CN103360603B - A kind of LED phenyl vinyl polysiloxane and preparation method thereof - Google Patents
A kind of LED phenyl vinyl polysiloxane and preparation method thereof Download PDFInfo
- Publication number
- CN103360603B CN103360603B CN201310250058.7A CN201310250058A CN103360603B CN 103360603 B CN103360603 B CN 103360603B CN 201310250058 A CN201310250058 A CN 201310250058A CN 103360603 B CN103360603 B CN 103360603B
- Authority
- CN
- China
- Prior art keywords
- phenyl
- led
- vinyl polysiloxane
- preparation
- phenyl vinyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to technical field of polymer materials, a kind of LED phenyl vinyl polysiloxane is provided, it comprises kernel and is cross-linked the soft segment outside kernel, wherein kernel is phenyl alkoxysilane polymkeric substance, and soft segment is at least one in the polydimethyldiphenylsiloxane of the polydimethylsiloxane of ethenyl blocking, the PSI of ethenyl blocking and ethenyl blocking.And the preparation method of above-mentioned LED phenyl vinyl polysiloxane is provided, method processing condition are gentle, simple, raw material sources are extensive, reproducible, the mechanical property such as product tensile strength, hardness after obtained phenyl vinyl polysiloxane solidification is better.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of LED phenyl vinyl polysiloxane and preparation method thereof.
Background technology
Power type light-emitting diode (LightEmittingDiode, LED) being is directly the device of luminous energy by electric energy conversion, with traditional incandescent light, luminescent lamp, the light sources such as high-intensity gas discharge lamp are compared, energy consumption is only 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 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, mark illumination, Landscape Lighting, big area picture and text showing full-color screen etc.
Traditional LED encapsulation material is bisphenol A-type or polyacrylie-type transparent epoxy resin, LED is applied to as patent US5998925, US6069440, US6608332, JP-A33241338 etc. describe epoxy resin respectively, but because epoxy resin easily turns to be yellow under uvioresistant illuminate condition, thermal resistance is high, low temperature becomes fragile, the defect such as easy to crack, along with the development of LED technology, also more and more higher to the various performance requriementss of packaged material, epoxy resin can not meet the requirement of LED to the performance such as heat, light, power of its packaged material.
The advantages such as organosilicon macromolecule material is as ageing-resistant in Silica hydrogel, silicon rubber, silicone resin etc. have, high-low temperature resistant, ultraviolet resistance radiation are packaged materials ideal at present.Wherein phenyl polysiloxane due to have high, the anti-ventilative water permeability of refractive index good, directly pour into, without the need to plastic casing, the advantage such as easy to use, has been widely used in the packaging procesies such as LED paster, Molding.Hydrosilylation is there is and to react and cross-linking vulcanized in the organosilicon polymer of phenyl polysiloxane and silicon-hydrogen bond containing under the effect of the metal catalyst such as platinum, cobalt, cure conditions is gentle, high-speed vulcanization is got final product under middle temperature, simultaneously the by product such as solvent-free, low molecule is discharged, bubble or trachoma is produced when avoiding sulfuration, and cured product water, shock, shock-resistance, thermal conductivity are good, are therefore well suited for LED.
Water is joined phenyl chlorosilane, vinyl end socket by patent US20040116640, US20050212008, take toluene as solvent, be hydrolyzed after being polymerized and wash layering again, removed under reduced pressure low molecule, obtain water white transparency product, because reaction monomers is organochlorosilane, a large amount of acid solution can be produced in reaction process, corrosion is caused to equipment, and the storage of raw material and the synthesis technique of product are made troubles, and there is no concentrated soft segment in the product of synthesis, excessive with product internal stress after hydrogeneous linking agent sulfuration, shock resistance is not good enough.
Patent TW201229496A adopts phenyl alkoxysilane to be raw material, with alkali as a catalyst, the phenyl vinyl polysiloxane of synthesis and the sulfuration under platinum catalyst of hydrogeneous linking agent, the product obtained cold cycling under-40 DEG C ~ 100 DEG C conditions is impacted and is not only ftractureed for 50 times.
CN1011787133 reports one phenyl or vinyl three-functionality-degree siloxanes and two functionality polysiloxane hydrolytic polymerization under hydrochloric acid catalysis, obtain a kind of method containing 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 acidic catalysis conditions, carry out the ring-closure reaction that head stings tail, easily make the ring body impurity being mixed with a small amount of low refractive index in product, easily make product muddy, and refractive index is on the low side, be applied to the transmission efficiency that LED will reduce its optical throughput.
