CN103627178B - A kind of LED encapsulation liquid silicon rubber composition and preparation method thereof - Google Patents
A kind of LED encapsulation liquid silicon rubber composition and preparation method thereof Download PDFInfo
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- CN103627178B CN103627178B CN201310624813.3A CN201310624813A CN103627178B CN 103627178 B CN103627178 B CN 103627178B CN 201310624813 A CN201310624813 A CN 201310624813A CN 103627178 B CN103627178 B CN 103627178B
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Abstract
The present invention relates to a kind of LED encapsulation liquid silicon rubber composition and preparation method thereof.A kind of LED encapsulation liquid silicon rubber composition, component is as follows, is weight portion: the organopolysiloxane 60 containing aliphatic unsaturated bond～120 parts, organic hydrogen polysiloxanes part 2～45 parts, features based polysiloxane 5～30 parts, platinum complex catalyst 0.01～0.5 part, inhibitor 0.01～0.05 part, viscosifier 0.5～3 parts.The invention still further relates to the preparation method of this LED encapsulation liquid silicon rubber composition.The present invention with the addition of features based polysiloxane in liquid silicon rubber composition, it serves the effect of high strength reinforcement, substantially increase the mechanical mechanics properties such as the hot strength of product, tearing strength, elongation at break, and product has good caking property, light transmittance >=99%.
Description
Technical field
The present invention relates to a kind of LED encapsulation liquid silicon rubber composition and preparation method thereof, belong to liquid silastic technology of preparing
Field.
Background technology
Light emitting diode (Light Emitting Diode is called for short LED), has efficiency high, and light colour purity, energy consumption is little, the longevity
The advantages such as life is long, and response is fast, pollution-free, all solid state, are a kind of novel illumination light sources, " solid-state illumination " of green of being known as.
Along with the development of LED technology is with ripe, the light efficiency of white light LEDs has met or exceeded the light efficiency level of ordinary incandescent lamp,
Luminous flux is also being significantly increased, and this makes LED be expected to become after electric filament lamp, fluorescent lamp, high-intensity gas discharge lamp
Four generation lighting sources.
Common LED encapsulation material mainly includes epoxy resin, Merlon, polymethyl methacrylate, thermoset epoxy
Resin and optics nylon etc., along with increasing and the raising of brightness of LED power, these materials are bad because of thermostability, are easily generated Huang
Become, cause light decay, it is impossible to meet the performance requirement of power type LED chip, accordingly, it would be desirable to seek new substitution material.Organic
Silicon materials have the advantages such as cold-hot impact, color inhibition, water white transparency, low stress, are the optimal materials of LED encapsulation.
When usual silicone rubber is without reinforcement, intensity is relatively low, does not substantially have serviceability.Gas-phase silica is used to carry out reinforcement, by
Relatively big with the refractive index of organosilicon material in gas-phase silica, the light transmittance of LED encapsulation material can be reduced, and with gas phase
The increase of white carbon consumption, compound viscosity is increased dramatically, and causes operating difficulties, affects gluing process.Only mend with MQ silicones
Qiang Shi, although the hot strength of silicone rubber can be made to make moderate progress, but for tearing strength and the raising of elongation at break, have one
Settle finally sex-limited, it is impossible to the LED encapsulation that satisfied requirement is higher.
Chinese patent literature CN102344684A(application number 201110233591.3) introduce diisocyanate modification, end
Vinyl silicone oil for hydroxyl is prepared for LED module packaging organic silicon rubber, improves the tear resistance of silicone rubber, but for drawing
The raising stretching intensity and elongation at break is inconspicuous.
Chinese patent literature CN103146202A(application number 201310087259.X) introduce the poly-silica of end-vinyl ultra-branching
Alkane, is applied in LED package liquid silastic, is improved for mechanical property, but still can not meet
The LED encapsulation of requirements at the higher level.
Chinese patent literature CN102181159A(application number 201110061714.X) POSS is applied in LED encapsulation material,
Owing to preparation POSS not only needs to use solvent, and complex process, relatively costly.
It addition, add the LED rubber composition of viscosifier, there is caking property in various degree with a lot of materials, therefore, make
When preparing test specimens with metal die or glass mold sulfuration, often allow LED silica gel be difficult to the demoulding, can not get complete silicon rubber
Glue test sheet, need add releasing agent or on mould plastic film mulch.Adding releasing agent and can make silastic surface dust easy to stick, impact is thoroughly
Light rate, plastic film mulch easily shifts, and causes LED silica gel piece surface ditch ditch bank, out-of-flatness, the standard of the data that affect the mechanical properties occur
Really property.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that a kind of LED encapsulation liquid silicon rubber composition and preparation method thereof.
