned component B terminal hydroxy ethylene polysiloxanes is：
Wherein x：Y is 1:1～1:2.
A kind of method for preparing above-mentioned LED encapsulation MOSS modified organic silicon packaging plastics, its levy be the method tool
Body step is as follows：
A. sodium hydrate solid is dissolved in the mixed solvent of n-butyl alcohol and deionized water, heating for dissolving, add with
Sodium hydroxide mass ratio is 2:1～6:1 trimethoxy-benzene base silane, at 100 DEG C～130 DEG C, is heated to reflux 20～60min；
Then will be 1 with sodium hydroxide mass ratio:1～2:1 Copper dichloride dihydrate is dissolved in n-butyl alcohol, by the Copper dichloride dihydrate
Butanol solution is added drop-wise in above-mentioned reaction system, after being added dropwise to complete, and continues 30～60min of backflow.After reaction terminates, will be anti-
Answer solution filtered while hot, concentrating filter liquor, stand still for crystals, filter, obtain blue colored crystal, obtain ten hexichol basic rings, 12 silanol
Copper/sodium complex crystal；
B. by ten hexichol basic ring obtained by step a, 12 silanol copper/sodium complex crystal and pyridine according to mass ratio 1:1～4:
1 is dissolved in normal hexane, and 30～60min of reaction is stirred at room temperature；Then the hexane solution of dimethylchlorosilane is slowly added dropwise, it is described
The mass ratio of ten hexichol basic rings, 12 silanol copper/sodium complex crystal and dimethylchlorosilane be 1:1～3:1, it is stirred at room temperature
After 20～60min, 1.5～3h of back flow reaction, after reaction terminates, is cooled to room temperature, filters, and is washed with deionized, anhydrous
Magnesium sulfate is dried, and removes solvent, obtains colourless viscous liquid and is annular oligomeric silsesquioxanes；
C. by octamethylcy-clotetrasiloxane and methylvinyldimethoxysilane according to 2:1～5:1 mass ratio is dissolved in
In toluene, and add the potassium hydroxide of catalytic amount as the catalyst of reaction, stirring 3～6h of lower back flow reaction, add from
Sub- water, continues to be heated to reflux 1～3h, after reaction terminates, is cooled to room temperature, and it is 7 that deionized water is washed till pH, then micro- with 0.45
The membrane filtration in metre hole footpath, removes solvent, obtains colorless transparent viscous liquid and is terminal hydroxy ethylene polysiloxanes；
During use, by component A and component B according to 1:The mass ratio of (1～5) is sufficiently mixed uniformly, and adds chloroplatinic acid to urge
Agent, its addition for reactant mixture gross mass 0.1%～0.3%, after excluding bubble, at a temperature of 60 DEG C～80 DEG C
1～2h of solidification, or solidify 48～72h at room temperature, the LED encapsulation MOSS modified organic silicons encapsulation for solidifying can be obtained
Glue.
The cubic cage and the higher bond energy of siliconoxygen bond of the annular oligomeric silsesquioxanes of the present invention so that ring itself
The addition that shape oligomeric silsesquioxanes have excellent heat resistance, annular oligomeric silsesquioxanes causes packaging plastic to have very well
Heat stability；At the same time, the phenyl ring with higher Lorentz-Lorenz molar refraction is introduced in annular oligomeric silsesquioxanes so that
Annular oligomeric silsesquioxanes modified organic silicon packaging plastic has higher refractive index, 500nm wavelength light transmittance 90%
More than, the refractive index at a temperature of 25 DEG C is 1.535, and thermal gravimetric analysis results show that the heat decomposition temperature of the packaging plastic is 416 DEG C,
It is 57% in 700 DEG C of residual rates, shows preferable heat resistance, the tensile strength of the packaging plastic and elongation at break difference
For 1.88MPa and 157%, Shore A hardness 36.The inventive method preparation process is simple, synthetic yield are high simultaneously.
Specific embodiment
After now be specified in the specific embodiment of the present invention.