Patent US200724979(A1) disclose and adopt two functional group's organopolysiloxane of chlorine end-blocking to be polymerized with phenyl-trichloro-silicane, vinyl end socket or hydrogeneous end socket cohydrolysis in toluene, obtain the solid silicon resin that molecular weight reaches 58000 ~ 62000, add the product after platinum sulfuration and can stand 100-50 DEG C/150 DEG C cold cycling impacts and not ftracture.But due to two functional group's organopolysiloxane segments and the disorderly and unsystematic state of three-dimensional silicone treated, as poor in tensile strength, tearing toughness with the product mechanical property after hydrogeneous linking agent sulfuration, and product relative molecular weight is large, in solid under normal temperature, greatly limit its application in LED, two functional group's organopolysiloxane raw material sources of chlorine end-blocking are few simultaneously, price.
Due to the technical development of LED, power is increasing, and thermal value is also increasing, therefore the thermal characteristics to packaged material, and particularly the requirement of cold-hot impact property is more and more harsher, as the impact of ability more than 1000 times at-40 DEG C ~ 110 DEG C.And by LED encapsulation material prepared by above-mentioned phenyl polysiloxane, excessive with internal stress after linking agent sulfuration, shock resistance is poor, be difficult to reach application requiring, and some product is solid-state at normal temperatures, is difficult to the requirement adapting to modern LED technique.
Summary of the invention
Technical problem to be solved by this invention is the defect overcoming prior art, provides a kind of LED phenyl vinyl polysiloxane and preparation method thereof.
The present invention realizes like this, a kind of LED phenyl vinyl polysiloxane, it comprises kernel and is cross-linked the soft segment outside kernel, wherein, kernel is phenyl alkoxysilane polymkeric substance, and soft segment is at least one in the polydimethyldiphenylsiloxane of the polydimethylsiloxane of ethenyl blocking, the PSI of ethenyl blocking and ethenyl blocking.
The present invention also provides the preparation method of above-mentioned LED phenyl vinyl polysiloxane, and it comprises the steps:
It is the water mixing of the phenyl alkoxysilane monomer of 1 ~ 100 part, the organic solvent of 10 ~ 50 parts and 20 ~ 40 parts by mass fraction, drip the acid catalyst of 0.1 ~ 10% phenyl alkoxysilane monomer mass, react 1 ~ 8 hour at 0 ~ 30 DEG C, obtain reaction solution A;
At least one in alkoxy end-capped polydimethylsiloxane, PSI, polydimethyldiphenylsiloxane is added in described reaction solution A, continue reaction and add vinyl closure agent after 3 ~ 10 hours, react 1 ~ 3 hour, obtain reaction solution B;
By described reaction solution B stratification, add alkali adjust ph after removing upper strata acid solution to neutral, washing, obtains mixture;
By mixture under vacuum tightness is equal to or higher than 0.1Mpa condition, be heated to 110 DEG C ~ 130 DEG C, obtain described phenyl vinyl polysiloxane.
The phenyl vinyl polysiloxane refractive index prepared by preparation method of LED phenyl vinyl polysiloxane of the present invention is high, 1.55/ DEG C can be reached), be liquid under normal temperature, be convenient to LED gluing process, fast with hydrogeneous linking agent vulcanization rate, and good with phenyl silicone oil compatibleness, non-whitening, become muddy, solidification rear surface is wrinkle resistant, without decorative pattern.Phenyl vinyl polysiloxane prepared by the present invention contains the soft segment of equivalent length, and not containing low refractive index impurity, and soft segment adds the condensation that is hydrolyzed again after formation inner core, the product mechanical property after crosslinking curing is as good in tensile strength, cold-and-heat resistent impact excellent.Manufacturing condition of the present invention is gentle, simple, and raw material sources are extensive, reproducible, and can adjust the parameters such as product viscosity, contents of ethylene, phenyl content according to actual needs, thus have adaptability widely.
Accompanying drawing explanation
Fig. 1 is the three-dimensional structure diagram of the LED phenyl vinyl polysiloxane of the embodiment of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, 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, be not intended to limit the present invention.
