CN103360603A - Phenyl vinyl silicone resin for packaging LED (light-emitting diode) and preparation method thereof - Google Patents
Phenyl vinyl silicone resin for packaging LED (light-emitting diode) and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of polymer materials and provides phenyl vinyl silicone resin for packaging an LED (light-emitting diode). The phenyl vinyl silicone resin comprises an inner core and a flexible chain segment which is cross-linked outside the inner core, wherein the inner core is a phenyl alkoxysilane polymer, and the flexible chain segment is at least one of vinyl-terminated polydimethylsiloxane, vinyl-terminated poly(methyl phenyl siloxane) and vinyl-terminated polydimethyl diphenyl siloxane. The invention further provides a preparation method of the phenyl vinyl silicone resin for packaging the LED. The method has the advantages of mild process conditions, simplicity and easiness in operation, wide range of sources of raw materials and good repeatability, and a product obtained after curing of the prepared phenyl vinyl silicone resin has the advantages of better tensile strength, hardness and other mechanical properties.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of LED encapsulation phenyl vinyl polysiloxane and preparation method thereof.
Background technology
Power type light-emitting diode (Light Emitting Diode, LED) being is the device of luminous energy with electric energy conversion directly, with traditional incandescent light, luminescent lamp, the light sources such as high-intensity gas discharge lamp are compared, energy consumption only is 1/10 of conventional light source, have energy-conservation, environmental protection, safety, low-heat, waterproof, shockproof, light, life-span is long, the advantages such as high brightness, be described as the 21 century new light sources, along with the development of technology, now be widely used in the backlight of liquid-crystal display, life lighting, automobile lighting, the sign illumination, Landscape Lighting, the big area picture and text show full-color screen etc.
Traditional LED packaged material is bisphenol A-type or polypropylene acid type transparent epoxy resin, introduce Resins, epoxy such as patent US5998925, US6069440, US6608332, JP-A33241338 philosophy and be applied to the LED encapsulation, but because Resins, epoxy easily jaundice under the uvioresistant illuminate condition, thermal resistance is high, low temperature becomes fragile, the defective such as easy to crack, development along with the LED technology, various performance requriementss to packaged material are also more and more higher, and Resins, epoxy can not satisfy LED to the requirement of the performances such as the heat of its packaged material, light, power.
The advantages such as that organosilicon macromolecule material such as silicon gel, silicon rubber, silicone resin etc. have is ageing-resistant, high-low temperature resistant, ultraviolet resistance radiation are present comparatively desirable packaged materials.The advantages such as wherein phenyl polysiloxane need not plastic casing owing to have refractive index height, good, the direct perfusion of anti-ventilative water permeability, and is easy to use have been widely used in the packaging procesies such as LED paster, Molding.Hydrosilylation reaction occurs and cross-linking vulcanized in the organosilicon polymer of phenyl polysiloxane and silicon-hydrogen bond containing under the metal catalyst effects such as platinum, cobalt, cure conditions is gentle, under middle temperature, get final product high-speed vulcanization, the by products such as solvent-free, low molecule of while are discharged, produce bubble or trachoma when having avoided sulfuration, and cured product water, shock, shock-resistance, thermal conductivity are good, therefore are well suited for the LED encapsulation.
Patent US20040116640, US20050212008 join phenyl chlorosilane, vinyl end socket with water, take toluene as solvent, be hydrolyzed and wash again layering after the polymerization, decompression removes low molecule, obtain the water white transparency product, because reaction monomers is organochlorosilane, can produce a large amount of acid solutions in the reaction process, equipment is caused corrosion, and the storage of raw material and the synthesis technique of product are made troubles, and do not have concentrated soft segment in the synthetic product, excessive with product internal stress after the hydrogeneous linking agent sulfuration, shock resistance is not good enough.
It is raw material that patent TW201229496A adopts the octadecyloxy phenyl TMOS, use alkali as a catalyst, synthetic phenyl vinyl polysiloxane and hydrogeneous linking agent vulcanize under platinum catalyst, and the product that obtains cold cycling under-40 ℃～100 ℃ conditions is impacted and only do not ftractureed for 50 times.
