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Preparation method and application of polyhedral oligomeric silsesquioxane skeleton containing vinyl silicone oil

A technology of polysilsesquioxane and vinyl silicone oil, which is applied in the direction of semiconductor devices, electrical components, circuits, etc., can solve the problems of easy precipitation, affecting the light transmittance and mechanical properties of products, and poor compatibility, and achieves the goal of preparing The effect of simple method

Active Publication Date: 2013-09-11
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the poor compatibility and easy precipitation of polysilsesquioxane (POSS) with vinyl silicone oil and hydrogen-containing silicone oil when directly blending polysilsesquioxane (POSS) with vinyl silicone oil and hydrogen-containing silicone oil, In order to solve the problem of affecting the light transmittance and mechanical properties of the product, the present invention proposes a preparation method of vinyl silicone oil containing polysilsesquioxane skeleton, and adopts a copolymerization reaction method to obtain And other copolymers with good compatibility with silicone polymers, the preparation method is simple

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 40g (0.5405 mol dimethylsiloxane chain link) D3 to a 100ml three-necked bottle, 25.66g (0.05405 mol) hexavinyl POSS, 0.3g (0.00161mol) 1,1,3,3-tetramethyl-1 ,3-Divinyl disiloxane, 0.4g NaOH was polymerized at 110 ℃ for 12 h, then reduced to room temperature, 0.735g concentrated phosphoric acid was added, stirred for 2h, until the system was neutral, and then heated to -0.08MPa At 170°C, the low boilers were removed under reduced pressure to obtain 44.2 g of vinyl silicone oil containing hexavinyl POSS skeleton with a yield of 65.0%;

Embodiment 2

[0030] Add 30 g (0.4054 mol of dimethylsiloxane chain link) D4 to a 100ml three-necked bottle, 10 g (0.07353 mol of methylphenylsiloxy chain link) methyl phenyl cyclotrisiloxane, 1.14 g (0.0018 mol) ) Octavinyl POSS, 3.22 g (0.00161 mol, average molecular weight 2000) α,ω-divinyl silicone oil, 3.6 g KOH polymerized at 130 ℃ for 8 hours, then cooled to room temperature, added 6.615 g concentrated phosphoric acid, stirred for 3 hours, Until the system is neutral, then the temperature is raised to 170 ℃ at -0.096 MPa, and low boilers are removed under reduced pressure to obtain 35.5 g of vinyl silicone oil containing octavinyl POSS skeleton with a yield of 85.6%;

Embodiment 3

[0035] Into a 100ml three-necked flask, add 5g (dimethylsiloxy chain link 0.06757mol) D3, 35g (methylphenylsiloxy chain link 0.2574mol) methyl phenyl cyclotetrasiloxane, 3.42 g (0.0054mol) ten Vinyl POSS, 3.22 g (0.00161mol, average molecular weight 2000) α,ω-dimethylphenylsilyl vinyl silicone oil, 1.2 g (CH 3 ) 4 NOH was polymerized at 110°C for 2h, then heated to 140°C to decompose the catalyst for 2h, and then heated to 170°C at -0.08~-0.096MPa, and low boilers were removed under reduced pressure to obtain 41.6 g of vinyl containing a decavinyl POSS skeleton Silicone oil, the yield is 95.2%;

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PUM

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Abstract

The invention relates to an organic silicon rubber for LED packaging. In order to solve the problems that during direct physical blending of POSS (polyhedral oligomeric silsesquioxane) with vinyl silicone oil and hydrogen containing silicone oil, POSS has poor compatibility with vinyl silicone oil and hydrogen containing silicone oil and is very easy to precipitate, so that the light transmittance and mechanical properties of the product can be affected, the invention provides a preparation method of a POSS skeleton containing vinyl silicone oil. The method includes: mixing POSS with one or two of dimethyl polysiloxane and methylphenyl polysiloxane at any proportion to obtain a mixture, in the presence of a catalyst, carrying out end-capping with a vinyl end-capping reagent, and performing a polymerization reaction to obtain the POSS skeleton containing vinyl silicone oil. The preparation method is simple. The invention also provides application of the POSS skeleton containing vinyl silicone oil in LED packaging materials.

Description

Technical field [0001] The invention relates to an LED packaging organic silicon rubber, in particular to a preparation method of a vinyl silicone oil containing a polysilsesquioxane skeleton and its application to LED packaging. Background technique [0002] High-brightness Light Emitting Diode (LED) is a new type of lighting source. It consumes only 1 / 10 of the traditional light source. It does not use mercury that seriously pollutes the environment. It is small in size, low in driving voltage and long in life. Become the new focus of the global lighting industry. With the deepening of research and development of ultra-high-brightness LEDs, power white LEDs are expected to become the fourth-generation light source after incandescent lamps, fluorescent lamps, and high-intensity gas discharge lamps. Silicone rubber is an ideal material for LED packaging because of its good heat resistance, weather resistance, moisture resistance, and thermal shock resistance. [0003] Ordinar...

Claims

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Application Information

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IPC IPC(8): C08G77/44C08G77/20C08L83/07C08L83/10C08L83/05H01L33/56
Inventor 杨雄发杨琳琳曹诚来国桥蒋剑雄吴连斌华西林罗蒙贤陈利民陈遒
Owner HANGZHOU NORMAL UNIVERSITY
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