CN102718971A - Method for modifying methyl vinyl MQ silicon resin - Google Patents
Method for modifying methyl vinyl MQ silicon resin Download PDFInfo
- Publication number
- CN102718971A CN102718971A CN2012101919226A CN201210191922A CN102718971A CN 102718971 A CN102718971 A CN 102718971A CN 2012101919226 A CN2012101919226 A CN 2012101919226A CN 201210191922 A CN201210191922 A CN 201210191922A CN 102718971 A CN102718971 A CN 102718971A
- Authority
- CN
- China
- Prior art keywords
- silicone resin
- stirring
- methyl vinyl
- silicon resin
- modifying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a method for modifying methyl vinyl MQ silicon resin, in particular to a method for modifying methyl vinyl MQ silicon resin for reinforcing LED (light-emitting diode) packaging, which comprises the following steps: adding 30-60 mass portions of organic solvent and 10-20 mass portions of blocking agent into 100 mass portions of silicon resin; stirring the mixture at 80-100 DEG C until the silicon resin is dissolved; adding 0.05-0.1 mass portions of catalyst; stopping heating and stirring after reaction for eight hours by stirring, and cooling to room temperature; opening the reaction vessel for stirring the reactant, adding 1.1-2 mass portions of alkaline inorganic salt powder, and stopping stirring after neutral reaction; and standing, filtering and evaporating, thereby obtaining the white powder solid which is modified silicon resin. The method provided by the invention has the advantages that the cost is low, the synthesis is easy, and a reinforcing agent prepared by the method can better meet the requirement of LED packaging material on the performance of the reinforcing agent.
Description
Technical field
The present invention relates to the method for a kind of methyl vinyl MQ silicone resin modification, particularly a kind of method that is used for the methyl vinyl MQ silicone resin modification of LED encapsulated strengthening.
Background technology
Along with the progressively enforcement of national semiconductor lighting plan, as the desirable reinforced filling of high-power LED encapsulation material with liquid silastic, the methyl vinyl MQ silicone resin shows out its vital role day by day especially.Organosilicon has characteristics such as transmittance height, specific refractory power are big, Heat stability is good, stress is little, water absorbability is low, and its performance is superior to epoxy resin far away.The white light LEDs packaged material not only needs higher transmittance, specific refractory power, also need certain tensile strength and hardness, and reinforcement Zylox physical strength is very not low, and wanting has good physical strength, just needs reinforced filling.And organosilicon LED packaged material requires high refractive index, high transmission rate and bigger tensile strength, higher hardness, and this just has higher requirement to reinforced filling.The main method of producing the methyl vinyl MQ silicone resin at present is water glass method and silicon ester method, and synthesis technique is more loaded down with trivial details, and the contents of ethylene of the methyl vinyl MQ silicone resin of gained is lower, and contents of ethylene is not easy control, and post-processed is complicated.
Summary of the invention
Technical problem to be solved by this invention is can make on the basis of LED encapsulation to the supporting material high performance requirements satisfied, and the methyl vinyl MQ silicone resin method of modifying that a kind of contents of ethylene is high and be easy to control is provided.
The technical scheme that the present invention solves the problems of the technologies described above is following: to mass parts is that to add mass parts in 100 parts the silicone resin be 30～60 parts organic solvent and the end-capping reagent that mass parts is 10～20 parts, under 80 ℃～100 ℃ temperature, is stirred to silicone resin and dissolves; The adding mass parts is 0.05～0.1 part a catalyzer, after 8 hours, stops heating and stirring through stirring reaction, is cooled to room temperature; Open and stir, the adding mass parts is 1.1～2 parts an alkaline, inorganic salts powder, carries out stopping to stir after the neutralization reaction; Leave standstill, filter, evaporate, obtain the white powder solid and be modified silicone resin
The invention has the beneficial effects as follows: cost of the present invention is low, easy to be synthetic, can be good at satisfying the performance requriements of LED packaged material high transmission rate, high refractive index, high tensile, high firmness with the strengthening agent of its preparation.
On the basis of technique scheme, the present invention can also do following improvement.
Further, said silicone resin is methyl MQ silicone resin or methyl vinyl MQ silicone resin.