CN1011787133 has reported a kind of with phenyl or vinyl three-functionality-degree siloxanes and two functionality polysiloxane hydrolytic polymerization under hydrochloric acid catalysis, obtain a kind of method that contains the silicone resin of three-functionality-degree polysilsesquioxane and two functionality polysiloxane segments, refractive index is on the low side, and add fashionable as reaction product with hydroxy silicon oil, easily under the acidic catalyst condition, carry out the ring-closure reaction that head is stung tail, easily make the ring body impurity that is mixed with a small amount of low refractive index in the product, easily make product muddy, and refractive index is on the low side, is applied to the transmission efficiency that the LED encapsulation will reduce its optical throughput.
Patent US200724979(A1) announced two functional group's organopolysiloxane and the cohydrolysis polymerization in toluene of phenyl-trichloro-silicane, vinyl end socket or hydrogeneous end socket of adopting the chlorine end-blocking, obtain molecular weight and reach 58000～62000 solid silicon resin, the product after the sulfuration of adding platinum can stand 100-50 ℃/150 ℃ cold cycling impacts and not ftracture.But because two functional group's organopolysiloxane segments and the disorderly and unsystematic state of three-dimensional silicone treated, relatively poor with product mechanical property after the sulfuration of hydrogeneous linking agent such as tensile strength, tearing toughness, and the product relative molecular weight is large, be solid under the normal temperature, greatly limit its application in the LED encapsulation, two functional group's organopolysiloxane raw material sources of chlorine end-blocking are few simultaneously, price.
Because the technical development of LED, power is increasing, and thermal value is also increasing, thus more and more harsher to the thermal characteristics, the particularly requirement of cold-hot impact property of packaged material, as in the impact of-40 ℃～110 ℃ lower abilities more than 1000 times.And with the LED packaged material of above-mentioned phenyl polysiloxane preparation, excessive with internal stress after the linking agent sulfuration, shock resistance is relatively poor, is difficult to reach application requiring, and some product is solid-state at normal temperatures, is difficult to adapt to the requirement of modern LED packaging process.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective of prior art, and a kind of LED encapsulation phenyl vinyl polysiloxane and preparation method thereof is provided.
The present invention realizes like this, a kind of LED encapsulation phenyl vinyl polysiloxane, it comprises kernel and crosslinked soft segment outside kernel, wherein, kernel is the phenyl alkoxysilane polymer, and soft segment is at least a in the polydimethyldiphenylsiloxane of the PSI of polydimethylsiloxane, ethenyl blocking of ethenyl blocking and ethenyl blocking.
The present invention also provides the preparation method of above-mentioned LED encapsulation with phenyl vinyl polysiloxane, and it comprises the steps:
Be that the water of 1～100 part octadecyloxy phenyl TMOS monomer, 10～50 parts organic solvent and 20～40 parts mixes with mass fraction, drip the acid catalyst of 0.1～10% octadecyloxy phenyl TMOS monomer mass, 0～30 ℃ of lower reaction 1～8 hour, obtain reaction solution A;
Add at least a in alkoxy end-capped polydimethylsiloxane, PSI, the polydimethyldiphenylsiloxane in the described reaction solution A, continue reaction and add the vinyl closure agent after 3～10 hours, reacted 1～3 hour, and obtained reaction solution B;
With described reaction solution B standing demix, add alkali after the acid solution of removal upper strata and regulate the pH value to neutral, wash, obtain mixture;
Mixture is equal to or higher than under the 0.1Mpa condition in vacuum tightness, is heated to 110 ℃～130 ℃, obtain described phenyl vinyl polysiloxane.
LED encapsulation of the present invention is high with the prepared phenyl vinyl polysiloxane refractive index of the preparation method of phenyl vinyl polysiloxane, can reach 1.55/ ℃), be liquid under the normal temperature, be convenient to LED encapsulation point adhesive process, fast with hydrogeneous linking agent vulcanization rate, and good with the phenyl silicone oil compatibleness, non-whitening, become muddy, the curing rear surface is wrinkle resistant, without decorative pattern.The prepared phenyl vinyl polysiloxane of the present invention contains the soft segment of equivalent length, and do not contain low refractive index impurity, and soft segment is to add the condensation that is hydrolyzed after forming inner core again, the product mechanical property behind the crosslinking curing such as tensile strength is good, the cold-and-heat resistent impact excellent.Manufacturing condition of the present invention is gentle, simple, and raw material sources are extensive, good reproducibility, and can adjust according to actual needs the parameters such as product viscosity, contents of ethylene, phenyl content, thereby have widely adaptability.
