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Preparation of methyl vinyl MQ resin for LED encapsulated strengthening

A methyl vinyl, LED encapsulation technology, applied in the field of organic resin preparation, can solve the problems of high price, limited scope of use, etc., and achieve the effects of simple operation, convenient industrialization, and mild conditions

Inactive Publication Date: 2008-12-17
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production of MQ silicone resin at home and abroad mainly uses tetraethyl orthosilicate as a raw material. Although the resulting product has excellent performance, it is expensive, which limits its application range.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 20mL of concentrated hydrochloric acid (36.5wt%) to a 250mL dry three-necked flask, stir rapidly at 40°C, add 60g of water glass with a solid content of 10wt% and a modulus of 1.33, hydrolyze for 50s, and then add dimethylvinylformazol A mixture of 3.1 g of oxysilane, 3.5 g of methylphenyldiethoxysilane, 17.7 g of hexamethyldisiloxane and 25 g of absolute ethanol, and add 50 mL of extractant hexamethyldisiloxane after 20 minutes of reaction, Heat up to 70°C and reflux for 4 hours, then stop the reaction, let stand to separate layers, take the upper oil layer, wash with deionized water until neutral, dry with anhydrous calcium chloride until clear and transparent, then raise the temperature to 145°C under normal pressure to recover most of the six Methyldisiloxane, and finally remove the low boilers at 145°C / -0.096MPa to obtain 8.4g of clear and transparent product MQ resin. The resulting product n D 25 =1.4615, GPC records number average molecular weight 0.41×10 ...

Embodiment 2

[0032] Add 20mL of concentrated hydrochloric acid (36.5wt%) to a 250mL dry three-necked flask, stir rapidly at 40°C, add 60g of water glass with a solid content of 10wt% and a modulus of 1.25, hydrolyze for 50s, and then add dimethylvinyl ethyl A mixture of 3.1g of oxysilane, 10g of methyldiphenylethoxysilane, 8.3g of decamethyltetrasiloxane and 25g of absolute ethanol. After reacting for 30min, add 50mL of extractant dixylene, heat up to 80°C and reflux 3h, then stop the reaction, let stand to separate the layers, take the upper oil layer, wash with deionized water until neutral, dry with anhydrous magnesium sulfate until clear and transparent, then raise the temperature to 145°C under normal pressure to recover most of the xylene, and finally at 145 Low boilers were removed at ℃ / -0.096MPa to obtain 20.2 g of clear and transparent MQ resin. The resulting product n D 25 =1.4750, the number average molecular weight measured by GPC is 0.31×10 4 , the molecular weight distribu...

Embodiment 3

[0034] Add 20mL of concentrated hydrochloric acid (36.5wt%) to a 250mL dry three-neck flask, stir rapidly at 50°C, add 60g of water glass with a solid content of 10% and a modulus of 1.35, hydrolyze for 50s, and then add 1,3-diethylene Dimethyl-1,1,3,3-tetramethyldisiloxane 5.1g, 1,3-dimethyl-1,1,3,3-tetraphenyl-disiloxane 18.9g and absolute ethanol 25g of the mixture, add 50mL of hexamethyldisiloxane after reacting for 80min, raise the temperature to 70°C and reflux for 2h, then stop the reaction, let stand to separate layers, take the upper oil layer, wash with deionized water until neutral, and use anhydrous chlorination Calcium is dried until clear and transparent, then the temperature is raised to 145°C under normal pressure to recover most of the hexamethyldisiloxane, and finally the low boilers are removed at 145°C / -0.096MPa to obtain 15.5g of clear and transparent product MQ resin. The resulting product n D 25 =1.4800, the number average molecular weight measured by ...

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Abstract

The invention discloses a preparation method of organic resin, in particular to a preparation method of a methyl vinyl MQ resin used for LED encapsulation and reinforcement. The method is that a soluble glass aqueous solution is added into concentrated hydrochloric acid (36.5 percent); after the reaction, the anhydrous ethanol solution of phenyl alkoxy silicane, vinyl alkoxy silicane and methyl alkoxy silicane is added; an extraction is carried out after cohydrolysis; the upper oil layer is removed; the reactants are washed to be neutral and dried; the low-boiling substances are removed; the colorless and transparent product of MQ resin is obtained. The preparation method of the invention has the advantages of accessible and cheap raw materials, simple and easy operation, and is convenient to industrialized with good effect. The products of the invention are especially suitable to be used as reinforcement materials in the LED encapsulation materials, also be expected as a reinforcing agent for other organosilicon materials and used in aspects of anchoring agent, surface treating agent, mold discharging agent, anti-blowing agent, adhesion preventives, brightening agent and other additives, etc.

Description

technical field [0001] The invention relates to a method for preparing an organic resin, in particular to a method for preparing a methyl vinyl MQ resin used for LED package reinforcement. technical background [0002] Since mankind entered the 21st century, the energy problem has become increasingly serious, and the energy situation in our country is also very severe. Saving energy is equally important as developing new energy, and saving energy is more economical and more environmentally friendly, and should be placed in the first place. At present, lighting accounts for about 20% of the world's total energy consumption. If low-efficiency, high-power-consumption traditional light sources can be replaced with low-energy, long-life, environmentally-friendly and safe light sources, it will undoubtedly bring about a worldwide lighting revolution. [0003] Ultra-high-brightness light-emitting diodes (Light Emitting Diode, LED) consume only 1 / 10 of the power of traditional lig...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06C08L83/04
Inventor 来国桥董红杨雄发伍川蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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