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Vinylphenylpolysiloxane, preparation method and application

A technology of vinyl phenyl and polysiloxane, which is applied in the direction of electrical components, circuits, semiconductor devices, etc., can solve the problems of uneven polymer, low refractive index of resin, low resistance to cold and heat shock, etc., and achieve cheap raw materials Easy to obtain, avoid industrial waste water, and improve stability

Inactive Publication Date: 2014-05-28
GUANGDONG HENGDA NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the large difference in the hydrolysis activity of the above components, the synthesized polymer is not uniform, which seriously affects the mechanical properties and light transmittance of the cured film, and finally leads to the product being exposed to severe temperature changes and ultraviolet radiation. Cracking and yellowing occur, and the above methods will generate a large amount of waste water, seriously polluting the environment
[0004] The research team of Byeong-Soo Bae from Korea Advanced Institute of Science and Technology recently published a number of papers on organosilicon hybrid materials in high-level SCI journals Research papers were published on Chemistry of materials in 2010 entitled Thermally Stable Transparent Sol-Gel Based Siloxane Hybrid Material with High Refractive Index for Light Emitting Diode (LED) Encapsulation, and in 2012 on Journal of Materials Chemistry For the research paper on High performance encapsulant for light-emitting diodes (LEDs) by a sol-gel derived hydrogen siloxane hybrid, Byeong-Soo Bae's research team used diphenylsiloxane as one of the raw materials and Ba(OH )2 was used as a catalyst to synthesize a series of silicone resins. The silicone resin synthesized by this method will cause a small amount of Ba(OH)2 to be stored in the system. The stability is very poor, and the synthetic resin has a great influence on the curing rate after compounding. In the literature, it is required to add 200ppm of platinum catalyst to increase the curing temperature to 150oC, so it is often It brings the problems of low refractive index and low hardness of the resin and low thermal shock resistance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0024] The vinylphenyl polysiloxane described in this embodiment is prepared by the following method:

[0025] In a 1000ml glass kettle, add 129.4g of diphenylsilanediol, 54.4g of methyltrimethoxysilane, 45g of diphenyldimethoxysilane, 74g of vinyltrimethoxysilane, 200g of toluene and the weight percentage concentration 6g of 10%~40% tetramethylammonium hydroxide alkali gel, stirred rapidly at 90°C and reacted for 3h, added 32.4g of hexamethyldisiloxane, reacted for 2h, stood still and filtered through a filter with a pore size of 0.5 micron Membrane filtration, and then pull down to 180°C under high vacuum -0.1Mpa to remove low boilers, and then obtain a clear and transparent product, vinyl phenyl polysiloxane. The obtained product has a refractive index of 1.5525, a viscosity of 16560 mPa.s, and a vinyl content of 6.5% by mass.

Embodiment 2

[0027] The vinylphenyl polysiloxane described in this embodiment is prepared by the following method:

[0028] In a 1000ml glass kettle, add 129.4g of diphenylsilanediol, 54.4g of dimethyldimethoxysilane, 40g of methylphenyldiethoxysilane, 37g of vinyltrimethoxysilane, 200g of xylene and 6g of tetramethylammonium hydroxide aqueous solution with a concentration of 10%~70% by weight, stirred rapidly at 90°C and reacted for 3h, added l,3-divinyl-1,1,3,3-tetramethyldi Siloxane 24.3g, react for 2h, let it stand and filter it with a filter membrane with a pore size of 0.5 microns, and then pull it down to 180°C under high vacuum -0.1Mpa to remove low boiling substances, and then obtain a clear and transparent product vinyl phenyl polysiloxane. The obtained product has a refractive index of 1.5503, a viscosity of 189000 mPa.s, and a vinyl mass percentage of 5.4%.

Embodiment 3

[0030] The vinylphenyl polysiloxane described in this embodiment is prepared by the following method:

[0031] Into a 1000ml glass kettle, add 172.8g of diphenylsilanediol, 54.4g of methyltriethoxysilane, 35g of diphenyldiethoxysilane, 26.4g of methylvinyldimethoxysilane, and 200g of methanol and tetramethylammonium hydroxide 6g, stirred rapidly at 90°C and reacted for 3h, added 24.3g of l,3-divinyl-1,1,3,3-tetramethyldisiloxane, reacted for 2h, static Place and filter with a filter membrane with a pore size of 0.5 micron, and then pull it down to 180°C under high vacuum -0.1Mpa to remove low boilers, and then obtain a clear and transparent product vinyl phenyl polysiloxane. The obtained product has a refractive index of 1.5583, a viscosity of 28760 mPa.s, and a vinyl mass percentage of 4.5%.

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Abstract

The invention discloses a preparation method of vinylphenylpolysiloxane. The method comprises the following steps: 1) stirring a solvent, diphenyl silanediol, an alkyloxy compound and a catalyst and heating the mixture in a reaction vessel to react for 1-40h, and adding an end plate agent for blocking; 2) heating the above mixed liquor and stirring; 3) standing and filtering; and 4) heating a filtrate, removing low-boiling-point substances so as to obtain vinylphenylpolysiloxane. The invention also discloses vinylphenylpolysiloxane prepared by the above method and an application of vinylphenylpolysiloxane in LED package resin. The preparation method of vinylphenylpolysiloxane has the following advantages: firstly, resin storage stability is raised; secondly, it is convenient for industrialization; and finally, generation of industrial wastewater is avoided, and the preparation method is more environmentally friendly. Refractive index of the vinylphenylpolysiloxane disclosed by the invention is 1.50-1.57, and the vinylphenylpolysiloxane is especially applicable to be used as a strengthening agent of macromolecules in an LED packaging material.

Description

technical field [0001] The invention relates to the field of encapsulation material design, in particular to a vinylphenyl polysiloxane used in LED encapsulation resin, its preparation method and application. Background technique [0002] Silicone is an important LED packaging material, which has the advantages of good temperature resistance, high light transmittance, large refractive index, good stability, small stress, low hygroscopicity, good mechanical properties and ultraviolet radiation resistance, etc. The performance is far superior to epoxy resin, which is also an LED packaging material, so it has become the first choice for power LED packaging. Silicone encapsulation material with high refractive index is made of vinyl silicone resin containing a certain amount of diphenylsiloxane chain or methylphenylsiloxane chain and hydrogen-containing silicone oil through hydrosilicon addition reaction under certain conditions. Got it. [0003] Many researchers use diphenyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/08H01L33/56
Inventor 刘关喜关怀王先胜何丹龙正宇周为民
Owner GUANGDONG HENGDA NEW MATERIALS TECH
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