Description of drawings
Fig. 1 is the three-dimensional structure diagram that phenyl vinyl polysiloxane is used in the LED encapsulation of the embodiment of the invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
The invention provides a kind of LED encapsulation phenyl vinyl polysiloxane, it comprises kernel and crosslinked soft segment outside kernel, wherein, kernel is the phenyl alkoxysilane polymer, and soft segment is at least a in the polydimethyldiphenylsiloxane of the PSI of polydimethylsiloxane, ethenyl blocking of ethenyl blocking and ethenyl blocking.
Wherein, preferably, the molecule of described phenyl vinyl polysiloxane link length is 5～50, the phenyl mole number account for methyl, phenyl and vinyl total mole number and 0.4～0.8, the vinyl mole number account for methyl, phenyl and vinyl total mole number and 0.1～0.4.The refractive index of described phenyl vinyl polysiloxane is about 1.53～1.55/20 ℃, and 25 ℃ of lower viscosity are less than 30000mPa.s.
More specifically, LED encapsulation of the present invention with the general structure of phenyl vinyl polysiloxane is:
(PhSiO
1.5)
a(Ph
2SiO)
b(PhMeSiO)
c(Me
2SiO)
d(ViMe
2SiO
0.5)
e
Wherein, Ph represents phenyl-C
6H
5, Me represents methyl-CH
3, Vi represents vinyl-CH=CH
2, the span of a is that the span of 0.01～1, b is that the span of 0～0.1, c is that the span of 0～0.8, d is 0～0.5, and a+b+c〉and 0, the span of e is 0.1～0.4.Described LED encapsulation is continuous link with phenyl vinyl polysiloxane, molecule link length is 5～50, the span of e is 0.1～0.4, and with all groups that Siliciumatom directly links to each other in, n (Ph)/n (Me+Ph+Vi) span is 0.4～0.8, n (Vi)/n (Me+Ph+Vi) span is 0.1～0.4 o'clock, and the product refractive index is at 1.53～1.55/20 ℃, and 25 ℃ of lower viscosity are less than 30000mPa.s.In the three-dimensional arrangement, a plurality of (PhSiO
1.5)
aForm and concentrate T kernel, (Ph
2SiO)
b(PhMeSiO)
c(Me
2SiO)
dForm and concentrate D soft segment, (ViMe
2SiO
0.5)
eBe in chain end.
The present invention also provides the preparation method of above-mentioned LED encapsulation with phenyl vinyl polysiloxane, and it comprises the steps:
Be that the water of 1～100 part octadecyloxy phenyl TMOS monomer, 10～50 parts organic solvent and 20～40 parts mixes with mass fraction, drip the acid catalyst of 0.1～10% octadecyloxy phenyl TMOS monomer mass, 0～30 ℃ of lower reaction 1～8 hour, obtain reaction solution A;
Add at least a in alkoxy end-capped polydimethylsiloxane, PSI, the polydimethyldiphenylsiloxane in the described reaction solution A, continue reaction and add the vinyl closure agent after 3～10 hours, reacted 1～3 hour, and obtained reaction solution B;
With described reaction solution B standing demix, add alkali after the acid solution of removal upper strata and regulate the pH value to neutral, wash, obtain mixture;
Mixture is equal to or higher than under the 0.1Mpa condition in vacuum tightness, is heated to 110 ℃～130 ℃, obtain described phenyl vinyl polysiloxane.
Concrete principle is: add first by octadecyloxy phenyl TMOS monomer, hydrolytic condensation under acidic conditions, form fine and close kernel (T), the soft segment that adds again an amount of concentrated D of containing structure (polydimethylsiloxane or PSI), add again at last the vinyl closure agent, obtain the phenyl vinyl polysiloxane product of three-dimensional arrangement as shown in Figure 1.
Particularly, described phenyl alkoxyl group monomer comprises at least a in phenyltrimethoxysila,e, phenyl triethoxysilane, dimethoxydiphenylsilane, phenylbenzene diethoxy silane, phenylbenzene methoxy base oxethyl silane, aminomethyl phenyl dimethoxy silane, the aminomethyl phenyl diethoxy silane.