Embodiment one：
1) synthesis of ten hexichol basic rings, 12 silanol copper/sodium complex crystal
Appropriate sodium hydrate solid is weighed first, the heating for dissolving in n-butanol solvent and a small amount of deionized water.To
It is 2 wherein to add with sodium hydroxide mass ratio:Reaction temperature is increased to 100 DEG C, is heated back by 1 trimethoxy-benzene base silane
Stream 60min.Then according to sodium hydroxide mass ratio 1:1 proportioning weighs Copper dichloride dihydrate, and is dissolved in appropriate
In n-butyl alcohol, it is slowly added in above-mentioned reaction system.After being added dropwise to complete, continue backflow 30min.After backflow terminates, will be anti-
Answer solution sucking filtration while hot.After by filtrate, vacuum distillation goes out the n-butanol solvent of half volume at a temperature of 70 DEG C, it is stored in relatively low
At a temperature of stand still for crystals.Finally filter, obtain blue colored crystal, the blue colored crystal is dried to constant weight in 80 DEG C of baking ovens, is obtained
To ten hexichol basic rings, 12 silanol copper/sodium complex crystal.
2) synthesis of component A annular oligomeric silsesquioxanes (MOSS)
By 12 silanol copper of obtained ten hexichol basic ring/sodium complex crystal with pyridine according to mass ratio 1:1 is mixed,
Appropriate normal hexane is being added thereto to as reaction dissolvent, 30min after mixing, is being stirred at room temperature.Then according to ten diphenyl
12 silanol copper of ring/sodium complex crystal mass compares 1:1 weighs dimethylchlorosilane, and is made in being dissolved in normal hexane molten
Liquid, and be slowly added in above-mentioned reaction system, after 30min is stirred at room temperature, temperature is increased to into 70 DEG C of 1.5～3h of backflow.
After backflow terminates, room temperature is cooled to, filters, and be washed with deionized three times and remove inorganic ionss therein, add suitable
The anhydrous magnesium sulfate of amount is dried, and vacuum distillation after filtration removes solvent, obtains colourless viscous liquid and is annular oligomerisation sesquialter silicon
Oxygen alkane MOSS.
3) synthesis of component B terminal hydroxy ethylene polysiloxanes
Octamethylcy-clotetrasiloxane (D is weighed respectively4) and methylvinyldimethoxysilane (VDMMS), according to quality
Than 2:1 mixing, and add a small amount of potassium hydroxide as the catalyst of reaction, add appropriate toluene and do reaction dissolvent.Room
After warm mix homogeneously, reaction temperature is increased to into 100 DEG C of heated and stirred 4～6h of backflow, appropriate deionized water is added, is continued
It is heated to reflux 2h.After reaction terminates, treat that solution is cooled down, it is 7 that deionized water is washed till pH, then with poly- the four of 0.45 micron pore size
Fluoride film is filtered, then filtrate decompression distillation is removed after solvent and water, is obtained colorless transparent viscous liquid and is terminal hydroxy group
Vinyl polysiloxane.
4) solidification of MOSS modified organic silicons packaging plastic
By component A annular oligomeric silsesquioxanes MOSS and component B terminal hydroxy ethylene polysiloxanes of synthesis according to matter
Amount compares 1:4 are sufficiently mixed and stir, and are subsequently adding a small amount of chloroplatinic acid catalyst and are mixed with, and the addition of catalyst is
The 0.1%～0.3% of mixture gross mass.Decompression excludes bubble, after excluding bubble, at a temperature of 60～80 DEG C solidification 1～
2h, or solidify 48～72h at room temperature.The LED encapsulation MOSS modified organic silicon packaging plastics for solidifying can be obtained.
The MOSS modified organic silicons packaging plastic that the present embodiment is prepared is 90% in the light transmittance of visible light wave range, 25
Refractive index at a temperature of DEG C is 1.516, and thermal gravimetric analysis results show that the heat decomposition temperature of the packaging plastic is 408 DEG C, at 700 DEG C
Residual rate is 53%, shows preferable heat resistance, and the tensile strength and elongation at break of the packaging plastic are respectively 1.87MPa
With 162%, Shore A hardness 32.