Further, said organic solvent is toluene or YLENE.
Further, said organic solvent preferably uses YLENE.
Further, said end-capping reagent is 1,3-divinyl-1,1,3,3-tetramethyl disiloxane.
Further, said catalyzer is an an acidic catalyst.
Further, said an acidic catalyst is any one or a few the mixing in trifluoromethanesulfonic acid, tosic acid resin or the perfluorinated sulfonic resin.
Further, said an acidic catalyst preferably uses trifluoromethanesulfonic acid.
Further, said alkaline, inorganic salts powder is any one or a few the mixing in lime carbonate, yellow soda ash, sodium hydrogencarbonate or the salt of wormwood.
Further, said alkaline, inorganic salts powder preferably uses lime carbonate.
Embodiment
Below principle of the present invention and characteristic are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
Embodiment 1
In the there-necked flask of being furnished with whisking appliance, TM and prolong, add 100g methyl MQ silicone resin, 50g YLENE and 20g1,3-divinyl-1,1; 3; The 3-tetramethyl disiloxane is stirred to methyl MQ silicone resin and dissolves fully under 90 ℃ temperature, add the 0.08g trifluoromethanesulfonic acid again; Stirring reaction stopped heating and stirring after 8 hours then.To be cooled to room temperature, to open and stir, adding 1.6g lime carbonate carries out neutralization reaction, stirs to stop after 8 hours stirring, and leaves standstill, and filters with the malleation strainer.Shift at last and filtrate to the pyriform flask, decompression steams low-boiling-point substance, obtains the white powder solid, it is dissolved in the deuterochloroform, with
1H NMR measures, and contents of ethylene is 4.8% (massfraction); Use GPC to measure number-average molecular weight and be 4500g/mol.
Embodiment 2
In the there-necked flask of being furnished with whisking appliance, TM and prolong, add 100g methyl vinyl MQ silicone resin, 60g toluene and 15g1,3-divinyl-1,1; 3; The 3-tetramethyl disiloxane is stirred to the methyl vinyl MQ silicone resin and dissolves fully under 85 ℃ temperature, add the mixture of 0.1g tosic acid and tosic acid again; Stirring reaction stopped heating and stirring after 8 hours then.To be cooled to room temperature, to open and stir, adding 2.0g yellow soda ash and sodium hydrogencarbonate carry out neutralization reaction, stir to stop after 8 hours stirring, and leave standstill, and filter with the malleation strainer.Shift at last and filtrate to the pyriform flask, decompression steams low-boiling-point substance, obtains the white powder solid, it is dissolved in the deuterochloroform, with
1H NMR measures, and contents of ethylene is 4.6% (massfraction); Use GPC to measure number-average molecular weight and be 4400g/mol.
Embodiment 3
In the there-necked flask of being furnished with whisking appliance, TM and prolong, add 100g methyl vinyl MQ silicone resin, 30g toluene and 10g1,3-divinyl-1,1; 3; The 3-tetramethyl disiloxane is stirred to the methyl vinyl MQ silicone resin and dissolves fully under 80 ℃ temperature, add the 0.05g perfluorinated sulfonic resin again; Stirring reaction stopped heating and stirring after 8 hours then.To be cooled to room temperature, to open and stir, the mixture of adding 1.1g yellow soda ash, salt of wormwood and lime carbonate carries out neutralization reaction, stirs to stop after 8 hours stirring, and leaves standstill, and filters with the malleation strainer.Shift at last and filtrate to the pyriform flask, decompression steams low-boiling-point substance, obtains the white powder solid, it is dissolved in the deuterochloroform, with
1H NMR measures, and contents of ethylene is 4.2% (massfraction); Use GPC to measure number-average molecular weight and be 4100g/mol.