The invention provides a kind of LED phenyl vinyl polysiloxane, it comprises kernel and is cross-linked the soft segment outside kernel, wherein, kernel is phenyl alkoxysilane polymkeric substance, and soft segment is at least one in the polydimethyldiphenylsiloxane of the polydimethylsiloxane of ethenyl blocking, the PSI of ethenyl blocking and ethenyl blocking.
Wherein, preferably, the molecule of described phenyl vinyl polysiloxane link length is 5 ~ 50, phenyl mole number account for methyl, phenyl and vinyl total mole number and 0.4 ~ 0.8, 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 DEG C, and at 25 DEG C, viscosity is less than 30000mPa.s.
More specifically, the general structure of LED phenyl vinyl polysiloxane of the present invention 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 the span of a to be the span of 0.01 ~ 1, b be 0 ~ 0.1, c is the span of 0 ~ 0.8, d is 0 ~ 0.5, and the span of a+b+c>0, e is 0.1 ~ 0.4.Described LED phenyl vinyl polysiloxane is continuous print link, molecule link length is 5 ~ 50, the span of e is 0.1 ~ 0.4, and in all groups be directly connected with Siliciumatom, n (Ph)/n (Me+Ph+Vi) span is 0.4 ~ 0.8, when n (Vi)/n (Me+Ph+Vi) span is 0.1 ~ 0.4, product refractive index is at 1.53 ~ 1.55/20 DEG C, and at 25 DEG C, viscosity is less than 30000mPa.s.In three-dimensional arrangement, multiple (PhSiO
1.5)
aformed and concentrate T kernel, (Ph
2siO)
b(PhMeSiO)
c(Me
2siO)
dformed 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 phenyl vinyl polysiloxane, and it comprises the steps:
It is the water mixing of the phenyl alkoxysilane monomer of 1 ~ 100 part, the organic solvent of 10 ~ 50 parts and 20 ~ 40 parts by mass fraction, drip the acid catalyst of 0.1 ~ 10% phenyl alkoxysilane monomer mass, react 1 ~ 8 hour at 0 ~ 30 DEG C, obtain reaction solution A;
At least one in alkoxy end-capped polydimethylsiloxane, PSI, polydimethyldiphenylsiloxane is added in described reaction solution A, continue reaction and add vinyl closure agent after 3 ~ 10 hours, react 1 ~ 3 hour, obtain reaction solution B;
By described reaction solution B stratification, add alkali adjust ph after removing upper strata acid solution to neutral, washing, obtains mixture;
By mixture under vacuum tightness is equal to or higher than 0.1Mpa condition, be heated to 110 DEG C ~ 130 DEG C, obtain described phenyl vinyl polysiloxane.
Concrete principle is: first add by phenyl alkoxysilane monomer, hydrolytic condensation in acid condition, form fine and close kernel (T), add the appropriate soft segment concentrated containing D structure (polydimethylsiloxane or PSI) again, finally add vinyl closure agent again, obtain the phenyl vinyl polysiloxane product of three-dimensional arrangement as shown in Figure 1.
Particularly, described phenyl Alkoxy monomeric comprises at least one in phenyltrimethoxysila,e, phenyl triethoxysilane, dimethoxydiphenylsilane, diphenyl diethoxy silane, phenylbenzene methoxy-ethoxy-silane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane.
Described an acidic catalyst can select 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 one in tetramethyl divinyl disiloxane, diphenyldimethyl divinyl disiloxane, dimethylvinyl siloxane, phenylethylene radical siloxane, wherein, is preferably tetramethyl divinyl disiloxane.
Described alkyloxydimethicone is the polydimethylsiloxane of the end-blocking such as methoxyl group, oxyethyl group, or methoxyl group, the PSI of oxyethyl group end-blocking, at least one in 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 in and the alkali of surplus acid can select ammoniacal liquor, sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium bicarbonate etc.
The preparation method of LED phenyl vinyl polysiloxane provided by the invention, control product kernel size, viscosity, refractive index, contents of ethylene etc. by conditions such as raw material monomer proportioning, reaction times, temperature, pH value, thus obtain the LED glue of different hardness, mechanical strength with the hydrogeneous linking agent addition of corresponding phenyl.Compared with existing synthesis technique, LED phenyl vinyl polysiloxane shading rate obtained by the method is high, good fluidity, containing two functionality polysiloxane segments and the mechanical property such as tensile strength, hardness is better, be used for LED with the product of this products solidifying gained, its cold-and-heat resistent impact property is very excellent.