Embodiment two：
1) synthesis of ten hexichol basic rings, 12 silanol copper/sodium complex crystal
Appropriate sodium hydrate solid is weighed first, the heating for dissolving in n-butanol solvent and a small amount of deionized water.To
It is 4 wherein to add with sodium hydroxide mass ratio:Reaction temperature is increased to 110 DEG C, is heated back by 1 trimethoxy-benzene base silane
Stream 40min.Then according to sodium hydroxide mass ratio 3:2 proportioning weighs Copper dichloride dihydrate, and is dissolved in appropriate
In n-butyl alcohol, it is slowly added in above-mentioned reaction system.After being added dropwise to complete, continue backflow 40min.After backflow terminates, will be anti-
Answer solution sucking filtration while hot.After by filtrate, vacuum distillation goes out the n-butanol solvent of half volume at a temperature of 80 DEG C, it is stored in relatively low
At a temperature of stand still for crystals.Finally filter, obtain blue colored crystal, the blue colored crystal is dried to constant weight in 90 DEG C of baking ovens, is obtained
To ten hexichol basic rings, 12 silanol copper/sodium complex crystal.
2) synthesis of component A annular oligomeric silsesquioxanes (MOSS)
By 12 silanol copper of obtained ten hexichol basic ring/sodium complex crystal with pyridine according to mass ratio 2:1 is mixed,
Appropriate normal hexane is being added thereto to as reaction dissolvent, 40min after mixing, is being stirred at room temperature.Then according to ten diphenyl
12 silanol copper of ring/sodium complex crystal mass compares 2:1 weighs dimethylchlorosilane, and is made in being dissolved in normal hexane molten
Liquid, and be slowly added in above-mentioned reaction system, after 40min is stirred at room temperature, temperature is increased to into 80 DEG C of 1.5～3h of backflow.
After backflow terminates, room temperature is cooled to, filters, and be washed with deionized three times and remove inorganic ionss therein, add suitable
The anhydrous magnesium sulfate of amount is dried, and vacuum distillation after filtration removes solvent, obtains colourless viscous liquid and is annular oligomerisation sesquialter silicon
Oxygen alkane MOSS.
3) synthesis of component B terminal hydroxy ethylene polysiloxanes
Octamethylcy-clotetrasiloxane (D4) and methylvinyldimethoxysilane (VDMMS) are weighed respectively, according to quality
Than 3:1 mixing, and add a small amount of potassium hydroxide as the catalyst of reaction, add appropriate toluene and do reaction dissolvent.Room
After warm mix homogeneously, reaction temperature is increased to into 115 DEG C of heated and stirred 3～5h of backflow, appropriate deionized water is added, is continued
It is heated to reflux 2h.After reaction terminates, treat that solution is cooled down, it is 7 that deionized water is washed till pH, then with poly- the four of 0.45 micron pore size
Fluoride film is filtered, then filtrate decompression distillation is removed after solvent and water, is obtained colorless transparent viscous liquid and is terminal hydroxy group
Vinyl polysiloxane.
4) solidification of MOSS modified organic silicons packaging plastic
By component A annular oligomeric silsesquioxanes MOSS and component B terminal hydroxy ethylene polysiloxanes of synthesis according to matter
Amount compares 1:3 are sufficiently mixed and stir, and are subsequently adding a small amount of chloroplatinic acid catalyst and are mixed with, and the addition of catalyst is
The 0.1%～0.3% of mixture gross mass.Decompression excludes bubble, after excluding bubble, at a temperature of 60～80 DEG C solidification 1～
2h, or solidify 48～72h at room temperature.The LED encapsulation MOSS modified organic silicon packaging plastics for solidifying can be obtained.
The MOSS modified organic silicons packaging plastic that the present embodiment is prepared is 90% in the light transmittance of visible light wave range, 25
Refractive index at a temperature of DEG C is 1.527, and thermal gravimetric analysis results show that the heat decomposition temperature of the packaging plastic is 415 DEG C, at 700 DEG C
Residual rate is 56%, shows preferable heat resistance, and the tensile strength and elongation at break of the packaging plastic are respectively 1.90MPa
With 159%, Shore A hardness 34.
