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A kind of preparation method of phenyl silicone 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, large spatial dimensions, and uniform product composition

Inactive Publication Date: 2017-11-28
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 a hydrolysis reaction for 0.5h, and raise the temperature 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 the atmosphere, distill at 20°C for 12h, 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 80 parts of xylene, 3 parts of dimethylvinylethoxysilane, stir at 50°C for 1h,...

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 hydrolyze 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-neck flask, then add 80 parts of n-butanol and 4...

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Abstract

The invention discloses a preparation method of a phenyl silicone resin, in particular to a preparation method of a vinyl phenyl silicone resin with high refractive index and high light transmittance for LED encapsulation reinforcement. In the present invention, the mixed solution composed of phenyltrialkoxysilane, organic solvent and water is firstly hydrolyzed, and then an acid catalyst is added to the hydrolyzed product to carry out the polycondensation reaction, and the prepared product is washed and neutralized. Most of the organic solvents are distilled off, and the residual low boilers are removed by vacuum drying, and the hydroxyl-terminated phenyl silicone resin can be prepared. The prepared hydroxyl-terminated phenyl silicone resin is used as a raw material, dissolved in an organic solvent, and the vinyl silane Add it into the organic solution of hydroxyl-terminated phenyl silicone resin, stir evenly, add the acid catalyst into the mixed solution, stir evenly, heat up the reaction, neutralize the product obtained, dry it, filter it with suction, distill it, and then dry it in vacuum. The target product can be obtained.

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 Patents(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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