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Method for preparing methyl and phenyl hydrogen-containing silicon oil for packaging LED

A technology of LED encapsulation and methylphenyl cyclosiloxane, which is applied in chemical recycling, electrical components, circuits, etc., can solve the problems of great difference in product composition, poor product repeatability and controllability, etc. The effect of easy industrialization and high refractive index

Active Publication Date: 2008-10-22
XINYAQIANG SILICON CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the composition of the product obtained under different raw material ratios and hydrolysis conditions varies greatly, resulting in poor repeatability and controllability of the product.

Method used

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  • Method for preparing methyl and phenyl hydrogen-containing silicon oil for packaging LED
  • Method for preparing methyl and phenyl hydrogen-containing silicon oil for packaging LED
  • Method for preparing methyl and phenyl hydrogen-containing silicon oil for packaging LED

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] in N 2 Add polysiloxane monomer D to a 100mL dry three-neck flask under protection n Me，Ph (35.1g, 0.065mol) and D 4 H (8.4g, 0.035mol), remove the water in polysiloxane monomer at 35℃~45℃ / -0.096MPa, and then add 0.67g end-capping agent 1,1,3,3-tetramethyl -1,3-dihydrodisiloxane, 2.24g strong acid type macroporous cation exchange resin, in N 2 Under protection, polymerize at 65°C for 5 hours, and recover the strong-acid large-pore size cation exchange resin by suction filtration. Reduce the pressure to -0.096MPa, gradually raise the temperature to 205°C to remove low-molecular compounds, stop heating when there is no fraction within 5 minutes, and cool to room temperature to obtain a colorless and transparent product. The resulting product n D 25 =1.5230, GPC records number average molecular weight 0.83×10 4 , the molecular weight distribution width (MWD) is 1.81, after 1 The Si-H mass percent content measured by H-NMR is 0.287%, the Ph / Si (molar ratio) is 65.8...

Embodiment 2

[0035] Using the same method as in Example 1, at N 2 Add polysiloxane monomer D to a 100mL dry three-neck flask under protection n Me，Ph (35.1g, 0.065mol), D 4 H (8.4g, 0.035mol) and D 4 Me，Et (0.38g, 0.001mol), remove the water in polysiloxane monomer at 35℃~45℃ / -0.096MPa, and then add 0.67g end-capping agent 1,1,3,3-tetramethyl -1,3-dihydrodisiloxane, 2.24g strong acid type macroporous cation exchange resin, in N 2 Under protection, polymerize at 65°C for 5 hours, and recover the strong-acid large-pore size cation exchange resin by suction filtration. Reduce the pressure to -0.096MPa, gradually raise the temperature to 205°C to remove low-molecular compounds, stop heating when there is no fraction within 5 minutes, and cool to room temperature to obtain a colorless and transparent product. The resulting product n D 25 =1.5130, the number average molecular weight measured by GPC is 0.75×10 4 , the molecular weight distribution width (MWD) is 1.51, after 1 H-NMR rec...

Embodiment 3

[0037] Using the same method as in Example 1, at N 2 Add polysiloxane monomer D to a 100mL dry three-neck flask under protection n Me，Ph (35.1g, 0.065mol), D 4 H (8.4g, 0.035mol) and D 4 Me，Et (1.14g, 0.003mol), remove the water in polysiloxane monomer at 35℃~45℃ / -0.096MPa, then add 0.67g end-capping agent 1,1,3,3-tetramethyl -1,3-dihydrodisiloxane, 2.24g strong acid type macroporous cation exchange resin, in N 2 Under protection, polymerize at 65°C for 5 hours, and recover the strong-acid large-pore size cation exchange resin by suction filtration. Reduce the pressure to -0.096MPa, gradually raise the temperature to 205°C to remove low-molecular compounds, stop heating when there is no fraction within 5 minutes, and cool to room temperature to obtain a colorless and transparent product. The resulting product n D 25 =1.5154, the number average molecular weight measured by GPC is 0.77×10 4 , the molecular weight distribution width (MWD) is 1.83, after 1 H-NMR records...

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Abstract

The invention relates to a method for making hydrogen-containing silicone oil, in particular to a method for making methyl phenyl hydrogen-containing silicone oil for the encapsulation of LEDs. The method is characterized in that the methyl-phenyl cyclic siloxane (Dn<Me, Ph>), the tetramethyl tetraethyl cyclic tetra-siloxane (D4<Me, Et>) and hydrocyclotetrasiloxane (D4<H>) are taken as monomers; under the protection of N2, right amount of an end capping agent is added into the monomer mixture to be copolymerized under the action of a catalyst, after the polymerization, the catalyst is filtered and recycled, the low molecular compound of the obtained clear solution is removed in decompression and high temperature conditions, the clear solution without low molecular compound is cooled to the room temperature, and the target product is obtained. The method has the advantages of available raw materials, low cost, moderate conditions, simple technique, simple operation, environmental protection and convenient industrialization. The product made by the method can be widely applied to the enterprises which manufacture and use the LEDs, etc.

Description

technical field [0001] The invention relates to a method for preparing hydrogen-containing silicone oil, in particular to a method for preparing methylphenyl hydrogen-containing silicone oil for LED packaging. 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 pow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/06H01L33/00H01L33/56
CPCY02P20/584
Inventor 杨雄发伍川蒋剑雄董红罗蒙贤华西林
Owner XINYAQIANG SILICON CHEM JIANGSU
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