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Refractive index-adjustable MDT silicone resin and preparation method thereof

An adjustable refractive index technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of poor optical performance of silicone polymer packaging materials, reduce the optical efficiency of semiconductor lighting devices, etc., and reduce the difference in refractive index , improve light efficiency, simple process effect

Active Publication Date: 2013-01-30
HANGZHOU NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem that the MDT silicone resin has a large difference in refractive index between the silicone resin and the polymer body due to the small refractive index, the resin-reinforced silicone polymer packaging material has poor optical performance and reduces the optical efficiency of semiconductor lighting devices. The present invention proposes a A kind of MDT type silicone resin with adjustable refractive index, the invention not only improves the optical properties of MDT silicone resin reinforced high refractive index organosilicon polymer encapsulation material, but also improves the mechanical properties of encapsulation material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 42.6 g (2.367 mol) of water, 11.2 g (0.193 mol) of acetone and 11.2 g (0.122 mol) of toluene into a 500 ml three-necked flask equipped with a mechanical stirrer, a thermometer, and a constant pressure dropping funnel, and mix them evenly under rapid stirring . When the material was raised from room temperature to 35°C, 8.80 g (0.0589 mol) methyltrichlorosilane, 7.20 g (0.0511 mol) methylvinyldichlorosilane, 9.20 g (0.0482 mol) For a mixed solution composed of methylphenyldichlorosilane and 11.2 g (0.122 mol) toluene, the dropping speed is from slow to fast, and the reaction temperature is controlled not to exceed 60°C, and the dropwise addition is completed in about 75 minutes; continue stirring at a constant temperature of 60°C for 90 minutes , then add 18.4 g (0.1136 mol) hexamethyldisiloxane and continue to stir the reaction for 55 minutes; then let stand to separate the water layer, wash the oil layer to neutral, filter after drying with anhydrous calcium chlori...

Embodiment 2

[0039] Add 46.6 g (2.589 mol) of water, 11.6 g (0.2 mol) of acetone and 11.6 g (0.126 mol) of toluene into a 500ml three-necked flask equipped with a mechanical stirrer, a thermometer, and a constant pressure dropping funnel, and mix them evenly under rapid stirring . When the material was raised from room temperature to 50°C, 11.06 g (0.074 mol) of methyltrichlorosilane, 18.74 g (0.0741 mol) of diphenyldichlorosilane and 11.6 g (0.126 mol) of toluene were added dropwise with a dropping funnel The mixed solution formed, the dropping speed is from slow to fast, and the reaction temperature is controlled not to exceed 70°C, and the dropwise addition is completed in about 30 minutes; continue to stir at a constant temperature of 65°C for 30 minutes, and then add 6 g (0.0371 mol) of hexamethyldisiloxane and continue to stir and react for 60 minutes; then let it stand to separate the water layer, wash the oil layer to neutrality, dry it with anhydrous calcium chloride and filter, t...

Embodiment 3

[0041] Add 44.3 g (2.46 mol) of water, 11.66 g (0.201 mol) of acetone and 11.66 g (0.127 mol) of toluene into a 500 ml three-necked flask equipped with a mechanical stirrer, a thermometer, and a constant pressure dropping funnel, and mix them evenly under rapid stirring . When the material was raised from room temperature to 60°C, 15.65 g (0.074 mol) of phenyltrichlorosilane, 10.44 g (0.074 mol) of methylvinyldichlorosilane and 11.66 g (0.127 mol) of For a mixed solution composed of toluene, the dropping speed is from slow to fast, and the reaction temperature is controlled not to exceed 75°C, and the dropwise addition is completed in about 60 minutes; continue to stir at a constant temperature of 60°C for 50 minutes, and then add 6 g (0.0371 mol) of hexamethyldisilica oxane and continue to stir for 70min; then let it stand to separate the water layer, and the oil layer is washed with saturated Na 2 CO 3 The aqueous solution is neutralized to neutral, dried with anhydrous ca...

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Abstract

The invention relates to the field of organic polymer chemistry and provides a refractive index-adjustable MDT silicone resin and a preparation method thereof. The refractive index-adjustable MDT silicone resin solves the problem that the existing MDT silicone resin has a small refractive index thereby leading to a large difference between refractive indexes of the silicone resin and a polymer and thus an organic silicon polymer packaging material reinforced by the existing MDT silicone resin has poor optical properties and a semiconductor lighting device adopting the organic silicon polymer packaging material has low optical efficiency. The preparation method comprises that hexamethyldisiloxane as a blocking agent, bifunctional organic dichlorosilane as a D chain unit source, and trifunctional organic trichlorosilane as a T chain unit source undergo a co-hydrolytic condensation reaction in the presence of a water-acetone-toluene mixed solution as a solvent under the self-catalysis effect of hydrochloric acid produced by chlorosilane hydrolysis to produce the refractive index-adjustable MDT silicone resin. The refractive index-adjustable MDT silicone resin improves optical properties of a MDT silicone resin-reinforced high-refractive index organic silicon polymer packaging material and also improves mechanical properties of the packaging material.

Description

technical field [0001] The invention relates to the field of organic polymer chemistry, in particular to an MDT type silicone resin with adjustable refractive index and a preparation method thereof. Background technique [0002] In recent years, with the development of semiconductor light-emitting technology, it has become an inevitable trend for semiconductor lighting to replace incandescent lamps with high energy consumption and low light efficiency, which has attracted widespread attention around the world. Silicone materials, especially silicone rubber or silicone resin vulcanized by hydrosilicon addition reaction, are by far the most ideal encapsulation materials for high-power LED devices. There are no microscopic bubbles, and the addition-type silicone polymer product has very good optical properties. It is not only an excellent internal protection material and light path material for LED chips, but also directly used as a lens material for LEDs. Due to the LED chip ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/04C08G77/06C09K3/10
Inventor 伍川张宝华董红蒋剑雄程大海陈世龙
Owner HANGZHOU NORMAL UNIVERSITY
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