Described an acidic catalyst can be selected the protonic acids such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, perchloric acid, Hydrogen bromide, hydroiodic acid HI, also can select trifluoromethane acid, strong acidic ion resin etc., wherein, is preferably hydrochloric acid.
Described vinyl closure agent is at least a in tetramethyl divinyl disiloxane, phenylbenzene dimethyl divinyl disiloxane, dimethyl vinylsiloxane, the phenyl vinyl siloxanes, wherein, is preferably tetramethyl divinyl disiloxane.
Described alkoxyl group polydimethylsiloxane is the polydimethylsiloxane of the end-blockings such as methoxyl group, oxyethyl group, or at least a in the PSI of methoxyl group, oxyethyl group end-blocking, polydimethyldiphenylsiloxane.
Described solvent comprises the varsols such as toluene, dimethylbenzene, cyclohexane; The ketones solvents such as acetone, butanone, pimelinketone; The alcoholic solvents such as methyl alcohol, ethanol, Virahol; The esters solvents such as ethyl acetate, ethyl formate, butylacetate.
Described for selecting ammoniacal liquor, sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium bicarbonate etc. with the alkali of surplus acid.
The LED encapsulation provided by the invention preparation method of phenyl vinyl polysiloxane, can control product kernel size, viscosity, refractive index, contents of ethylene etc. by conditions such as raw material monomer proportioning, reaction times, temperature, pH values, thereby obtain the LED packaging plastic of different hardness, mechanical strength with the hydrogeneous linking agent addition of corresponding phenyl.Compare with existing synthesis technique, the prepared LED encapsulation of the method, good fluidity high with the phenyl vinyl polysiloxane shading rate, it is better to contain the mechanical properties such as two functionality polysiloxane segments and tensile strength, hardness, product with this products solidifying gained is used for the LED encapsulation, and its cold-and-heat resistent impact property is very excellent.
Embodiment 1:
In the 2L there-necked flask that 100g toluene and 50g water are housed, add 198g phenyltrimethoxysila,e, 244.4g dimethoxydiphenylsilane, 18.2g aminomethyl phenyl dimethoxy silane, 30 parts of massfractions of dropping are 25% hydrochloric acid under 30 ℃, fully stir, dropwise in one hour, continue to stir 2～3 hours, adding the 76.3g structure is CH again again
3O (CH
3)
2Si[(OSi (CH
3)
2)]
18OSi (CH
3)
2OCH
3Polydimethylsiloxane and 20g toluene, react after 1 hour, be warming up to 80 ℃, add 111.6g tetramethyl-divinyl sily oxide, maintain the temperature at 80 ℃, react and stop after 10 hours, be cooled to again layering after the room temperature, add the neutralization of 5g sodium hydroxide, be washed to neutrality, at 110 ℃, decompression is 3 hours under the condition of vacuum tightness 0.9MPa～1.0MPa, remove low-boiling point material, obtain water white transparency phenyl vinyl polysiloxane 392.3g, viscosity is 8000mPa.s/25 ℃, 1.5356/20 ℃ of refractive index, contents of ethylene are 3.0%(m/m)
Embodiment 2:
In the 2L there-necked flask that 100g toluene and 50g water are housed, add 198g phenyltrimethoxysila,e, 488.8g dimethoxydiphenylsilane, 9.1g aminomethyl phenyl dimethoxy silane, lower to drip 30 parts of massfractions be 25% hydrochloric acid at 30 ℃ again, fully stir, dropwise in one hour, continue to stir 2～3 hours, adding the 43g structure is CH again again
3O (CH
3)
2Si[(OSi (CH
3)
2)]
9OSi (CH
3)
2OCH
3Polydimethylsiloxane and 20g toluene, react after 1 hour, be warming up to 80 ℃, add 223.2g tetramethyl-divinyl sily oxide, maintain the temperature at 80 ℃, react and stop after 10 hours, be cooled to again layering after the room temperature, add the neutralization of 5g sodium hydroxide, be washed to neutrality, at 110 ℃, decompression is 3 hours under the condition of vacuum tightness 0.9MPa～1.0MPa, remove low-boiling point material, obtain water white transparency phenyl vinyl polysiloxane 392.3g, viscosity is 3000mPa.s/25 ℃, 1.5401/20 ℃ of refractive index, contents of ethylene are 4.1%(m/m).
