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Preparation method for MDT silicone resin used for high-power package

A silicone resin, high-power technology, applied in the field of preparation of MDT silicone resin for high-power packaging

Inactive Publication Date: 2018-05-08
YANTAI DARBOND TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the deficiencies of existing MDT silicone resins, the present invention provides a method for synthesizing MDT resins composed of methyl M links, vinyl M links, methylphenyl D links, methylvinyl D links, and phenyl T links.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 1.77g concentrated hydrochloric acid, 30.46g dimethyldimethoxysilane, 182.29g methylphenyldimethoxysilane, 198.26g phenyltrimethoxysilane, 15.10g ethanol and 5g water in the four-necked flask, stir , Heat to 25°C and react for 2 hours. After the reaction is completed, add 57.40g of water, 15.13g of vinyl double-caps, and 67.70g of hexamethyldisiloxane dropwise at room temperature, and control the temperature in the system at 30-40°C In between, react at 70°C for 2 hours after the dropwise addition, then distill off the alcohol in the system, then add 300g of toluene and an appropriate amount of Na2CO3 to adjust the pH of the system to 10, react at 90°C for 1 hour, then heat up to 120°C to evaporate The remaining alcohol and water in the system are finally cooled down, neutralized with acetic acid, and washed with water until the system pH=6-7; the toluene is removed by rotary evaporation at 120°C to obtain the silicone resin; the yield is 95%.

Embodiment 2

[0024] Add 1.77g of concentrated hydrochloric acid, 30.46g of dimethyldiethoxysilane, 210.35g of methylphenyldiethoxysilane, 240.37g of phenyltriethoxysilane, 15.10g of ethanol and 5g of water into the four-necked flask, Stir and heat to 25°C to react for 2 hours. After the reaction is completed, add 57.40g of water, 15.13g of vinyl double-caps, and 67.70g of hexamethyldisiloxane dropwise at room temperature, and control the temperature in the system at 30-40 ℃, react at 70℃ for 2 hours after the dropwise addition, then distill off the alcohol in the system, then add 300g toluene and an appropriate amount of NaHCO3 to adjust the pH of the system to 10, react at 90℃ for 1 hour, then heat up to 120℃ to evaporate Remove the remaining alcohol and water in the system, and finally lower the temperature, neutralize with acetic acid, and wash with water until the pH of the system is 6-7; rotary evaporation at 120°C removes the toluene to obtain silicone resin with a yield of 94%.

Embodiment 3

[0026] Add 1.60g of concentrated sulfuric acid, 30.46g of dimethyldimethoxysilane, 182.29g of methylphenyldimethoxysilane, 198.26g of phenyltrimethoxysilane, 15.10g of alcohol and 5g of water into a four-necked flask, stir, Heat to 25°C and react for 2 hours. After the reaction is completed, add 57.40g of water, 15.13g of vinyl double-caps, and 67.70g of hexamethyldisiloxane dropwise at room temperature, and control the temperature in the system between 30-40°C. After the dropwise addition, react at 70°C for 2 hours, then evaporate the alcohol in the system, then add 300g of toluene and an appropriate amount of NaOH to adjust the pH of the system to 10, react at 90°C for 1 hour, then raise the temperature to 120°C to evaporate the system The remaining alcohol and water are finally cooled down, neutralized with acetic acid, and washed with water until the pH of the system is 6-7; the toluene is removed by rotary evaporation at 120°C to obtain the silicone resin; the yield is 90%...

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PUM

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Abstract

The invention relates to a preparation method for MDT silicone resin used for high-power package. The preparation method comprises the following steps: adding an acid, dimethyldialkoxysilane, methylphenyldialkoxysilane, phenyltrialkoxysilane, an alcohol and water in a four-mouth flask, carrying out stirring and heating to 25 DEG C, carrying out a reaction for 1-2 hours, after the reaction is completed, simultaneously dropwise adding remaining total amount of water, divinyltetramethyldisiloxane and hexamethyldisiloxane at room temperature, controlling the temperature in the system to be 30-40 DEG C, after the adding is completed, carrying out a reaction at 70 DEG C for 1-2 hours, then distilling off the alcohol in the system, adding toluene and an alkali which have larger amounts than a theoretical resin amount to regulate the pH value of the system to be 9-10, carrying out a reaction at 90 DEG C for 1 hour, then carrying out heating to distill off the residual alcohol and water in thesystem, finally carrying out cooling, neutralizing with acid, and washing with water until the pH value of the system is 6-7, and carrying out rotary evaporation at a temperature of 120 DEG C to remove the toluene to obtain the silicone resin. The prepared MDT silicone resin is mainly used for a reinforcing agent, an organic silica gel adhesive and an organosilicon molding compound of packaging resin.

Description

technical field [0001] The invention relates to a preparation method of MDT silicone resin for high-power packaging, and belongs to the technical field of silicone resin synthesis. technical background [0002] In recent years, with the development of semiconductor light-emitting technology, it has become an inevitable trend for semiconductor lighting to replace incandescent lamps with high energy consumption and low light efficiency, which has attracted widespread attention around the world. Due to its good high and low temperature resistance and reproducibility, silicone rubber or silicone resin vulcanized by hydrosilicon addition reaction is by far the most ideal packaging material for high-power LED devices. MDT type silicon Resin is a kind of silicone resin, which consists of monofunctional silicone chain (R3SiO1 / 2, M chain), difunctional silicone chain (R2SiO, D chain) and trifunctional silicone chain Section (RSiO3 / 2, T chain section) organosilicon monomer formed by ...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06
CPCC08G77/06C08G77/20C08G77/70
Inventor 秦余磊陈维
Owner YANTAI DARBOND TECH