Embodiment 1:
To 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 dimethoxysilane, at 30 DEG C, drip 30 parts of massfractions is the hydrochloric acid of 25%, abundant stirring, dropwise in one hour, continue stirring again 2 ~ 3 hours, then to add 76.3g structure be CH
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 DEG C, add 111.6g tetramethyl-divinyl sily oxide, maintain the temperature at 80 DEG C, react after 10 hours and stop, layering again after being cooled to room temperature, add 5g sodium hydroxide neutralization, be washed to neutrality, at 110 DEG C, reduce pressure 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 DEG C, refractive index 1.5356/20 DEG C, contents of ethylene is 3.0%(m/m)
Embodiment 2:
To 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 dimethoxysilane, at 30 DEG C, dripping 30 parts of massfractions is again the hydrochloric acid of 25%, abundant stirring, dropwise in one hour, continue stirring again 2 ~ 3 hours, then to add 43g structure be CH
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 DEG C, add 223.2g tetramethyl-divinyl sily oxide, maintain the temperature at 80 DEG C, react after 10 hours and stop, layering again after being cooled to room temperature, add 5g sodium hydroxide neutralization, be washed to neutrality, at 110 DEG C, reduce pressure 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 DEG C, refractive index 1.5401/20 DEG C, contents of ethylene is 4.1%(m/m).
Comparative example 1:
To 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 dimethoxysilane, then to add 76.3g structure be CH
3o (CH
3)
2si [(OSi (CH
3)
2)]
18oSi (CH
3)
2oCH
3polydimethylsiloxane, 111.6g tetramethyl-divinyl sily oxide, at 30 DEG C, drip 30 parts of massfractions is the hydrochloric acid of 25%, be warming up to 80 DEG C, maintain the temperature at 80 DEG C, react after 10 hours and stop, layering again after being cooled to room temperature, add 5g sodium hydroxide neutralization, be washed to neutrality, at 110 DEG C, under the condition of vacuum tightness 0.9MPa ~ 1.0MPa, decompression is de-low 3 hours, obtain, water white transparency phenyl vinyl polysiloxane 391.5g, viscosity is 5000mPa.s/25 DEG C, refractive index 1.5326/20 DEG C, contents of ethylene is 2.5%(m/m).
Comparative example 2:
To 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 dimethoxysilane, add 65.87g dimethyldimethoxysil,ne again, 223.2g tetramethyl-divinyl sily oxide, at 30 DEG C, dripping 30 parts of massfractions is again the hydrochloric acid of 25%, abundant stirring, dropwise in one hour, be warming up to 80 DEG C, maintain the temperature at 80 DEG C, react after 10 hours and stop, be cooled to layering again after room temperature, add the neutralization of 5g sodium hydroxide, be washed to neutrality, at 110 DEG C, under the condition of vacuum tightness 0.9MPa-1.0MPa, decompression is de-low 3 hours, obtain water white transparency phenyl vinyl polysiloxane 388.2g, viscosity is 2300mPa.s/25 DEG C, refractive index 1.5396/20 DEG C, contents of ethylene is 3.4%(m/m).
Test the refractive index of the synthesized phenyl vinyl polysiloxane of refractive index test at the viscosity of synthesized phenyl vinyl polysiloxane at 25 DEG C and 20 DEG C respectively, referenced standard is respectively: DIN53019, GB/T614-2006.
Adopt the contents of ethylene of iodometric determination product, namely the product getting about 0.1g is dissolved in tetracol phenixin, add the iodine bromide IBr reagent of 10mL0.1mol/L again, fully after vibration, in the dark place 1 hour, then the liquor kalii iodide that 5mL concentration is 10% is added, fully vibrating, with the sodium thiosulfate standard solution titration of 0.1mol/L, take starch as index agent again, drop to blue disappearance and be terminal, do blank test simultaneously.
Contents of ethylene is calculated as follows:
Vinyl %=[CB × ((V0-V1)/2) × 27 × 100%]/(m × 1000)
In 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 solidification of Vinylphenyl silicon resin and the sign of cured product
Get a certain amount of synthesized Vinylphenyl silicon resin, adding appropriate 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, 3, the complex compound of 3-tetramethyl disiloxane and platinum, wherein platinum content is 50ppm, the isocyanuric acid ester Trimethoxy silane of 1% is adhesion promotor, the ethyl cyclohexanol of 0.01% is as cured modified dose, control product operable time, stir, deaeration is to transparent, steel die or the injection of injecting 2mm comprise GaN chip, PPA support, weld in the LED light emitting composition (5050 SMD lamp) of gold thread, cure conditions toasts 3 hours at 150 DEG C, obtain water white test piece or 5050 type Surface-mount LED lamp.
