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Preparation of methyl phenyl hydrogen-containing silicone oil for LED encapsulation

A technology of LED encapsulation and methylphenylcyclosiloxane, applied in chemical instruments and methods, other chemical processes, electrical components, etc., can solve problems such as troublesome operation, many types, and great differences in product composition, and achieve operational The effect of simplicity, mild conditions and simple process

Inactive Publication Date: 2008-12-24
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The methylphenyl hydrogen-containing silicone oils for LED packaging reported in foreign patents are all hydrogen-containing silicone oils containing diphenylsiloxane chains, which are formed by hydrolysis and polycondensation of hydrochlorosilanes and non-hydrogen-containing chlorosilanes. , the composition of the product obtained under different raw material ratios and hydrolysis conditions is very different, resulting in poor repeatability and controllability of the product
The Chinese invention patent applied by the laboratory in the early stage uses polydimethylcyclosiloxane, polymethylhydrocyclosiloxane, methylphenyl mixed ring body and methylphenyl hydrolysis mixed ring body as polymerization Reactive monomers, ring-opening copolymerization at 50-70°C to prepare a methylphenyl hydrogen-containing silicone oil, which is suitable for use as a liquid crosslinking agent for LED packaging, but requires many types of raw materials and can obtain clear and transparent The temperature range of the product is narrow, and the product needs to be decolorized and filtered with activated carbon, which makes the operation more troublesome

Method used

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  • Preparation of methyl phenyl hydrogen-containing silicone oil for LED encapsulation
  • Preparation of methyl phenyl hydrogen-containing silicone oil for LED encapsulation
  • Preparation of methyl phenyl hydrogen-containing silicone oil for LED encapsulation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] in N 2 Add polysiloxane monomer D to a 100mL dry three-necked bottle under protection n Me，Ph (35.36 g, (MePhSiO) unit 0.26 mol) and D 4 H (8.4g, (MePhSiO) unit 0.14mol), remove the moisture in the 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 large pore cation exchange resin, in N 2 Under the protection, the polymer was polymerized at 40 °C for 5 hours, and the strong acid type large pore cation exchange resin was recovered by suction filtration. Reduce the pressure to -0.096MPa, gradually heat up to 205°C to remove low molecular compounds, stop heating when there is no fraction within 5min, and cool to room temperature to obtain a colorless and transparent product with a yield of 73%. Refractive index n of the obtained methylphenyl hydrogen-containing silicone oil D 25 =1.5195, after 1 The mass percentage of Si-H measured by H-NMR is 0.276%, the Ph / Si (molar ratio)...

Embodiment 2

[0030] in N 2 Add polysiloxane monomer D to a 100mL dry three-necked bottle under protection n Me，Ph (35.36 g, (MePhSiO) unit 0.26 mol) and D 4 H(8.4g, (MePhSiO) unit 0.14mol), remove the moisture in the 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 large pore cation exchange resin, in N 2 Under the protection, polymerize at 50 °C for 5 hours, and recover the strong acid type large-pore cation exchange resin by suction filtration. Reduce the pressure to -0.096MPa, gradually heat up to 205°C to remove low molecular compounds, stop heating when there is no fraction within 5min, and cool to room temperature to obtain a colorless and transparent product with a yield of 78%. Refractive index n of the obtained methylphenyl hydrogen-containing silicone oil D 25 =1.5225, after 1 The mass percentage of Si-H measured by H-NMR is 0.277%, the Ph / Si (molar ratio) is 0.623, and the numbe...

Embodiment 3

[0032] in N 2 Add polysiloxane monomer D to a 100mL dry three-necked bottle under protection n Me，Ph (35.36 g, (MePhSiO) unit 0.26 mol) and D 4 H (8.4g, (MePhSiO) unit 0.14mol), remove the moisture in the 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 large pore cation exchange resin, in N 2 Under the protection, polymerize at 65 °C for 5 h, and recover the strong acid type large-pore cation exchange resin by suction filtration. Reduce the pressure to -0.096MPa, gradually heat up to 205°C to remove low molecular compounds, stop heating when there is no fraction within 5min, and cool to room temperature to obtain a colorless and transparent product with a yield of 79%. Refractive index n of the obtained methylphenyl hydrogen-containing silicone oil D 25 =1.5230, after 1 The mass percentage of Si-H measured by H-NMR is 0.287%, the Ph / Si (molar ratio) is 0.658, and the number a...

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Abstract

The invention discloses a method for preparing an organic substance, in particular to a method for preparing methyl phenyl cyclosiloxane for LED packaging. The method takes methyl phenyl cyclic siloxane (Dn<Me, Ph>, n is equal to 3 and 4) and tetramethyl tetrahydric cyclotetrasiloxane (D4<H>) as monomers; under the protection of N2, an end-capping agent is added into the cyclosiloxane monomer which is subjected to pressure reduction and water removal to copolymerize under the action of a catalyst, then the filtration is performed to recover the catalyst, and the a low molecular compound in clear solution is removed under the condition of pressure reduction and high temperature and then is cooled to room temperature to produce a target product. The method has the advantages of easily-obtained raw materials, low cost, mild conditions, simple process, simple and convenient operation, no pollution, and easiness for industrialization. A product prepared by the method has good effect in the packaging process of LEDs.

Description

technical field [0001] The invention relates to a preparation method of organic silicone oil, in particular to a preparation method of methylphenyl hydrogen-containing silicone oil for LED packaging. technical background [0002] Ultra-bright light-emitting diode (Light Emitting Diode, LED) consumes only 1 / 10 of the power of traditional light sources, does not use mercury that seriously pollutes the environment, is small in size and has a long life, and has been used in decorative lighting, automotive lighting, and traffic lights. On the other hand, it is expected to become the fourth-generation light source after incandescent lamps, fluorescent lamps and high-intensity gas discharge lamps. ("China Lighting" 2007 (1-2): 54-59). [0003] At present, the packaging materials of ordinary LEDs are mainly bisphenol A transparent epoxy resins. With the development of white light LEDs, especially those based on ultraviolet light, the outer packaging materials need to be able to mai...

Claims

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Application Information

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IPC IPC(8): C08G77/12C09K3/10H01L23/29
Inventor 邱化玉杨雄发董红伍川蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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