Embodiment 4
In the there-necked flask of being furnished with whisking appliance, TM, prolong, add 100g methyl MQ silicone resin, 50g YLENE, 16g1; 3-divinyl-1,1,3; The 3-tetramethyl disiloxane is stirred to methyl MQ silicone resin at 88 ℃ and dissolves fully, adds the mixture of 0.08g trifluoromethanesulfonic acid, tosic acid and perfluorinated sulfonic acid again; Stirring reaction stopped heating and stirring after 8 hours then.Then open and stir, adding 1.6g salt of wormwood carries out neutralization reaction, stirs to stop after 8 hours stirring, and leaves standstill, and filters with the malleation strainer.Transfer is filtrated to the pyriform flask, and decompression steams low-boiling-point substance, obtains the white powder solid, it is dissolved in the deuterochloroform, with
1H NMR measures, and contents of ethylene is 4.6% (massfraction); Use GPC to measure number-average molecular weight and be 4300g/mol.
Comparative Examples
At 180gSiO
2Content is in the water glass (aqueous solution of water glass) of 17.8% (massfraction), adds the dilution of 200g water, then under violent stirring, is injected into 100g mass concentration concentration fast and is in 35%～38% the hydrochloric acid, adds 12.6gViMe then
2SiOC
2H
5, 14.8g (Me
3Si)
2O and 200g ethanol, and under 50～60 ℃, reacted 30 minutes.Add 300g (Me again
3Si)
2The O dilution, and keep and stirred 1 hour.Standing demix removes sub-cloud sour water ethanolic soln then.Oil phase under agitation adds the 30g mass concentration greater than 70% the vitriol oil, at room temperature stirs 2h, and standing demix is discharged the acid layer again, and the resin solution water is washed till neutrality, and is dry through Calcium Chloride Powder Anhydrous, steams (Me
3Si)
2O obtains the methyl vinyl MQ silicone resin of water white transparency, contents of ethylene 2.5%～3.0% (massfraction).
It is thus clear that; The defective that method of modifying provided by the invention has overcome that synthesis technique is more loaded down with trivial details, the contents of ethylene of gained methyl vinyl MQ silicone resin is lower, contents of ethylene is not easy to control, post-processed is complicated; Using methyl vinyl MQ silicone resin clear, the contents of ethylene of method of modifying preparation according to the invention is 3%～5% (massfraction), and molecular weight is 3000～5000g/mol.Be suitable as LED packaged material strengthening agent.
The above is merely preferred embodiment of the present invention, and is in order to restriction the present invention, not all within spirit of the present invention and principle, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. the method for methyl vinyl MQ silicone resin modification; It is characterized in that comprising: to mass parts is that to add mass parts in 100 parts the silicone resin be 30～60 parts organic solvent and the end-capping reagent that mass parts is 10～20 parts, under 80 ℃～100 ℃ temperature, is stirred to silicone resin and dissolves; The adding mass parts is 0.05～0.1 part a catalyzer, after 8 hours, stops heating and stirring through stirring reaction, is cooled to room temperature; Open and stir, the adding mass parts is 1.1～2 parts an alkaline, inorganic salts powder, carries out stopping to stir after the neutralization reaction; Leave standstill, filter, evaporate, obtain the white powder solid and be modified silicone resin.
2. method of modifying according to claim 1 is characterized in that, said silicone resin is methyl MQ silicone resin or methyl vinyl MQ silicone resin.
3. method of modifying according to claim 1 is characterized in that, said organic solvent is toluene or YLENE.
4. method of modifying according to claim 1 is characterized in that, said end-capping reagent is 1,3-divinyl-1,1,3,3-tetramethyl disiloxane.
5. method of modifying according to claim 1 is characterized in that, said catalyzer is an an acidic catalyst.
6. according to the method for modifying of claim 4 gained, it is characterized in that said an acidic catalyst is any one or a few the mixing in trifluoromethanesulfonic acid, tosic acid resin or the perfluorinated sulfonic resin.