Comparative Examples 1:
In the 2L there-necked flask that 100g toluene and 50g water are housed, add 198g phenyltrimethoxysila,e, 244.4g dimethoxydiphenylsilane, 18.2g aminomethyl phenyl dimethoxy silane, adding the 76.3g structure is CH again
3O (CH
3)
2Si[(OSi (CH
3)
2)]
18OSi (CH
3)
2OCH
3Polydimethylsiloxane, 111.6g tetramethyl-divinyl sily oxide, 30 parts of massfractions of dropping are 25% hydrochloric acid under 30 ℃, be warming up to 80 ℃, maintain the temperature at 80 ℃, react and stop after 10 hours, be cooled to again layering after the room temperature, add the neutralization of 5g sodium hydroxide, be washed to neutrality, at 110 ℃, decompression was taken off low 3 hours under the condition of vacuum tightness 0.9MPa～1.0MPa, obtain, water white transparency phenyl vinyl polysiloxane 391.5g, viscosity is 5000mPa.s/25 ℃, 1.5326/20 ℃ of refractive index, contents of ethylene are 2.5%(m/m).
Comparative Examples 2:
In the 2L there-necked flask that 100g toluene and 50g water are housed, add the 198g phenyltrimethoxysila,e, 488.8g dimethoxydiphenylsilane, 9.1g aminomethyl phenyl dimethoxy silane, add again the 65.87g dimethyldimethoxysil,ne, 223.2g tetramethyl-divinyl sily oxide, lower to drip 30 parts of massfractions be 25% hydrochloric acid at 30 ℃ again, fully stir, dropwise in one hour, be warming up to 80 ℃, maintain the temperature at 80 ℃, react and stop after 10 hours, be cooled to again layering after the room temperature, add the neutralization of 5g sodium hydroxide, be washed to neutrality, at 110 ℃, decompression was taken off low 3 hours under the condition of vacuum tightness 0.9MPa-1.0MPa, obtain water white transparency phenyl vinyl polysiloxane 388.2g, viscosity is 2300mPa.s/25 ℃, and 1.5396/20 ℃ of refractive index, contents of ethylene are 3.4%(m/m).
Test respectively the refractive index of the lower refractive index test of the viscosity of 25 ℃ of lower institute synthesis of phenyl vinyl polysiloxanes and 20 ℃ institute synthesis of phenyl vinyl polysiloxane, the standard of institute's reference is respectively: DIN53019, GB/T614-2006.
Adopt the contents of ethylene of iodometric determination product, the product of namely getting about 0.1g is dissolved in tetracol phenixin, the iodine bromide IBr reagent that adds again 10mL0.1mol/L fully after the vibration, was in the dark placed 1 hour, then add 5mL concentration and be 10% liquor kalii iodide, again fully vibration is with the sodium thiosulfate standard solution titration of 0.1mol/L, take starch as the index agent, drop to blue the disappearance and be terminal point, do simultaneously blank test.
Contents of ethylene is calculated as follows:
Vinyl %=[CB * ((V0-V1)/2) * 27 * 100%]/(m * 1000)
In the formula:
V0---blank test Sulfothiorine consumption, mL;
V1---titration sample Sulfothiorine consumption, mL;
CB---Concentration of Sodium Thiohsulfate Standard Solution, mol/L;
M---sample mass, g.
The curing of ethenylphenyl silicone resin and the sign of cured product
Get a certain amount of ethenylphenyl silicone resin that synthesizes, adding an amount of hydrogen content is 0.4158%, and structure is (PhSiO
1.5)
0.1(Ph
2SiO)
0.6(Me
2SiO)
0.2(HMe
2SiO
0.5)
0.4The hydrogeneous linking agent of phenyl, make wherein n (Si-H)/n (Vi)=1.5/1, add a small amount of 1,3-divinyl-1,1, the complex compound of 3,3-tetramethyl disiloxane and platinum, wherein platinum content is 50ppm, 1% isocyanuric acid ester Trimethoxy silane is adhesion promotor, 0.01% ethyl cyclohexanol is as cured modified dose, and control product operable time stirs, deaeration is to transparent, steel die or the injection of injecting 2mm comprise the GaN chip, the PPA support, welded in the LED light emitting composition (5050 SMD lamp) of gold thread, cure conditions is 150 ℃ of lower bakings 3 hours, obtains water white test piece or 5050 type LED SMD lamps.