Summary of the invention
A kind of LED encapsulation liquid silicon rubber composition that the present invention provides and preparation method thereof, is at liquid silicon rubber composition
In with the addition of be readily available, lower-cost features based polysiloxane high strength reinforcement component, obtain hot strength, tear
The liquid silastic product that the mechanical mechanics property such as intensity, elongation at break is greatly improved, uses politef mould simultaneously
Tool preparation test specimens.
Detailed Description Of The Invention
A kind of LED encapsulation liquid silicon rubber composition, component is as follows, is weight portion:
Organopolysiloxane (A) 60～120 parts containing aliphatic unsaturated bond, organic hydrogen polysiloxanes (B) part 2～45
Part, features based polysiloxane (C) 5～30 parts, platinum complex catalyst (D) 0.01～0.5 part, inhibitor (E)
0.01～0.05 part, viscosifier (F) 0.5～3 part；
The described organopolysiloxane (A) containing aliphatic unsaturated bond is that the straight chain containing 2 alkenyl groups above in molecule has
Machine polysiloxanes (A-1) and/or molecule contain the organopolysiloxane (A-2) of the resin structure of 2 alkenyl groups above；
Described organic hydrogen polysiloxanes (B) is the straight chain organic hydrogen polysiloxanes (B-1) in molecule containing more than 2 H atom
And/or molecule contains the organic hydrogen polysiloxanes (B-2) of the resin structure of more than 2 H atom；
Described features based polysiloxane (C), for containing the polysiloxanes (C-1) of many vinylcyclosiloxanes base in molecule
And/or hydroxy vinyl based polysiloxane (C-2)；
The formula of the polysiloxanes containing many vinylcyclosiloxanes base in molecule is as follows:
In formula: R1For the cyclosiloxane base containing many vinyls, wherein k1=2,3 or 4, k2=2,3 or 4, k3=2,3 or
4, R1It is positioned at the end of strand and/or the sidepiece of strand；R2、R2' it is methyl, ethyl, propyl group and/or phenyl；Link
Number a=10～1000, b=0～1000, c=5～1000, viscosity is 1000-20000mPa.s；
The formula of hydroxy vinyl based polysiloxane is as follows:
Wherein Me represents methyl；Link number s=0～1000, t=1～100, q=1～1000；Viscosity is 10～10000mPa.s；
Described platinum complex catalyst (D) is platinum water or Ka Shi platinum catalyst；
Described inhibitor (E) is alkynol class inhibitor, and viscosifier (F) are methyl silicone rubber viscosifier or phenyl siloxane rubber thickening
Agent.
According to currently preferred, LED encapsulation liquid silicon rubber composition, component is as follows, is weight portion:
Organopolysiloxane (A) 80～100 parts containing aliphatic unsaturated bond, organic hydrogen polysiloxanes (B) 7～30 parts,
Features based polysiloxane (C) 5～15 parts, platinum complex catalyst (D) 0.015～0.03 part, inhibitor (E) 0.015～
0.02 part, viscosifier (F) 1～2 part.
According to currently preferred, in described molecule, the straight chain organopolysiloxane (A-1) containing 2 alkenyl groups above is selected from
Vinyl silicone oil and/or phenyl-vinyl silicon oil, viscosity is 3000～15000mPa.s；Containing 2 with cochain in described molecule
The organopolysiloxane (A-2) of the resin structure of thiazolinyl is selected from vinyl polysiloxane and/or phenyl vinyl polysiloxane, and viscosity is
5000～20000mPas；
According to currently preferred, in described molecule, the straight chain organic hydrogen polysiloxanes (B-1) containing more than 2 H atom selects
From containing hydrogen silicone oil and/or phenyl hydrogen-containing silicon oil, viscosity is 20～100mPas；Containing more than 2 H atom in described molecule
The organic hydrogen polysiloxanes (B-2) of resin structure selected from the viscosity of Silicon Containing Hydrogen resin and/or phenyl Silicon Containing Hydrogen resin be 20～
1500mPas。
According to currently preferred, described R1For many vinyl three cyclosiloxane bases, many vinyls Fourth Ring siloxy group, many ethylene
One or more in the siloxy group of base five rings are with the combination of any ratio；It is further preferred that R1For many vinyl three ring silicon
One or more of oxyalkyl, many vinyls Fourth Ring siloxy group are with the combination of any ratio；
According to currently preferred, described R1The link number a=10～100 of the polysiloxanes containing many vinylcyclosiloxanes base,
B=50～500, c=10～500；
According to currently preferred, the platinum content of described platinum complex catalyst (D) is 3000～10000ppm.