Mechanical property such as hardness, tensile strength, the elongation at break etc. of cured article can be tested by the test piece of gained, and reference standard is respectively D2204, D412.
Cold-and-heat resistent impact is tested
After carrying out cold cycling Impact Test 1000 times under 5050 made type Surface-mount LED lamp are placed in-40 DEG C of (30min) ~ 110 DEG C (30min), the cold-and-heat resistent impact property of cured article is judged with the whether dead lamp of Surface-mount LED lamp, if there is dead lamp situation, do not pass through, without dead lamp situation then by test.
Distinguish the phenyl vinyl polysiloxane 100g in Example 1 and 2 and comparative example 1 and 2, add appropriate (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 the isocyanuric acid ester Trimethoxy silane of about 1% is as adhesion promotor, and the ethyl cyclohexanol of 0.01% is as cured modified dose, be heating and curing at 150 DEG C 3 hours, test mechanical property, cold-and-heat resistent impact property, the anti-Gas permeability of the product obtained respectively by the method for reference example 2.Table 1 lists its accordingly result.
As can be seen from Table 1, the performance of the LED phenyl vinyl resin that embodiment 1 and embodiment 2 obtain is better than comparative example 1 and 2, again demonstrates the advantage that this soft segment is cross-linked kernel polymer materials.
Table 1
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a preparation method for LED phenyl vinyl polysiloxane, comprises the steps:
It is the water mixing of the phenyl alkoxysilane monomer of 1 ~ 100 part, the organic solvent of 10 ~ 50 parts and 20 ~ 40 parts by mass fraction, drip the acid catalyst of 0.1 ~ 10% phenyl alkoxysilane monomer mass, react 1 ~ 8 hour at 0 ~ 30 DEG C, obtain reaction solution A;
At least one in alkoxy end-capped polydimethylsiloxane, PSI, polydimethyldiphenylsiloxane is added in described reaction solution A, continue reaction and add vinyl closure agent after 3 ~ 10 hours, react 1 ~ 3 hour, obtain reaction solution B;
By described reaction solution B stratification, add alkali adjust ph after removing upper strata acid solution to neutral, washing, obtains mixture;
By mixture under vacuum tightness is equal to or higher than 0.1MPa condition, be heated to 110 DEG C ~ 130 DEG C, obtain described phenyl vinyl polysiloxane.
2. the preparation method of LED phenyl vinyl polysiloxane according to claim 1, it is characterized in that, described phenyl Alkoxy monomeric is at least one in phenyltrimethoxysila,e, phenyl triethoxysilane, dimethoxydiphenylsilane, diphenyl diethoxy silane, phenylbenzene methoxy-ethoxy-silane, aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane.
3. the preparation method of LED phenyl vinyl polysiloxane according to claim 1, it is characterized in that, described an acidic catalyst is at least one in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, perchloric acid, Hydrogen bromide, hydroiodic acid HI fluoroform alkanoic acid, strong acidic ion resin.
4. the preparation method of LED phenyl vinyl polysiloxane according to claim 3, is characterized in that, described an acidic catalyst is hydrochloric acid.
5. the preparation method of LED phenyl vinyl polysiloxane according to claim 1, it is characterized in that, described vinyl closure agent is at least one in tetramethyl divinyl disiloxane, diphenyldimethyl divinyl disiloxane, dimethylvinyl siloxane, phenylethylene radical siloxane.
6. the preparation method of LED phenyl vinyl polysiloxane according to claim 5, is characterized in that, described vinyl closure agent is tetramethyl divinyl disiloxane.
7. the preparation method of LED phenyl vinyl polysiloxane according to claim 1, is characterized in that, described solvent is at least one in varsol, ketones solvent, alcoholic solvent, esters solvent.
