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Preparation method of phenyl-based hydrogen-based silicone resin for encapsulating LED

A technology of LED packaging and phenyltriethoxysilane, which is applied in chemical instruments and methods, electrical components, and other chemical processes, can solve the problems of low viscosity of hydrogen-containing silicone oil, difficulty in obtaining rings, and large amounts of hydrochloric acid. Achieve the effect of high refractive index and simple and feasible preparation method

Inactive Publication Date: 2010-11-24
SHENZHEN ANPIN SILICONE MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses chlorosilane as a raw material, and a large amount of hydrochloric acid will be produced in the production, which needs to be recycled, otherwise it will cause serious pollution to the environment
Chinese patent application CN101215381A reports the preparation of hydrogen-containing silicone oil by ring-opening such as hydrogen-containing ring body and methylphenyl ring body. as crosslinking agent

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0027] The preparation method of the present invention comprises the following steps carried out in sequence:

[0028] (A) Mix alkoxysilane, end-capping agent, solvent and catalyst, stir at 40°C to 50°C and add water dropwise for reaction, after the dropwise addition, continue to react at 50°C for 1 to 3 hours;

[0029] (B), add hydroalkoxysilane and / or hydrosiloxane, add acetic acid dropwise under stirring, after the drop is completed, heat up to 50°C-80°C to carry out polycondensation polymerization for 1-3 hours;

[0030] (C), add solvent and water and stir to mix, then stand still and separate the organic layer and the water layer, wash the separated organic layer repeatedly to neutrality and then dry, then distill under reduced pressure to remove low molecular weight.

[0031] Different types of phenylhydrogen silicone resins can be prepared by selecting different raw materials. For example, in step (A), alkoxysilanes include phenyltrimethoxysilane, phenyltriethoxysilane,...

Embodiment 1

[0039] Accurately weigh 400g of toluene, 27.6g of triphenylsilanol, 12g of dimethyldimethoxysilane, 475.2g of phenyltrimethoxysilane, and 0.40g of trifluoromethanesulfonic acid into a 2L four-necked flask, and place at 40°C Add water dropwise while stirring to react, the amount of water to be added dropwise is 43.2g, after the dropwise addition, heat to 50°C to continue the reaction for 3 hours, then add 107.2g of tetramethyldisiloxane, stir and add 100g of acetic acid dropwise, after the dropwise , reacted at 50°C for 3 hours, cooled to room temperature, added toluene and water, mixed well, then stood still and separated the organic layer and the water layer, washed the separated organic layer repeatedly until neutral, then dried, and then reduced pressure Low molecules such as solvents are removed by distillation. Get (PhSiO 3 / 2 ) 0.57 (Me 2 SiO) 0.025 (Ph 3 SiO 1 / 2 ) 0.025 (HMe 2 SiO 1 / 2 ) 0.38 High phenyl vinyl hydrogen silicone resin 365g, viscosity 7500mPa·s (2...

Embodiment 2

[0041] Accurately weigh 400g of toluene, 55.2g of triphenylsilanol, 24.4g of diphenyldimethoxysilane, 475.2g of phenyltrimethoxysilane and 0.40g of trifluoromethanesulfonic acid and add them to a 2L four-necked flask. Add water dropwise while stirring at ℃, the amount of water to be added is 43.2g, after the dropwise addition, heat to 50°C to continue the reaction for 1.5 hours, then add 107.2g of tetramethyldisiloxane, stir and add 100g of acetic acid dropwise, dropwise Afterwards, heat up to 80°C to react for 2 hours, cool to room temperature, add toluene and water, mix thoroughly, then let stand and separate the organic layer and the water layer, wash the separated organic layer repeatedly until neutral, then dry, then reduce Pressure distillation to remove low molecular weight. Get (PhSiO 3 / 2 ) 0.56 (Ph 2 SiO) 0.02 (Ph 3 SiO 1 / 2 ) 0.05 (HMe 2 SiO 1 / 2 ) 0.37 376g of phenylhydrogen silicone resin, the viscosity is 9300mPa·s (25°C), and the refractive index is 1.541...

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Abstract

The invention relates to a preparation method of phenyl-based hydrogen-based silicone resin for encapsulating LED. The preparation method comprises the following steps of: (A) mixing alkoxy silane, blocking agent, solvent and catalyst, stirring the mixture at the temperature of 40 DEG C to 50 DEG C, dropwise adding water for reaction, and making the mixture continue to react for 1 to 3 hours at the temperature of 50 DEG C; (B) adding hydrogen-based alkyl oxygen-based silicon and / or hydrogen-based siloxane, stirring and dropwise adding acetic acid, and raising the temperature to 50 DEG C to 80 DEG C to carry out condensation polymerization for 1 to 3 hours; and (C) adding solvent and water and stirring for mixing, standing the mixture, separating an organic layer and a water layer, repeatedly washing the separated organic layer until the separated organic layer is neutral, drying decompressing and distilling to remove low molecular weight. In the method, hydrogen chloride and other by-products which are not easy to recover for processing are not produced, silicone resin with any appropriate viscosity and phenyl content can be produced, and the hydrogen content of the silicone resin can be adjusted.

Description

technical field [0001] The invention relates to a preparation method of an organic silicon resin, in particular to a preparation method of a phenylhydrogen-based silicone resin used as a light-emitting diode (LED) packaging material. Background technique [0002] Nowadays, LEDs are widely used in a wide range of fields. For example, electronic products, home appliances, automobiles, traffic signs, billboards, etc., which require point or area light sources, are all LED application markets. As the fourth-generation electric light source, high-power LED has excellent characteristics such as small size, safe low voltage, long life, high electro-optical conversion efficiency, fast response, energy saving, and environmental protection, and is even called "green lighting source". [0003] The LED packaging structure and process are complex, which directly affects the performance and life of the LED. The packaging materials used in it have been a research hotspot in recent years. ...

Claims

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Application Information

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IPC IPC(8): C08G77/12C08G77/06H01L33/56C09J183/05C09K3/10
Inventor 丁小卫许家琳廖义军欧阳冲
Owner SHENZHEN ANPIN SILICONE MATERIAL
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