According to currently preferred, the value of link number t and s of described hydroxy vinyl based polysiloxane is s=0～200, t
=20～50, q=30～200；
According to currently preferred, in described LED encapsulation liquid silicon rubber composition, the mol ratio of Si-Vi:Si-H is 1:
(1～1.8), wherein Si-Vi represents silico ethylene base, Si-H represents silicon hydrogen-based, it is further preferred that Si-Vi:Si-H's rubs
That ratio is 1:(1.1～1.5).
According to currently preferred, described inhibitor be propilolic alcohol, 1-acetenyl-1-Hexalin, 2-phenyl-3-crotonylene-
Alcohol, methyl butynol.
According to currently preferred, the polysiloxanes (C-1) of described many vinylcyclosiloxanes base can use this area conventional
Method synthesizes, it is possible to adopts and prepares with the following method:
(1) after respectively dimethicone and methyl phenyl ring siloxane being removed moisture, 90:(0 in mass ratio～1)
Or 1:(18.5～37) mixing, then press dimethicone and the 0.08 of methyl phenyl ring siloxane gross mass～0.1
Ratio adds the concentrated sulphuric acid of mass concentration 98% of the hydrogeneous ring body being dried, hydrogeneous double-seal head and gross weight 0.5～1.5%,
Polyreaction 3～5h at 30～50 DEG C, add in sodium bicarbonate and pH is to neutral, filter, de-low, obtain hydrogeneous poly-silica
Alkane；
(2) in the hydrogen containing siloxane that step (1) prepares, add the tetravinyl tetramethyl-ring siloxanes of more than 5 times of quality,
Adding platinum catalyst, the concentration making platinum catalyst is 15～25ppm, reacts 4～6h, rise under conditions of 80～100 DEG C
Temperature, to 140～150 DEG C of vacuum removal low molecule, obtains the polysiloxanes (C-1) of many vinylcyclosiloxanes base；
It is further preferred that described hydrogeneous ring body is selected from methylhydracyclosiloxane；Described hydrogeneous double-seal head is selected from tetramethyl two
Hydrogen-based disiloxane.
According to currently preferred, described hydroxy vinyl based polysiloxane (C-2) can use this area conventional method synthesis,
May be used without following method to prepare:
Dimethicone, methyl phenyl ring siloxane and methylvinylcyclosiloxane are removed water at 35～40 DEG C respectively
Point, then by the mass ratio of dimethicone, methyl phenyl ring siloxane and methylvinylcyclosiloxane be 10:(0～
0.005): (1～1.2) or 1:(18.4～37.5): (0.1～0.12) mixes, alkali glue is added, at 90～100 DEG C
Under the conditions of polyase 13～5h, add 0.18～0.20g water, be warming up to 140～160 DEG C, decomposition catalyst 3～5h, then warp
Vacuum takes off low molecule, obtains hydroxy vinyl based polysiloxane (C-2)；
It is further preferred that described alkali glue is selected from the silicon alkoxide of Tetramethylammonium hydroxide.
The preparation method of a kind of above-mentioned LED encapsulation liquid silicon rubber composition, comprises the steps:
By the organopolysiloxane (A) containing aliphatic unsaturated bond, organic hydrogen polysiloxanes (B) and the poly-silicon of features base
After oxygen alkane (C) is mixed in proportion, adds platinum complex catalyst, inhibitor, viscosifier, mix homogeneously, prepare LED
Encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 5～30min, it is placed in poly-four
In fluorothene mould；Through vulcanizing 0.5～1.5h at 50～80 DEG C, then 100～200 DEG C of sulfurations 0.5～4h, or, warp
Vulcanize 2h at 100～200 DEG C, obtain test specimens.
Beneficial effect
1, the present invention with the addition of features based polysiloxane in liquid silicon rubber composition, and it serves high strength reinforcement
Effect, substantially increases the mechanical mechanics properties such as the hot strength of product, tearing strength, elongation at break, and product has very
Good caking property, light transmittance >=99%；
2, the features based polysiloxane that the present invention adds in liquid silicon rubber composition, is readily available, and cost is relatively low；
3, preparation method of the present invention uses Teflon mould to prepare test specimens, and the demoulding is easy, and preparation process is simple,
Product surface cleans；
4, the liquid silicon rubber composition that the present invention prepares, is very suitable for the embedding of LED, paster type encapsulation, it is also possible to should
For fields such as optical lens, solar cell substrate, touch screens.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is further elaborated, but institute of the present invention protection domain is not limited to this.
