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Preparation method for methyl phenyl vinyl polysiloxane for packaging LED

A methyl phenyl ethylene and LED packaging technology, applied in the field of silicone preparation, can solve the problems of large difference in refractive index, complex product composition, low product light transmittance, etc., to improve light transmittance and optimize polymerization time. , the effect of high refractive index

Inactive Publication Date: 2009-01-14
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to Ph 2 SiCl 2 with Me 2 SiCl 2 and MeViSiCl 2 The difference in hydrolysis activity is large, which makes the composition of the product complex. Among them, there are organosilicon block polymers containing both diphenylsiloxane chains and dimethylsiloxane chains, and there are only dimethylsiloxane chains. Or polymers composed of diphenylsiloxane chains, the refractive index of each component is quite different, which eventually leads to low light transmittance of the product

Method used

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  • Preparation method for methyl phenyl vinyl polysiloxane for packaging LED

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Experimental program
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Effect test

Embodiment 1

[0032] Into a 1L three-neck flask filled with 46ml of toluene and 360ml of water, under stirring at 45°C, 50ml of PhSiCl 3 , 39.2mlMeViSiCl 2 , 45.1ml Me 2 SiCl 2 , 95ml of toluene was added dropwise for about 1 hour, and the stirring was continued for 1 hour. Stand still, separate layers, and remove the acid solution in the lower layer with a separatory funnel. Use deionized water at 40°C~50°C to neutral. Take 50g of the obtained silanol toluene solution, add 50g toluene and 0.05g KOH, reflux in a 250ml three-necked flask at 70~80°C for 5h, cool, add 1.5g MeSiCl 3 , stirred for 1 h, washed with deionized water until neutral. Concentrate at 0.8MPa~0.96MPa, and remove the remaining toluene and the water generated by the polycondensation reaction to obtain a clear and transparent methylphenyl vinyl silicone resin with a vinyl mole percentage of 0.304, R / Si=1.38, and a refractive index Rate 1.490.

Embodiment 2

[0034] To a 1L three-neck flask filled with 46ml of toluene and 360ml of water, add 50ml of PhSiCl dropwise within 2h under stirring at 40°C 3 , 22ml MeViSiCl 2 , 26ml Me 2 SiCl 2 , 35ml MePhSiCl 2 , 88ml of toluene mixed solution, continue to stir for 1h. Stand still, separate layers, and remove the acid solution in the lower layer with a separatory funnel. Wash with deionized water at 40°C~50°C for 7-8 times until neutral, and add 50g of silanol toluene solution to 50g of toluene and 0.05gKOH, reflux in a 250ml three-necked flask at 70~80°C for 2h, cool, Add 1.5g MeSiCl 3 , stirred for 1 h, washed with deionized water until neutral. Concentrate at 0.8MPa~0.96MPa, and remove the remaining toluene and the water generated by the polycondensation reaction to obtain a clear and transparent methylphenyl vinyl silicone resin with a vinyl mole percentage of 0.185, R / Si=1.47, and a refractive index Rate n D 25 = 1.5465.

Embodiment 3

[0036] To a 1L three-neck flask containing 46ml of toluene and 360ml of water, add 50ml of PhSiCl dropwise within 2h under stirring at 50°C 3 , 22ml MeViSiCl 2 , 13ml Me 2 SiCl 2 , 17.5ml MePhSiCl 2 , 88ml of toluene mixed solution, continue to stir for 1h. Stand still, separate layers, and remove the acid solution in the lower layer with a separatory funnel. Wash 7-8 times with deionized water at 40°C~50°C until neutral, add 50g of silanol toluene solution to 50g of toluene, 0.15g KOH, reflux in a 250ml three-necked flask at 70~80°C for 2h, cool , add 4.5g MeSiCl 3 , stirred for 1 h, washed with deionized water until neutral. Concentrate at 0.8MPa~0.96MPa, remove the remaining toluene and water generated by polycondensation reaction, and obtain a product containing part of white filaments. After decolorization by activated carbon and filtration, it is a colorless transparent methylphenyl vinyl silicone resin. The molar percentage of its vinyl group is 0.242, R / Si=1.31,...

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Abstract

The invention discloses a preparation method for organosilicon, in particular relates to a preparation method of methyl-phenyl-vinyl silicone resin with high refractive index and high light transmission rate for packaging LED. The preparation method adopts the steps that the mixture of chlorosilane and toluene is added into the solvent which is composed of water and the toluene, the hydrolysis reaction is performed, then an amount of catalyzer is added into the silanol-toluene solution as hysrolysis product, the polycondensation reaction is performed, end capping reagent is finally added to perform the reaction, thus the objective product is obtained. The methyl-phenyl-vinyl silicone resin prepared by utilizing the method has the advantages of high refractive index, transparent clarification, radiation resistance, and high and low temperature resistance and weather resistance, thereby being especially suitable for the high modular basic glue in the packaging material for LED and expected to be applied in organosilicon material such as elastomeric sealant, pouring sealant, elastomoric adhesive and the like.

Description

technical field [0001] The invention relates to a method for preparing organic silicon, in particular to a method for preparing methylphenylvinyl silicone resin with high refractive index and high light transmittance for LED packaging. technical background [0002] After decades of development, power light-emitting diodes (Light Emitting Diode, LED) are widely used in large-area graphic display full-color screens, status indications, sign lighting, signal displays, backlights for liquid crystal displays, automobile combination taillights and vehicle Internal lighting etc. LED has the advantages of energy saving, environmental protection, safety, long life, low consumption, low heat, shockproof, waterproof, miniature, high brightness, easy dimming, concentrated beam and reduced maintenance, etc. After the fourth generation of light sources. [0003] The traditional LED packaging material is epoxy resin. Due to the large difference in refractive index between the semiconduc...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06
Inventor 吴连斌杨雄发伍川陈遒陈利民蒋剑雄齐帆
Owner HANGZHOU NORMAL UNIVERSITY
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