7. method of modifying according to claim 1 is characterized in that, said alkaline, inorganic salts powder is any one or a few the mixing in lime carbonate, yellow soda ash, sodium hydrogencarbonate or the salt of wormwood.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101919226A CN102718971A (en) | 2012-06-11 | 2012-06-11 | Method for modifying methyl vinyl MQ silicon resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101919226A CN102718971A (en) | 2012-06-11 | 2012-06-11 | Method for modifying methyl vinyl MQ silicon resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102718971A true CN102718971A (en) | 2012-10-10 |
Family
ID=46944855
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101919226A Pending CN102718971A (en) | 2012-06-11 | 2012-06-11 | Method for modifying methyl vinyl MQ silicon resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102718971A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105873985A (en) * | 2014-01-08 | 2016-08-17 | 道康宁公司 | Method for capping mq-type silicone resins |
| CN106065073A (en) * | 2016-05-31 | 2016-11-02 | 上海回天新材料有限公司 | Vinyl polysiloxane, and its production and use |
| CN110591098A (en) * | 2019-10-09 | 2019-12-20 | 浙江新安化工集团股份有限公司 | Methyl phenyl vinyl silicone oil and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4774310A (en) * | 1986-06-28 | 1988-09-27 | Dow Corning, Ltd. | Method for making siloxane resins |
-
2012
- 2012-06-11 CN CN2012101919226A patent/CN102718971A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4774310A (en) * | 1986-06-28 | 1988-09-27 | Dow Corning, Ltd. | Method for making siloxane resins |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105873985A (en) * | 2014-01-08 | 2016-08-17 | 道康宁公司 | Method for capping mq-type silicone resins |
| CN105873985B (en) * | 2014-01-08 | 2019-02-12 | 美国陶氏有机硅公司 | Method for blocking MQ type organic siliconresin |
| CN106065073A (en) * | 2016-05-31 | 2016-11-02 | 上海回天新材料有限公司 | Vinyl polysiloxane, and its production and use |
| CN106065073B (en) * | 2016-05-31 | 2019-04-19 | 上海回天新材料有限公司 | Vinyl polysiloxane, and its preparation method and application |
| CN110591098A (en) * | 2019-10-09 | 2019-12-20 | 浙江新安化工集团股份有限公司 | Methyl phenyl vinyl silicone oil and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105906810B (en) | A kind of preparation method of organopolysiloxane resins | |
| CN105400446B (en) | A kind of high refractive index LED liquid casting glue tackifier and preparation method thereof | |
| CN103122149B (en) | Optical package high refractive index High-transparency silicon rubber and its preparation method | |
| CN101747860B (en) | Single component organic silicon packaging glue cured by ultraviolet for high-power LED | |
| CN101215381B (en) | Method for preparing methylphenyl hydrogen-containing silicone oil | |
| CN104004491B (en) | A kind of LED ultraviolet curing organic silicon packaging plastic and preparation method thereof | |
| CN104151558B (en) | Preparation method for MDTQ type methyl phenyl vinyl silicone resin | |
| CN102898650B (en) | MTQ silicon resin with T-chain unit containing phenyl and preparation method thereof | |
| CN101851333B (en) | Method for preparing methyl phenyl hydrogen-containing silicone oil by rare earth super acid catalysis | |
| CN103232601B (en) | Phenyl MDT silicon resin and preparation method thereof | |
| CN104974349B (en) | A kind of preparation method of silicones | |
| CN103012797A (en) | Preparation method of methyl phenyl vinyl silicone oil | |
| CN101885845B (en) | Method for synthesizing vinyl phenyl silicone oil | |
| CN102584884A (en) | Benzoxazine monomer, benzoxazine precursor and low-dielectric benzoxazine resin | |
| CN104892939B (en) | A kind of preparation method of phenyl polysiloxane | |
| CN102775612B (en) | Vinyl MQ silicon resin and preparation method thereof | |
| CN103951827B (en) | A kind of phenyl-based hydrogen-based MQ silicones and preparation method thereof | |
| CN104955900B (en) | Solidification compound and its solidfied material comprising polysiloxanes | |
| CN102718971A (en) | Method for modifying methyl vinyl MQ silicon resin | |
| CN101323667A (en) | Preparation of methyl vinyl MQ resin for LED encapsulated strengthening | |
| TW200914461A (en) | (Thio) phenoxy phenyl silane composition and method for making same | |
| CN103242531A (en) | Preparation method of phenyl hydrogen-containing MT silicone resin | |
| CN108300408B (en) | Organic silicon material for packaging LED with high luminous flux maintenance rate | |
| CN104031392A (en) | Addition-type silica gel, and preparation method and application thereof | |
| CN102660121A (en) | TiO2 semigel modified transparent silicon resin with high refractive index and preparation [method] thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20121010 |