Raw material explanation
Described embodiment 1～4 and the polysiloxanes (C-1) of many vinylcyclosiloxanes base of comparative example 3 adopt and make with the following method
Standby:
After dimethicone is removed moisture, in the there-necked flask that 500mL is clean, add dimethicone 370g,
Add hydrogeneous ring body (methylhydracyclosiloxane), the hydrogeneous double-seal head of 1.34g (tetramethyl two hydrogen-based two silica that 30g is dried
Alkane) and the concentrated sulphuric acid of 4g mass concentration 98%, at 40 DEG C, it is polymerized 4h, adds in 12g sodium bicarbonate and pH is to neutral,
Filter, de-low, obtain 360g hydrogen containing siloxane；By 360g hydrogen containing siloxane, 1720g tetravinyl tetramethyl-ring
Siloxanes and 0.04g platinum catalyst add in 3000mL, react 6h at 90 DEG C, are warming up to 150 DEG C of vacuum removal low molecule,
Obtain the polymethyl siloxane (C-1) of 640g vinylcyclosiloxanes base；Viscosity is 5200mPa.s；
The polysiloxanes (C-1) of many vinylcyclosiloxanes base of described embodiment 5～6 is adopted and is prepared with the following method:
Respectively by after dimethicone, methyl phenyl ring siloxane removing moisture, add in the there-necked flask that 500mL is clean
Enter dimethicone 5g, methyl phenyl ring siloxane 136g, add hydrogeneous ring body (the methyl hydrogen ring silicon that 22g is dried
Oxygen alkane), the hydrogeneous double-seal head of 1.8g (tetramethyl two hydrogen-based disiloxane) and the concentrated sulphuric acid of 1.5g mass concentration 98%, 30
It is polymerized 5h at DEG C, adds in 4.5g sodium bicarbonate and pH is to neutral, filter, de-low, obtain the hydrogeneous poly-silica of 140g phenyl
Alkane；140g phenyl hydrogen containing siloxane, 680g tetravinyl tetramethyl-ring siloxanes and 0.016g platinum catalyst are added
In the there-necked flask of 1000mL, react 6h at 80 DEG C, be warming up to 150 DEG C of vacuum removal low molecule, obtain the many vinyls of 250g
The phenyl silicone (C-1) of cyclosiloxane base；Viscosity is 9100mPa.s；
Described embodiment 1～4 and the hydroxy vinyl based polysiloxane (C-2) of comparative example 3 adopt and prepare with the following method:
Dimethicone, methylvinylcyclosiloxane are removed moisture at 40 DEG C respectively, then clean to 500mL
There-necked flask adds the dimethicone 150g and methylvinylcyclosiloxane 6.50g of removing moisture, adds alkali glue
(silicon alkoxide of Tetramethylammonium hydroxide), is polymerized 4h at 100 DEG C, adds the water of 0.20g, be warming up to 150 DEG C of decomposition
Catalyst 4h, then take off low molecule through vacuum, obtain 110g hydroxyvinyl polymethyl siloxane (C-2)；Viscosity is 2300mPa.s.
The hydroxy vinyl based polysiloxane (C-2) of described embodiment 5～6 is adopted and is prepared with the following method:
Dimethicone, methyl phenyl ring siloxane, methylvinylcyclosiloxane are removed moisture at 35 DEG C respectively,
Then in there-necked flask clean for 500mL, add removing the dimethicone 20g of moisture, methyl phenyl ring siloxane
350g and methylvinylcyclosiloxane 5.95g, adds alkali glue (silicon alkoxide of Tetramethylammonium hydroxide), poly-at 100 DEG C
Close 3h, add the water of 0.20g, be warming up to 140 DEG C of decomposition catalyst 5h, then take off low molecule through vacuum, obtain 300g hydroxyl
Base vinyl phenyl silicone (C-2)；Viscosity is 5600mPa.s.
Vinyl silicone oil, phenyl-vinyl silicon oil, common commercially available prod, viscosity is 3000～15000mPa.s.
Vinyl polysiloxane, phenyl vinyl polysiloxane, common commercially available prod, viscosity is 5000～20000mPa.s.
