CN106854282A - A kind of preparation of methyl ethylene silane resin - Google Patents
A kind of preparation of methyl ethylene silane resin Download PDFInfo
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- CN106854282A CN106854282A CN201510898896.4A CN201510898896A CN106854282A CN 106854282 A CN106854282 A CN 106854282A CN 201510898896 A CN201510898896 A CN 201510898896A CN 106854282 A CN106854282 A CN 106854282A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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Abstract
The present invention relates to a kind of preparation of methyl ethylene silane resin, including：41-43g tetraethyl orthosilicates, 8g toluene, 9g HMDOs, 3g tetramethyl divinyl disiloxanes, 10-20g absolute ethyl alcohols, 1.4g concentrated hydrochloric acids are added in equipped with agitator, thermometer, the there-necked flask of condenser pipe（wt%=36%）；And 15g water is added dropwise with the speed of 1d/s in ice-water bath, and 5min is stirred after dripping off, it is warming up to 35 DEG C of initial reaction 25-40min；System temperature is risen into 78 DEG C of reaction 4h, stops reaction, add 1.43gNaHCO3, and be warming up to 125 DEG C and steam water and ethanol.Back flow reaction 4h at this temperature after having steamed, is subsequently added 0.3g HMDOs and reacts 1h at this temperature, and washing is until PH=7.The filtrate of water white transparency is filtrated to get, by filtrate transfer filtrate to pear-shaped flask, decompression steams the low-boiling-point substances such as dimethylbenzene, obtains methyl ethylene silane resin.
Description
Technical field
The present invention relates to a kind of preparation of methyl ethylene silane resin, belong to synthesis chemical field.
Background technology
Organosilicon LED packaging plastics have excellent heat resistance, UV resistance, radiation resistance, do index of refraction, high transparency and good mechanical property etc., are highly suitable for the encapsulation of LED especially great power LEDs.At present, many characteristics of organosilicon LED encapsulation material make its reinforced filling to itself propose requirement higher.And increasingly manifest as the critical role of the reinforced filling-methyl vinyl MQ silicon resin of high-power LED encapsulation material liquid silastic.The main method of production methyl vinyl MQ silicon resin is sodium metasilicate method and silicic acid ester process at present, two methods respectively have advantage and disadvantage, the general character for generally occurring is mainly the more difficult control of molecular weight of the methyl vinyl MQ silicon resin of gained, and substantial amounts of unreacted Si-OH and Si-OR is contained in molecule（R is Me, Et etc.）Group, immiscible with LED encapsulating compound each components, muddy, contents of ethylene is low.So that the organosilicon encapsulating compound light transmittance that this resin for producing carries out reinforcement is poor, low intensity, Storage period there are problems that it is great.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation of methyl ethylene silane resin, and technical scheme is as follows：41-43g tetraethyl orthosilicates, 8g toluene, 9g HMDOs, 3g tetramethyl divinyl disiloxanes, 10-20g absolute ethyl alcohols, 1.4g concentrated hydrochloric acids are added in equipped with agitator, thermometer, the there-necked flask of condenser pipe（wt%=36%）；And 15g water is added dropwise with the speed of 1d/s in ice-water bath, and 5min is stirred after dripping off, it is warming up to 35 DEG C of initial reaction 25-40min；System temperature is risen into 78 DEG C of reaction 4h, stops reaction, add 1.43gNaHCO3, and be warming up to 125 DEG C and steam water and ethanol.Back flow reaction 4h at this temperature after having steamed, is subsequently added 0.3g HMDOs and reacts 1h at this temperature, and washing is until PH=7.The filtrate of water white transparency is filtrated to get, by filtrate transfer filtrate to pear-shaped flask, decompression steams the low-boiling-point substances such as dimethylbenzene, obtains methyl ethylene silane resin.
The beneficial effects of the invention are as follows：Synthesis process is simple, be easily controlled, it is not necessary to use special equipment, solvent-free, low production cost and product purpose is extensive.
Specific embodiment
Principle of the invention and feature are described below, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment
1
42g tetraethyl orthosilicates, 8g toluene, 9g HMDOs, 3g tetramethyl divinyl disiloxanes, 15g absolute ethyl alcohols, 1.4g concentrated hydrochloric acids are added in equipped with agitator, thermometer, the there-necked flask of condenser pipe（wt%=36%）；And 15g water is added dropwise with the speed of 1d/s in ice-water bath, and 5min is stirred after dripping off, it is warming up to 35 DEG C of initial reaction 30min；System temperature is risen into 78 DEG C of reaction 4h, stops reaction, add 1.43gNaHCO3, and be warming up to 125 DEG C and steam water and ethanol.Back flow reaction 4h at this temperature after having steamed, is subsequently added 0.3g HMDOs and reacts 1h at this temperature, and washing is until PH=7.The filtrate of water white transparency is filtrated to get, by filtrate transfer filtrate to pear-shaped flask, decompression steams the low-boiling-point substances such as dimethylbenzene, obtains methyl ethylene silane resin.