8. the preparation method of LED phenyl vinyl polysiloxane according to claim 1, is characterized in that, described alkali is at least one in ammoniacal liquor, sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium bicarbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310250058.7A CN103360603B (en) | 2013-06-21 | 2013-06-21 | A kind of LED phenyl vinyl polysiloxane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310250058.7A CN103360603B (en) | 2013-06-21 | 2013-06-21 | A kind of LED phenyl vinyl polysiloxane and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103360603A CN103360603A (en) | 2013-10-23 |
| CN103360603B true CN103360603B (en) | 2015-12-23 |
Family
ID=49362920
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310250058.7A Active CN103360603B (en) | 2013-06-21 | 2013-06-21 | A kind of LED phenyl vinyl polysiloxane and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103360603B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177619B (en) * | 2014-08-04 | 2017-05-31 | 深圳市明粤科技有限公司 | The synthesis method of organic silicon resin of LED encapsulation core shell structures |
| 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 |
| 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 |
| CN108369927B (en) * | 2015-11-27 | 2021-06-11 | 三菱电机株式会社 | Power semiconductor device |
| CN107828057B (en) * | 2017-11-13 | 2021-01-29 | 唐山三友硅业有限责任公司 | Preparation method and application of siloxane modified epoxy resin for LED packaging |
| 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 |
| 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 |
| CN115975596B (en) * | 2023-03-20 | 2023-07-18 | 淄博国创中心先进车用材料技术创新中心 | Double-component organic silicon pouring sealant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101875724A (en) * | 2009-04-30 | 2010-11-03 | 东莞市贝特利新材料有限公司 | Preparation method of phenyl silicone resin |
| CN102898651A (en) * | 2012-10-25 | 2013-01-30 | 浙江润禾有机硅新材料有限公司 | Preparation method of vinylphenyl silicon resin for LED (light-emitting diode) packaging |
-
2013
- 2013-06-21 CN CN201310250058.7A patent/CN103360603B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101875724A (en) * | 2009-04-30 | 2010-11-03 | 东莞市贝特利新材料有限公司 | Preparation method of phenyl silicone resin |
| CN102898651A (en) * | 2012-10-25 | 2013-01-30 | 浙江润禾有机硅新材料有限公司 | Preparation method of vinylphenyl silicon resin for LED (light-emitting diode) packaging |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103360603A (en) | 2013-10-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103360603B (en) | A kind of LED phenyl vinyl polysiloxane and preparation method thereof | |
| CN102391529B (en) | Preparation method of silicone resin type organic/inorganic hybrid material for packaging | |
| CN101475689B (en) | Preparation of methyl phenyl vinyl silicon resin | |
| CN102181159B (en) | Polysilsesquioxane reinforced light emitting diode (LED) encapsulation organic silicon rubber and preparation method thereof | |
| CN101215381B (en) | Method for preparing methylphenyl hydrogen-containing silicone oil | |
| CN101343365A (en) | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED | |
| CN105400446B (en) | A kind of high refractive index LED liquid casting glue tackifier and preparation method thereof | |
| CN103342816B (en) | A kind of organic siliconresin and curable organopolysiloxane composition and application | |
| CN102504270B (en) | High-performance organic silicon electronic pouring sealant and preparation method and application thereof | |
| KR102067384B1 (en) | Solid state light and method of forming | |
| US20120083056A1 (en) | Light emitting diode sealing member and method for producing light emitting diode device | |
| JP2010265437A (en) | Composition for thermosetting silicone resin | |
| CN104448318B (en) | A kind of MDQ type phenyl vinyl polysiloxane and preparation method thereof | |
| US8952108B2 (en) | Organic silicon compound, thermosetting composition containing said organic silicon compound, and sealing material for optical semiconductor | |
| CN104262970A (en) | Silicone Composition For Producing Transparent Silicone Materials And Optical Devices | |
| CN101426835A (en) | Curable resin composition | |
| CN105802532A (en) | Silicon boron tackifier, preparation method thereof and application thereof in double-component LED packaging gel | |
| CN103059306B (en) | High-refractive index transparent silicone resin and preparation method thereof | |
| CN102268186A (en) | Composition for thermosetting silicone resin | |
| CN102190888B (en) | Composition for thermosetting silicone resin | |
| CN104073215A (en) | Preparation method for nano silicon dioxide modified organic silicon sealant for packaging of light emitting diode (LED) | |
| CN102532900B (en) | Organosilicon lens material for power type light-emitting diode (LED) packaging | |
| CN105860083A (en) | Methods for preparing modified vinyl silicone resin and organosilicone sealing compound containing modified vinyl silicone resin | |
| CN106751893A (en) | A kind of refractive power LED encapsulation add-on type liquid silicon rubbers high and preparation method thereof | |
| CN101619170A (en) | Preparation and application of silica gel for LED packaging |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
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. |