Containing hydrogen silicone oil, phenyl hydrogen-containing silicon oil, common commercially available prod, viscosity is 20～100mPas.
Silicon Containing Hydrogen resin, phenyl Silicon Containing Hydrogen resin, common commercially available prod, viscosity is 20～1500mPa.s.
Propilolic alcohol, 1-alkynyl-1-Hexalin, 2-phenyl-3-butyne-2-alcohol, methyl butynol, for analytical reagent, commonly
Commercially available prod.
Methyl silicone rubber viscosifier, phenyl siloxane rubber viscosifier, common commercially available prod.
Platinum water, Ka Shi platinum catalyst, common commercially available prod.
Embodiment 1
The preparation method of a kind of LED encapsulation liquid silicon rubber composition, comprises the steps:
In 50.0g vinyl silicone oil, addition 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.50g3000ppm,
5.92g gained contains the polymethyl siloxane (C-1) of many vinylcyclosiloxanes base, the poly-methyl of 3.55g gained hydroxyvinyl
Siloxanes (C-2), 0.017g1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 0.65g, mix, then
Add 4.50g containing hydrogen silicone oil, discharging after overall mix homogeneously, prepare LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, it is placed in polytetrafluoroethyl-ne
In alkene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 2h at 150 DEG C, obtain the product test sample of smooth cleaning.
Embodiment 2
The preparation method of a kind of LED encapsulation liquid silicon rubber composition, comprises the steps:
In 50.0g vinyl silicone oil, addition 30.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.36g3000ppm,
4.2g contains the polymethyl siloxane (C-1) of many vinylcyclosiloxanes base, 2.5g hydroxyvinyl polymethyl siloxane (C-2),
0.012g1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 0.90g, mix, be eventually adding 3.50g hydrogeneous
Silicones, discharging after overall mix homogeneously, prepare LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, it is placed in polytetrafluoroethyl-ne
In alkene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test sample of smooth cleaning.
Embodiment 3
The preparation method of a kind of LED encapsulation liquid silicon rubber composition, comprises the steps:
In 50.0g vinyl silicone oil, addition 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.27g5000ppm,
9.80g contains the polymethyl siloxane (C-1) of many vinylcyclosiloxanes base, 5.50g hydroxyvinyl polymethyl siloxane
(C-2), 0.018g1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 2.76g, mix, be eventually adding 7.50g
Containing hydrogen silicone oil, discharging after overall mix homogeneously, prepare LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, it is placed in polytetrafluoroethyl-ne
In alkene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 4h at 150 DEG C, obtain the product test sample of smooth cleaning.
Embodiment 4
The preparation method of a kind of LED encapsulation liquid silicon rubber composition, comprises the steps:
In 10.0g vinyl silicone oil, addition 80g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.22g5000ppm,
10.00g contains the polymethyl siloxane (C-1) of many vinylcyclosiloxanes base, 5.00g hydroxyvinyl polymethyl siloxane
(C-2), 0.015g1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 2.30g, mix, be eventually adding 9.75g
Containing hydrogen silicone oil, discharging after overall mix homogeneously, prepare LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, it is placed in polytetrafluoroethyl-ne
In alkene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test sample of smooth cleaning.
Embodiment 5
The preparation method of a kind of LED encapsulation liquid silicon rubber composition, comprises the steps:
In 50.0g phenyl-vinyl silicon oil, add 50.0g phenyl vinyl polysiloxane, the Ka Shi of 0.03g10000ppm
Platinum catalyst, 14.00g contains the phenyl silicone (C-1) of many vinylcyclosiloxanes base, 5.00g hydroxyvinyl
Phenyl silicone (C-2), 0.015g1-acetenyl-1-Hexalin, the phenyl siloxane rubber viscosifier of 0.81g, mix,
It is eventually adding 43.30g phenyl hydrogen-containing silicon oil, discharging after overall mix homogeneously, prepares LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, it is placed in polytetrafluoroethyl-ne
In alkene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test sample of smooth cleaning.
Embodiment 6
The preparation method of a kind of LED encapsulation liquid silicon rubber composition, comprises the steps:
In 50.0g phenyl vinyl polysiloxane, adding the Ka Shi platinum catalyst of 0.015g10000ppm, 4.50g contains many
The phenyl silicone (C-1) of vinylcyclosiloxanes base, 1.60g hydroxyvinyl phenyl silicone (C-2), 0.0075g
1-acetenyl-1-Hexalin, the phenyl siloxane rubber viscosifier of 1.72g, mix, finally add 30.00g phenyl Silicon Containing Hydrogen
Resin, discharging after overall mix homogeneously, prepare LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, it is placed in polytetrafluoro
In ethylene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test sample of smooth cleaning.