The mechanical property of cured article such as hardness, tensile strength, elongation at break etc. can be tested by the test piece of gained, and reference standard is respectively D2204, D412.
The test of cold-and-heat resistent impact
By 5050 made type LED SMD lamps are placed carry out cold cycling Impact Test 1000 times under-40 ℃ of (30min)～110 ℃ (30min) after, with the LED SMD lamp whether dead lamp judge the cold-and-heat resistent impact property of cured article, if there is dead lamp situation then not pass through, then pass through test without dead lamp situation.
Get respectively embodiment 1 and 2 and comparative example 1 and 2 in phenyl vinyl polysiloxane 100g, add an amount of (PhSiO
1.5)
0.1(Ph
2SiO)
0.6(Me
2SiO)
0.2(HMe
2SiO
0.5)
0.40.1g1,3-divinyl-1,1,3, the complex compound of 3-tetramethyl disiloxane and platinum, wherein platinum content is 50ppm, and about 1% isocyanuric acid ester Trimethoxy silane is as adhesion promotor, and 0.01% ethyl cyclohexanol is as cured modified dose, be heating and curing under 150 ℃ 3 hours, and tested respectively mechanical property, cold-and-heat resistent impact property, the anti-gas permeation performance of resulting product by the method for reference example 2.Table 1 has been listed its accordingly result.
As can be seen from Table 1, the LED encapsulation that embodiment 1 and embodiment 2 obtains is better than comparative example 1 and 2 with the performance of phenyl vinyl resin, proving again the advantage of the crosslinked kernel polymer materials of this soft segment.
Table 1
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a LED encapsulates and uses phenyl vinyl polysiloxane, it is characterized in that, described phenyl vinyl resin comprises kernel and crosslinked soft segment outside kernel, wherein, kernel is the phenyl alkoxysilane polymer, and soft segment is at least a in the polydimethyldiphenylsiloxane of the PSI of polydimethylsiloxane, ethenyl blocking of ethenyl blocking and ethenyl blocking.
2. a kind of LED according to claim 1 encapsulates and uses phenyl vinyl polysiloxane, it is characterized in that, the molecule link length of described phenyl vinyl polysiloxane is 5～50, the phenyl mole number account for methyl, phenyl and vinyl total mole number and 0.4～0.8, the vinyl mole number account for methyl, phenyl and vinyl total mole number and 0.1～0.4.
3. LED encapsulation according to claim 1 and 2 comprises the steps: with the preparation method of phenyl vinyl polysiloxane
Be that the water of 1～100 part octadecyloxy phenyl TMOS monomer, 10～50 parts organic solvent and 20～40 parts mixes with mass fraction, drip the acid catalyst of 0.1～10% octadecyloxy phenyl TMOS monomer mass, 0～30 ℃ of lower reaction 1～8 hour, obtain reaction solution A;
Add alkoxy end-capped polydimethylsiloxane, PSI, polydimethyldiphenylsiloxane (at least a in the poly-phenylbenzene in the described reaction solution A, continue reaction and add the vinyl closure agent after 3～10 hours, reacted 1～3 hour, and obtained reaction solution B;
With described reaction solution B standing demix, add alkali after the acid solution of removal upper strata and regulate the pH value to neutral, wash, obtain mixture;
Mixture is equal to or higher than under the 0.1Mpa condition in vacuum tightness, is heated to 110 ℃～130 ℃, obtain described phenyl vinyl polysiloxane.
4. LED according to claim 3 encapsulates the preparation method with phenyl vinyl polysiloxane, it is characterized in that described phenyl alkoxyl group monomer is at least a in phenyltrimethoxysila,e, phenyl triethoxysilane, dimethoxydiphenylsilane, phenylbenzene diethoxy silane, phenylbenzene methoxy base oxethyl silane, aminomethyl phenyl dimethoxy silane, the aminomethyl phenyl diethoxy silane.