Embodiment three：
1) synthesis of ten hexichol basic rings, 12 silanol copper/sodium complex crystal
Appropriate sodium hydrate solid is weighed first, the heating for dissolving in n-butanol solvent and a small amount of deionized water.To
It is 6 wherein to add with sodium hydroxide mass ratio:Reaction temperature is increased to 130 DEG C, is heated back by 1 trimethoxy-benzene base silane
Stream 30min.Then according to sodium hydroxide mass ratio 2:1 proportioning weighs Copper dichloride dihydrate, and is dissolved in appropriate
In n-butyl alcohol, it is slowly added in above-mentioned reaction system.After being added dropwise to complete, continue backflow 40min.After backflow terminates, will be anti-
Answer solution sucking filtration while hot.After by filtrate, vacuum distillation goes out the n-butanol solvent of half volume at a temperature of 80 DEG C, it is stored in relatively low
At a temperature of stand still for crystals.Finally filter, obtain blue colored crystal, the blue colored crystal is dried to constant weight in 90 DEG C of baking ovens, is obtained
To ten hexichol basic rings, 12 silanol copper/sodium complex crystal.
2) synthesis of component A annular oligomeric silsesquioxanes (MOSS)
By 12 silanol copper of obtained ten hexichol basic ring/sodium complex crystal with pyridine according to mass ratio 3:1 is mixed,
Appropriate normal hexane is being added thereto to as reaction dissolvent, 40min after mixing, is being stirred at room temperature.Then according to ten diphenyl
12 silanol copper of ring/sodium complex crystal mass compares 3:1 weighs dimethylchlorosilane, and is made in being dissolved in normal hexane molten
Liquid, and be slowly added in above-mentioned reaction system, after 40min is stirred at room temperature, temperature is increased to into 90 DEG C of 1.5～3h of backflow.
After backflow terminates, room temperature is cooled to, filters, and be washed with deionized three times and remove inorganic ionss therein, add suitable
The anhydrous magnesium sulfate of amount is dried, and vacuum distillation after filtration removes solvent, obtains colourless viscous liquid and is annular oligomerisation sesquialter silicon
Oxygen alkane MOSS.
3) synthesis of component B terminal hydroxy ethylene polysiloxanes
Octamethylcy-clotetrasiloxane (D4) and methylvinyldimethoxysilane (VDMMS) are weighed respectively, according to quality
Than 5:1 mixing, and add a small amount of potassium hydroxide as the catalyst of reaction, add appropriate toluene and do reaction dissolvent.Room
After warm mix homogeneously, reaction temperature is increased to into 130 DEG C of heated and stirred 3～5h of backflow, appropriate deionized water is added, is continued
It is heated to reflux 2h.After reaction terminates, treat that solution is cooled down, it is 7 that deionized water is washed till pH, then with poly- the four of 0.45 micron pore size
Fluoride film is filtered, then filtrate decompression distillation is removed after solvent and water, is obtained colorless transparent viscous liquid and is terminal hydroxy group
Vinyl polysiloxane.
4) solidification of MOSS modified organic silicons packaging plastic
By component A annular oligomeric silsesquioxanes MOSS and component B terminal hydroxy ethylene polysiloxanes of synthesis according to matter
Amount compares 1:2 are sufficiently mixed and stir, and are subsequently adding a small amount of chloroplatinic acid catalyst and are mixed with, and the addition of catalyst is
The 0.1%～0.3% of mixture gross mass.Decompression excludes bubble, after excluding bubble, at a temperature of 60～80 DEG C solidification 1～
2h, or solidify 48～72h at room temperature.The LED encapsulation MOSS modified organic silicon packaging plastics for solidifying can be obtained.
The MOSS modified organic silicons packaging plastic that the present embodiment is prepared is 90% in the light transmittance of visible light wave range, 25
Refractive index at a temperature of DEG C is 1.535, and thermal gravimetric analysis results show that the heat decomposition temperature of the packaging plastic is 416 DEG C, at 700 DEG C
Residual rate is 57%, shows preferable heat resistance, and the tensile strength and elongation at break of the packaging plastic are respectively 1.88MPa
With 157%, Shore A hardness 36.