Comparative example 1
In 50.0g vinyl silicone oil, addition 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.50g3000ppm,
0.017g1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 0.65g, mix, then add 3.75g and contain
Hydrogen silicone oil, discharging after overall mix homogeneously, prepare contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned contrast LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared contrast LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, it is placed in poly-four
In fluorothene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 2h at 150 DEG C, obtain the product test of smooth cleaning
Sample.
Comparative example 2
In 50.0g vinyl silicone oil, addition 30.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.36g3000ppm,
0.012g1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 0.90g, mix, finally add 2.65g and contain
Discharging after hydrogen silicones entirety mix homogeneously, prepares contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned contrast LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared contrast LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, it is placed in poly-four
In fluorothene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test of smooth cleaning
Sample.
Comparative example 3
In 50.0g vinyl silicone oil, addition 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.27g5000ppm,
9.80g contains the polymethyl siloxane (C-1) of many vinylcyclosiloxanes base, 5.50g hydroxyvinyl polymethyl siloxane
(C-2), 0.018g1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 2.76g, mix, finally add
7.50g containing hydrogen silicone oil, discharging after overall mix homogeneously, prepare contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned contrast LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared contrast LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, it is placed in metal
In mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 4h at 150 DEG C, obtain product test sample.
Comparative example 4
To 10.0g vinyl silicone oil, add 80g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.22g5000ppm, 0.015g
1-acetenyl-1-Hexalin, the methyl silicone rubber viscosifier of 2.30g, mix, finally add 8.65g containing hydrogen silicone oil,
Discharging after overall mix homogeneously, prepares contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned contrast LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared contrast LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, it is placed in poly-four
In fluorothene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test of smooth cleaning
Sample.
Comparative example 5
In 50.0g phenyl-vinyl silicon oil, add 50.0g phenyl vinyl polysiloxane, the Ka Shi of 0.03g10000ppm
Platinum catalyst, 0.015g1-acetenyl-1-Hexalin, the phenyl siloxane rubber viscosifier of 0.81g, mix, the most again
Add 34.40g phenyl hydrogen-containing silicon oil, discharging after overall mix homogeneously, prepare contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned contrast LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared contrast LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, it is placed in poly-four
In fluorothene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test of smooth cleaning
Sample.
Comparative example 6
In 50.0g phenyl vinyl polysiloxane, add the Ka Shi platinum catalyst of 0.015g10000ppm, 0.0075g1-
Acetenyl-1-Hexalin, the phenyl siloxane rubber viscosifier of 1.72g, mix, finally add 30.00g phenyl hydrogeneous
Silicones, discharging after overall mix homogeneously, prepare contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of above-mentioned contrast LED encapsulation liquid silicon rubber composition, step is as follows:
By prepared contrast LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, it is placed in poly-four
In fluorothene mould, levelling；At 80 DEG C, vulcanize 1h, then vulcanize 3h at 150 DEG C, obtain the product test of smooth cleaning
Sample.
Test example
Hot strength and the elongation at break of the product test sample that above example and comparative example prepare are surveyed according to GB/T528-1998
Examination, tearing strength is according to GB/T529-1999 test, and hardness is according to GB/T531-1999, and refractive index uses Abbe refractometer to exist
Testing at 25 DEG C, light transmittance uses the test sheet that ultraviolet-visible spectrophotometer test 1mm is thick.
After testing, result is as shown in table 1.
Table 1
From table 1 embodiment 1～2 and 4～6 and the testing result contrast of comparative example 1～2 and 4～6, embodiment 1～2
With 4～6 owing to adding features based polysiloxane so that the hot strength of LED encapsulation liquid silastic, tear are by force
The mechanical mechanics properties such as degree, elongation at break have had than the silicone rubber (comparative example 1～2 and 4～6) of common reinforcement and have been greatly improved,
Wherein, hot strength improves more than 35%, and tearing strength improves more than 40%, and elongation at break improves more than 30%,
Hardness the most slightly improves.
Additionally, by embodiment 3 and comparative example 3 it can be seen that the liquid silicon rubber composition of same component, same sulfuration work
Skill condition, uses Teflon mould better, thoroughly than the mechanical mechanics property of the silicone rubber test specimens using metal die to prepare
Light rate is the highest, and this is primarily due to the test specimens using Teflon mould to prepare, and the demoulding is easy, and surface cleaning is flawless
Defect.