Embodiment
2
43g tetraethyl orthosilicates, 8g toluene, 9g HMDOs, 3g tetramethyl divinyl disiloxanes, 20g absolute ethyl alcohols, 1.4g concentrated hydrochloric acids are added in equipped with agitator, thermometer, the there-necked flask of condenser pipe（wt%=36%）；And 15g water is added dropwise with the speed of 1d/s in ice-water bath, and 5min is stirred after dripping off, it is warming up to 35 DEG C of initial reaction 40min；System temperature is risen into 78 DEG C of reaction 4h, stops reaction, add 1.43gNaHCO3, and be warming up to 125 DEG C and steam water and ethanol.Back flow reaction 4h at this temperature after having steamed, is subsequently added 0.3g HMDOs and reacts 1h at this temperature, and washing is until PH=7.The filtrate of water white transparency is filtrated to get, by filtrate transfer filtrate to pear-shaped flask, decompression steams the low-boiling-point substances such as dimethylbenzene, obtains methyl ethylene silane resin.
Embodiment
3
41g tetraethyl orthosilicates, 8g toluene, 9g HMDOs, 3g tetramethyl divinyl disiloxanes, 10g absolute ethyl alcohols, 1.4g concentrated hydrochloric acids are added in equipped with agitator, thermometer, the there-necked flask of condenser pipe（wt%=36%）；And 15g water is added dropwise with the speed of 1d/s in ice-water bath, and 5min is stirred after dripping off, it is warming up to 35 DEG C of initial reaction 25min；System temperature is risen into 78 DEG C of reaction 4h, stops reaction, add 1.43gNaHCO3, and be warming up to 125 DEG C and steam water and ethanol.Back flow reaction 4h at this temperature after having steamed, is subsequently added 0.3g HMDOs and reacts 1h at this temperature, and washing is until PH=7.The filtrate of water white transparency is filtrated to get, by filtrate transfer filtrate to pear-shaped flask, decompression steams the low-boiling-point substances such as dimethylbenzene, obtains methyl ethylene silane resin.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc. should be included within the scope of the present invention.
Claims (3)
1. a kind of preparation of methyl ethylene silane resin, characterized in that, adding 41-43g tetraethyl orthosilicates, 8g toluene in equipped with agitator, thermometer, the there-necked flask of condenser pipe, 9g HMDOs, 3g tetramethyl divinyl disiloxanes, 10-20g absolute ethyl alcohols, 1.4g concentrated hydrochloric acids；And 15g water is added dropwise with the speed of 1d/s in ice-water bath, and 5min is stirred after dripping off, it is warming up to 35 DEG C of initial reaction 25-40min；System temperature is risen into 78 DEG C of reaction 4h, stops reaction, add 1.43gNaHCO3And be warming up to 125 DEG C and steam water and ethanol, back flow reaction 4h at this temperature after having steamed, it is subsequently added 0.3g HMDOs and reacts 1h at this temperature, washing is filtrated to get the filtrate of water white transparency up to PH=7, by filtrate transfer filtrate to pear-shaped flask, decompression steams the low-boiling-point substances such as dimethylbenzene, obtains methyl ethylene silane resin.
2. the preparation method according to belonging to claim 1, it is characterised in that reactant is tetramethyl divinyl disiloxane.
3. the preparation method according to belonging to claim 1, it is characterised in that concentration of hydrochloric acid is 36%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510898896.4A CN106854282A (en) | 2015-12-09 | 2015-12-09 | A kind of preparation of methyl ethylene silane resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510898896.4A CN106854282A (en) | 2015-12-09 | 2015-12-09 | A kind of preparation of methyl ethylene silane resin |
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| CN106854282A true CN106854282A (en) | 2017-06-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510898896.4A Pending CN106854282A (en) | 2015-12-09 | 2015-12-09 | A kind of preparation of methyl ethylene silane resin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286671A (en) * | 2017-07-05 | 2017-10-24 | 东莞市联洲知识产权运营管理有限公司 | A kind of hydrophobic enhanced heat vulcanized silicone rubber and preparation method thereof |
| CN109280535A (en) * | 2018-09-12 | 2019-01-29 | 烟台德邦先进硅材料有限公司 | A kind of preparation method of functionality methyl vinyl MQ resin |
| CN114262438A (en) * | 2021-12-30 | 2022-04-01 | 合盛硅业股份有限公司 | Method for preparing powder MQ silicon resin |
-
2015
- 2015-12-09 CN CN201510898896.4A patent/CN106854282A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286671A (en) * | 2017-07-05 | 2017-10-24 | 东莞市联洲知识产权运营管理有限公司 | A kind of hydrophobic enhanced heat vulcanized silicone rubber and preparation method thereof |
| CN109280535A (en) * | 2018-09-12 | 2019-01-29 | 烟台德邦先进硅材料有限公司 | A kind of preparation method of functionality methyl vinyl MQ resin |
| CN109280535B (en) * | 2018-09-12 | 2020-11-10 | 烟台德邦科技有限公司 | Preparation method of functional methyl vinyl resin |
| CN114262438A (en) * | 2021-12-30 | 2022-04-01 | 合盛硅业股份有限公司 | Method for preparing powder MQ silicon resin |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170616 |
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| WD01 | Invention patent application deemed withdrawn after publication |