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Preparation method for phenyl silicon resin

A phenyl silicone resin, silicone resin technology, applied in electrical components, circuits, adhesives, etc., can solve the problems of poor mechanical properties of vulcanized rubber, and achieve the effects of improving mechanical properties, high degree of branching, and uniform product composition

Inactive Publication Date: 2015-09-09
马凤国
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unreinforced vulcanizate has poor physical and mechanical properties and cannot meet the requirements, so reinforcing fillers must be added to reinforce the packaging material, but the addition of fillers can easily have a negative impact on the refractive index and light transmittance of the packaging material , which puts forward higher requirements for the selection of reinforcing fillers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 20 parts of phenyltrimethoxysilane, 50 parts of xylene, and 70 parts of deionized water into a 250ml dry four-neck flask, stir rapidly at 20°C under a nitrogen atmosphere, perform a hydrolysis reaction for 5 hours, and heat up to 75°C. Add 3.6 parts of concentrated hydrochloric acid (37wt%), polycondensation reaction 10h, stop the reaction, let stand to separate layers, take the upper oil phase, wash with deionized water to neutral, wash to neutral solution containing the resin product in nitrogen Under the atmosphere, distill at 65°C for 2h, pour the distilled product into a petri dish, and remove low boilers at 100°C / -0.1MPa to obtain a colorless and transparent product, hydroxyl-terminated phenyl silicone resin, under nitrogen atmosphere , add 10 parts of the prepared hydroxy-terminated phenyl silicone resin into a 250ml dry four-necked flask, then add 100 parts of toluene, 4 parts of dimethylvinylethoxysilane, stir at 30°C for 1h, add 3 parts Concentrated hydroc...

Embodiment 2

[0041] Add 20 parts of phenyltriethoxysilane, 50 parts of toluene, and 160 parts of deionized water into a 250ml dry four-necked bottle, stir rapidly at 80°C under a nitrogen atmosphere, perform hydrolysis reaction for 0.5h, and heat up to 75°C. Add 6 concentrated sulfuric acid (96wt%), polycondensation reaction 8h, stop reaction then, leave standstill layering, take upper layer oily phase, wash with deionized water to neutrality, the solution that is dissolved in the resin product that washes to neutrality is in nitrogen gas Under atmosphere, distill at 20°C for 12 hours, pour the distilled product into a petri dish, remove low boilers at 100°C / -0.1MPa, and obtain a colorless and transparent product, hydroxyl-terminated phenyl silicone resin, under nitrogen atmosphere , add 10 parts of the prepared hydroxy-terminated phenyl silicone resin into a 250ml dry four-necked flask, then add 80 parts of xylene, 3 parts of dimethylvinylethoxysilane, stir at 50°C for 1h, add 1 Part of c...

Embodiment 3

[0043] Add 20 parts of phenyltrimethoxysilane, 50 parts of xylene, 50 parts of isopropanol, and 60 parts of deionized water into a 250ml dry four-necked bottle, stir rapidly at 35°C under a nitrogen atmosphere, and perform a hydrolysis reaction for 2 hours. Raise the temperature to 80°C, add 3 parts of cation exchange resin, conduct polycondensation reaction for 12 hours, then stop the reaction, let stand to separate layers, take the upper oil phase, wash with deionized water until neutral, and wash until neutral to dissolve the resin product. The solution was distilled at 45°C for 8 hours under a nitrogen atmosphere, and the product obtained from the distillation was poured into a petri dish, and the low boilers were removed at 100°C / -0.1MPa to obtain a colorless and transparent product, hydroxyl-terminated phenyl silicone resin. Under a nitrogen atmosphere, add 10 parts of the prepared hydroxy-terminated phenyl silicone resin into a 250ml dry four-necked flask, then add 80 pa...

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Abstract

The present invention discloses a preparation method for phenyl silicon resin, in particular to a preparation method for vinyl phenyl silicone resin which is high in refraction index and light transmittance and is applied to LED encapsulation and reinforcement. Hydrolysis reaction is first conducted on a mixed solution formed by phenyl tri-alkoxysilane, an organic solvent and water; an acid catalyst is added in hydrolysis product then to conduct polycondensation reaction; the prepared product is conducted by water washing neutralization; distillation is conducted to remove a majority of organic solvent; vacuum drying is conducted to remove residual low-boiling-point substances; hydroxyl phenyl silicone resin is prepared and obtained; the prepared hydroxyl phenyl silicone resin is taken as a raw material to be dissolved in the organic solvent; vinyl silane is added in the phenyl silicone resin organic solution end capped by hydroxyl, and is stirred uniformly; the acid catalyst is added in the mixed solution, and is stirred uniformly; the temperature is raised, and reaction is conducted; the obtained product, after neutralization and drying treatment, is conducted by suction filtration, distillation and vacuum drying to prepare the target product.

Description

technical field [0001] The invention designs a preparation method of phenyl silicone resin, especially a preparation method of vinyl phenyl silicone resin, a reinforcing material with high refractive index and high light transmittance for LED packaging. technical background [0002] As mankind enters the 21st century, energy issues are increasingly prominent, and energy conservation is as important as developing new energy sources. Currently, lighting consumes about 20% of the world's total energy consumption. If the traditional light source with low efficiency and high energy consumption can be replaced with a new light source with low energy consumption, long life, safety and environmental protection, it will save a lot of energy. [0003] The power consumption of light emitting diode (Light Emitting Diode, LED) is only 1 / 10 of the traditional light source, and it is not suitable for mercury that seriously pollutes the environment. It is small in size, long in life, low i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/16C08G77/06C08G77/08C08G77/34H01L33/56C09J183/07
Inventor 马凤国刘涛
Owner 马凤国
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