5. LED according to claim 3 encapsulates and uses phenyl vinyl polysiloxane, it is characterized in that described an acidic catalyst is at least a in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, perchloric acid, Hydrogen bromide, hydroiodic acid HI fluoroform alkanoic acid, the strong acidic ion resin.
6. phenyl vinyl polysiloxane is used in LED encapsulation according to claim 5, it is characterized in that described an acidic catalyst is hydrochloric acid.
7. LED according to claim 3 encapsulates and uses phenyl vinyl polysiloxane, it is characterized in that described vinyl closure agent is at least a in tetramethyl divinyl disiloxane, phenylbenzene dimethyl divinyl disiloxane, dimethyl vinylsiloxane, the phenyl vinyl siloxanes.
8. phenyl vinyl polysiloxane is used in LED encapsulation according to claim 7, it is characterized in that described vinyl closure agent is tetramethyl divinyl disiloxane.
9. phenyl vinyl polysiloxane is used in LED according to claim 3 encapsulation, it is characterized in that, described solvent is at least a in varsol, ketones solvent, alcoholic solvent, the esters solvent.
10. phenyl vinyl polysiloxane is used in LED according to claim 3 encapsulation, it is characterized in that, described alkali is at least a in ammoniacal liquor, sodium hydroxide, potassium hydroxide, lithium hydroxide, the sodium bicarbonate.
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| CN104177619A (en) * | 2014-08-04 | 2014-12-03 | 深圳市明粤科技有限公司 | Synthetic method of organic silicon resin with core-shell structure for LED (light-emitting diode) encapsulating |
| CN104558617A (en) * | 2015-01-15 | 2015-04-29 | 杭州杭科光电股份有限公司 | Method for preparing toughened phenyl vinyl silicone resin |
| CN104558617B (en) * | 2015-01-15 | 2017-02-22 | 杭州杭科光电股份有限公司 | Method for preparing toughened phenyl vinyl silicone resin |
| CN104592518A (en) * | 2015-01-30 | 2015-05-06 | 上海交通大学 | Methyl phenyl vinyl aluminum-silicon resin for LED packaging adhesive and preparation method thereof |
| CN105111442A (en) * | 2015-07-20 | 2015-12-02 | 中国工程物理研究院化工材料研究所 | Three-layer core-shell tight ball type MDT silicon resin and preparation method thereof |
| CN105111442B (en) * | 2015-07-20 | 2018-09-25 | 中国工程物理研究院化工材料研究所 | Close ball-type MDT silicones of three-layer nuclear shell and preparation method thereof |
| CN108369927A (en) * | 2015-11-27 | 2018-08-03 | 三菱电机株式会社 | Power semiconductor device |
| CN108369927B (en) * | 2015-11-27 | 2021-06-11 | 三菱电机株式会社 | Power semiconductor device |
| CN107828057A (en) * | 2017-11-13 | 2018-03-23 | 唐山三友硅业有限责任公司 | The silicone-modified epoxy resin preparation method and applications of LED encapsulation |
| CN111349242A (en) * | 2019-08-28 | 2020-06-30 | 江西纳恩新材料有限公司 | Preparation method of isocyanate-containing silicon rubber tackifier |
| CN112680179A (en) * | 2020-12-25 | 2021-04-20 | 苏州禾川化学技术服务有限公司 | Nano interface treating agent for silicon sulfide rubber and preparation method thereof |
| CN112680179B (en) * | 2020-12-25 | 2022-10-28 | 苏州禾川化学技术服务有限公司 | Nano interface treating agent for silicon sulfide rubber and preparation method thereof |
| CN115975596A (en) * | 2023-03-20 | 2023-04-18 | 淄博国创中心先进车用材料技术创新中心 | Bi-component organic silicon pouring sealant and preparation method thereof |
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Address after: Longgang District of Shenzhen City, Guangdong province 518000 Ping Street in the community square Po Village building I No. 1, C building Patentee after: Shenzhen Square Silicone Co., Ltd. Address before: 518000 Guangdong city of Shenzhen province Nanshan District Shekou Sea Garden 8 Building 303 Patentee before: Shenzhen Square Silicone Materials Co., Ltd. |