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Preparation method of silicone resin

The technology of silicone resin and phenyl trialkoxy silane is applied in the field of preparation of high molecular weight vinyl phenyl silicone resin for LED encapsulation reinforcement, which can solve the problem that the preparation method of polysilsesquioxane is not included, and the packaging materials are affected. Light transmittance, poor mechanical properties of vulcanized rubber, etc., to achieve the effect of improving mechanical properties, large spatial dimension, and excellent thermal stability.

Inactive Publication Date: 2015-10-14
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
[0006] Lai Guoqiao et al. (Chinese invention patent CN101323667A) developed a methyl vinyl MQ resin for LED packaging reinforcement. The MQ resin has a more obvious reinforcing effect on silicone packaging materials, but its maximum refractive index is 1.51. The refractive index of the phenyl silicone resin with a high refractive index that is gradually being developed is still somewhat different, which will affect the light transmittance of the packaging material.
Chinese invention patent CN102181159A discloses the use of polysilsesquioxane to reinforce silicone rubber for LED packaging. The reinforced silicone rubber has better light transmittance and physical and mechanical properties, and the adhesion between the product and the bracket is better. But did not include any studies on the preparation method of polysilsesquioxane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 40 parts of phenyltriethoxysilane, 100 parts of xylene, and 400 parts of deionized water into a 500ml dry four-neck flask, stir rapidly at 40°C under a nitrogen atmosphere, perform a hydrolysis reaction for 1.5 hours, and heat up to 80 ℃, add 5 parts of concentrated sulfuric acid (96wt%), polycondensation reaction 7h, after the reaction, stand and separate layers, take the upper oil phase, wash with deionized water to neutral, pour the oil phase washed to neutral into 500ml In a dry four-necked flask, in a nitrogen atmosphere, reflux at 90°C for 2 hours, add 0.02 parts of potassium hydroxide, and react for 2 hours. After the reaction, cool and add acetic acid for neutralization under stirring. The filtered oil phase was distilled at 60°C for 3 hours under a nitrogen atmosphere, and the concentrated 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 with h...

Embodiment 2

[0049] Add 40 parts of phenyltrimethoxysilane, 400 parts of toluene, and 150 parts of deionized water into a 500ml dry four-neck flask, stir rapidly at 20°C under a nitrogen atmosphere, perform hydrolysis reaction for 5 hours, heat up to 85°C, add 6 parts of concentrated sulfuric acid (96wt%), polycondensation reaction 7h, after the reaction finishes, stand to separate layers, take the upper oil phase, wash with deionized water to neutrality, pour the oily phase washed to neutrality into 500ml dry four In a nitrogen atmosphere, reflux at 80°C for 2 hours, add, for example, 0.2 parts of tetramethylammonium hydroxide, and react for 2 hours. After the reaction, cool and add acetic acid under stirring for neutralization. After the neutralization is completed, suction filter. The filtered oil phase was distilled at 100°C for 1 hour under nitrogen atmosphere, and the concentrated product obtained from the distillation was poured into a petri dish, and the low boilers were removed at ...

Embodiment 3

[0051] Add 40 parts of phenyltrimethoxysilane, 100 parts of tetrahydrofuran, 100 parts of isopropanol, and 150 parts of deionized water into a 500ml dry four-neck flask, stir rapidly at 80°C under nitrogen atmosphere, and hydrolyze for 0.5h , heat up to 100°C, add 6 parts of hydrochloric acid (36.5wt%), polycondensation reaction for 3h, after the reaction, stand and separate layers, take the upper oil phase, wash with deionized water until neutral, wash with water until neutral oil Pour the phase into a 500ml dry four-neck flask, reflux at 75°C for 2 hours in a nitrogen atmosphere, add 0.08 parts of potassium hydroxide, and react for 2 hours. After the reaction is completed, cool and add acetic acid to neutralize under stirring. Suction filtration, distill the filtered oil phase at 70°C for 2 hours under nitrogen atmosphere, pour the concentrated product obtained from the distillation into a petri dish, remove low boiling substances at 100°C / -0.1MPa, and obtain a colorless and ...

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Abstract

The invention discloses a preparation method of silicone resin and especially relates to a preparation method of high-molecular-weight phenyl silicone resin used in LED package reinforcement. The preparation method includes the steps of a) adding an acid catalyst to a mixed solution composed of phenyltrialkoxyl silane, an organic solvent and water and carrying out a reaction; b) water-washing an oil phase after the reaction finished until the oil phase is neutral; c) performing heating reflux to the oil phase to remove water; d) adding an alkaline catalyst to the oil phase and carrying out a reaction; e) adding an weak acid to neutralize the oil phase; and f) suction-filtering, distilling and vacuum-drying the oil phase to obtain the colorless transparent product which is the high-molecular-weight phenyl silicone resin. The preparation method allows the raw material to be obtained easily, is simple in operation, is easy to control and is convenient to industrialize. The silicone resin is excellent in performances and is wide in market prospect. The silicone resin is especially suitable as a reinforcing material in an LED package material, and is also expected for being used as a reinforcing agent in other organic silicon materials, and can be used as stripping strength regulation agents and other additives and the like in a surface treatment agent, a demoulding agent, a defoaming agent, an anti-sticking agent, a brightening agent and an addition-type anti-sticking agent.

Description

technical field [0001] The invention relates to a preparation method of a phenyl silicone resin, in particular to a preparation method of a high molecular weight vinyl phenyl silicone resin used for LED package reinforcement. technical background [0002] With the increasingly prominent energy problems, saving energy becomes more and more important. At present, the energy consumed by lighting accounts for about 20% of the world's total energy consumption. If new energy sources with low energy consumption, long life, safety and environmental protection are developed to replace traditional light sources with low efficiency and high energy consumption, a lot of energy will be saved. [0003] Semiconductor lighting technology is one of the most promising high-tech technologies in the 21st century, and Light Emitting Diode (LED) is its core technology. LED has the advantages of low working voltage, low power consumption, high luminous efficiency, extremely short luminous respons...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/16C08G77/08
Inventor 马凤国刘涛
Owner 马凤国
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