Claims (17)
1. a LED encapsulation liquid silicon rubber composition, it is characterised in that component is as follows, is weight portion:
Organopolysiloxane (A) 60～120 parts containing aliphatic unsaturated bond, organic hydrogen polysiloxanes (B) 2～45 parts, features based polysiloxane (C) 5～30 parts, platinum complex catalyst (D) 0.01～0.5 part, inhibitor (E) 0.01～0.05 part, viscosifier (F) 0.5～3 part；
The described organopolysiloxane (A) containing aliphatic unsaturated bond is containing the organopolysiloxane (A-2) of resin structure containing 2 alkenyl groups above in the straight chain organopolysiloxane (A-1) of 2 alkenyl groups above and/or molecule in molecule；
Described organic hydrogen polysiloxanes (B) is containing the organic hydrogen polysiloxanes (B-2) of resin structure containing more than 2 H atom in the straight chain organic hydrogen polysiloxanes (B-1) of more than 2 H atom and/or molecule in molecule；
Described features based polysiloxane (C), for containing the polysiloxanes (C-1) of many vinylcyclosiloxanes base in molecule, or is polysiloxanes (C-1) and the hydroxy vinyl based polysiloxane (C-2) containing many vinylcyclosiloxanes base in molecule；
The formula of the polysiloxanes (C-1) containing many vinylcyclosiloxanes base in molecule is as follows:
In formula: R1For the cyclosiloxane base containing many vinyls, wherein k1=2,3 or 4, k2=2,3 or 4, k3=2,3 or 4, R1It is positioned at the end of strand and/or the sidepiece of strand；R2、R2 ′ For methyl, ethyl, propyl group or phenyl；Viscosity is 1000-20000mPa s；
The formula of hydroxy vinyl based polysiloxane is as follows:
Wherein Me represents methyl；Chain number s=0～1000, t=1～100, q=1～1000；Viscosity is 10～10000mPa s；
Described platinum complex catalyst (D) is platinum water or Ka Shi platinum catalyst；
Described inhibitor (E) is alkynol class inhibitor, and viscosifier (F) are methyl silicone rubber viscosifier or phenyl siloxane rubber viscosifier；
The chain number a=10～100 of the described polysiloxanes containing many vinylcyclosiloxanes base, b=50～500, c=10～500.
2. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterised in that component is as follows, is weight portion:
Organopolysiloxane (A) 80～100 parts containing aliphatic unsaturated bond, organic hydrogen polysiloxanes (B) 7～30 parts, features based polysiloxane (C) 5～15 parts, platinum complex catalyst (D) 0.015～0.03 part, inhibitor (E) 0.015～0.02 part, viscosifier (F) 1～2 part.
3. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterized in that, in described molecule, the straight chain organopolysiloxane (A-1) containing 2 alkenyl groups above is selected from vinyl silicone oil and/or phenyl-vinyl silicon oil, and viscosity is 3000～15000mPa s；The organopolysiloxane (A-2) of the resin structure containing 2 alkenyl groups above in described molecule is selected from vinyl polysiloxane and/or phenyl vinyl polysiloxane, and viscosity is 5000～20000mPa s.
4. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterised in that in described molecule, the straight chain organic hydrogen polysiloxanes (B-1) containing more than 2 H atom is selected from containing hydrogen silicone oil and/or phenyl hydrogen-containing silicon oil, and viscosity is 20～100mPa s；The organic hydrogen polysiloxanes (B-2) of the resin structure containing more than 2 H atom in described molecule is 20～1500mPa s selected from the viscosity of Silicon Containing Hydrogen resin and/or phenyl Silicon Containing Hydrogen resin.
5. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterised in that described R1For one or more in many vinyl three cyclosiloxane bases, many vinyls Fourth Ring siloxy group, many vinyls five rings siloxy group with the combination of any ratio.
6. LED encapsulation liquid silicon rubber composition as claimed in claim 5, it is characterised in that R1For many vinyls cyclotrisiloxane base, many vinyls Fourth Ring siloxy group one or both with the combination of any ratio.
7. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterised in that the platinum content of described platinum complex catalyst (D) is 3000～10000ppm.
8. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterised in that the value of chain number s, t and q of described hydroxy vinyl based polysiloxane is s=0～200, t=20～50, q=30～200.
9. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterised in that in described LED encapsulation liquid silicon rubber composition, the mol ratio of Si-Vi:Si-H is 1:(1～1.8).
10. LED encapsulation liquid silicon rubber composition as claimed in claim 9, it is characterised in that the mol ratio of Si-Vi:Si-H is 1:(1.1～1.5).
11. LED encapsulation liquid silicon rubber compositions as claimed in claim 1, it is characterised in that described inhibitor is propilolic alcohol, 1-acetenyl-1-Hexalin, 2-phenyl-3-butyne-2-alcohol, methyl butynol.
12. LED encapsulation liquid silicon rubber compositions as claimed in claim 1, it is characterised in that the polysiloxanes (C-1) of described many vinylcyclosiloxanes base is adopted and prepared with the following method:
(1) after respectively dimethicone and methyl phenyl ring siloxane being removed moisture, 90:(0 in mass ratio～1) or 1:(18.5～37) mixing, the concentrated sulphuric acid of mass concentration 98% of the hydrogeneous ring body being dried, hydrogeneous double-seal head and gross weight 0.5～1.5% is added again in the ratio of dimethicone and the 0.08 of methyl phenyl ring siloxane gross mass～0.1, polyreaction 3～5h at 30～50 DEG C, add in sodium bicarbonate and pH is to neutral, filter, de-low, obtain hydrogen containing siloxane；
(2) in the hydrogen containing siloxane that step (1) prepares, add the tetravinyl tetramethyl-ring siloxanes of more than 5 times of quality, add platinum catalyst, the concentration making platinum catalyst is 15～25ppm, 4～6h are reacted under conditions of 80～100 DEG C, it is warming up to 140～150 DEG C of vacuum removal low molecule, obtains the polysiloxanes (C-1) of many vinylcyclosiloxanes base.
13. LED encapsulation liquid silicon rubber compositions as claimed in claim 12, it is characterised in that described hydrogeneous ring body is selected from methylhydracyclosiloxane；Described hydrogeneous double-seal head is selected from tetramethyl two hydrogen-based disiloxane.
14. LED encapsulation liquid silicon rubber compositions as claimed in claim 1, it is characterised in that described hydroxy vinyl based polysiloxane (C-2) is adopted and prepared with the following method:
By dimethicone, methyl phenyl ring siloxane and methylvinylcyclosiloxane remove moisture at 35～40 DEG C respectively, then dimethicone is pressed, methyl phenyl ring siloxane is 10:(0～0.005 with the mass ratio of methylvinylcyclosiloxane): (1～1.2) or 1:(18.4～37.5): (0.1～0.12) mixes, add alkali glue, polyase 13～5h under conditions of 90～100 DEG C, add 0.18～0.20g water, it is warming up to 140～160 DEG C, decompose catalysis 3～5h, low molecule is taken off again through vacuum, obtain hydroxy vinyl based polysiloxane (C-2).
15. LED encapsulation liquid silicon rubber compositions as claimed in claim 14, it is characterised in that described alkali glue is selected from the silicon alkoxide of Tetramethylammonium hydroxide.
The preparation method of LED encapsulation liquid silicon rubber composition described in 16. 1 kinds of claim 1, it is characterised in that comprise the steps:
After organopolysiloxane (A) containing aliphatic unsaturated bond, organic hydrogen polysiloxanes (B) and features based polysiloxane (C) are mixed in proportion, add platinum complex catalyst (D), inhibitor (E), viscosifier (F), mix homogeneously, prepares LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of LED encapsulation liquid silicon rubber composition described in 17. claim 16, it is characterised in that step is as follows:
By prepared LED encapsulation liquid silicon rubber composition at ambient temperature, vacuum defoamation 5～30min, it is placed in Teflon mould；Through vulcanizing 0.5～1.5h at 50～80 DEG C, then 100～200 DEG C of sulfurations 0.5～4h, or, through vulcanizing 2h at 100～200 DEG C, obtain test specimens.
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| CN112679958A (en) * | 2020-12-18 | 2021-04-20 | 厦门赛尔特电子有限公司 | Silicon rubber and preparation method thereof, and piezoresistor and preparation method thereof |
| CN113105863B (en) * | 2021-03-01 | 2022-06-14 | 华南理工大学 | Ultrahigh-hardness silicone resin film and preparation method and application thereof |
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| CN101712800B (en) * | 2009-11-06 | 2012-10-03 | 陈俊光 | Organic silicon resin encapsulant of large power LED and preparing method thereof |
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