Claims (4)
1. a kind of annular oligomeric silsesquioxanes, it is characterised in that the structural formula of annular oligomeric silsesquioxanes MOSS is：
2. a kind of LED is encapsulated and is used MOSS modified organic silicon packaging plastics, and the packaging plastic is double-component, it is characterised in that described component
A adopts annular oligomeric silsesquioxanes MOSS according to claim 1, and component B is terminal hydroxy ethylene polysiloxanes, is made
Used time, by component A and component B according to 1:The mass ratio of (1～5) is sufficiently mixed uniformly, and adds chloroplatinic acid catalyst, its addition
0.1%～0.3% for reactant mixture gross mass is measured, after excluding bubble, solidifies 1～2h at a temperature of 60 DEG C～80 DEG C,
Or solidify 48～72h at room temperature, the LED encapsulation MOSS modified organic silicon packaging plastics for solidifying can be obtained.
3. LED according to claim 2 is encapsulated with MOSS modified organic silicon packaging plastics, it is characterised in that described component B
The structural formula of terminal hydroxy ethylene polysiloxanes is：
Wherein x：Y is 1:1～1:2.
4. a kind of method of the LED encapsulation MOSS modified organic silicon packaging plastics prepared described in Claims 2 or 3, which is levied and is
The method is comprised the following steps that：
A. sodium hydrate solid is dissolved in the mixed solvent of n-butyl alcohol and deionized water, heating for dissolving is added and hydrogen-oxygen
It is 2 to change sodium mass ratio:1～6:1 trimethoxy-benzene base silane, at 100 DEG C～130 DEG C, is heated to reflux 20～60min；Then
To be 1 with sodium hydroxide mass ratio:1～2:1 Copper dichloride dihydrate is dissolved in n-butyl alcohol, by the positive fourth of the Copper dichloride dihydrate
Alcoholic solution is added drop-wise in above-mentioned reaction system, after being added dropwise to complete, and continues 30～60min of backflow.After reaction terminates, will react molten
Liquid filtered while hot, concentrating filter liquor, stands still for crystals, filters, and obtains blue colored crystal, obtains ten hexichol basic rings, 12 silanol copper/sodium
Complex Crystal；
B. by ten hexichol basic ring obtained by step a, 12 silanol copper/sodium complex crystal and pyridine according to mass ratio 1:1～4:1 is molten
In normal hexane, 30～60min of reaction is stirred at room temperature；Then the hexane solution of dimethylchlorosilane is slowly added dropwise, it is described
Ten hexichol basic rings, 12 silanol copper/sodium complex crystal is 1 with the mass ratio of dimethylchlorosilane:1～3:1, it is stirred at room temperature 20
After～60min, 1.5～3h of back flow reaction, after reaction terminates, is cooled to room temperature, filters, and is washed with deionized, anhydrous sulfur
Sour magnesium is dried, and removes solvent, obtains colourless viscous liquid and is annular oligomeric silsesquioxanes；
C. by octamethylcy-clotetrasiloxane and methylvinyldimethoxysilane according to 2:1～5:1 mass ratio is dissolved in toluene
In, and the potassium hydroxide of catalytic amount is added as the catalyst of reaction, the lower 3～6h of back flow reaction of stirring adds deionized water,
Continue to be heated to reflux 1～3h, after reaction terminates, be cooled to room temperature, it is 7 that deionized water is washed till pH, then uses 0.45 micron openings
The membrane filtration in footpath, removes solvent, obtains colorless transparent viscous liquid and is terminal hydroxy ethylene polysiloxanes；
During use, by component A and component B according to 1:The mass ratio of (1～5) is sufficiently mixed uniformly, and adds chloroplatinic acid catalyst,
Its addition for reactant mixture gross mass 0.1%～0.3%, after excluding bubble, solidifies 1 at a temperature of 60 DEG C～80 DEG C
～2h, or solidify 48～72h at room temperature, the LED encapsulation MOSS modified organic silicon packaging plastics for solidifying can be obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610927462.7A CN106543440B (en) | 2016-10-31 | 2016-10-31 | Annular oligomeric silsesquioxanes, its modified organic silicon packaging plastic and preparation method thereof |
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| CN102827477A (en) * | 2011-06-16 | 2012-12-19 | 日东电工株式会社 | Silicone resin composition, encapsulating layer, reflector, and optical semiconductor device |
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| CN110194946A (en) * | 2019-05-16 | 2019-09-03 | 上海大学 | Organic silicon packaging glue and preparation method thereof |
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