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Preparation method of methyl phenyl hydrogen-containing silicone oil for LED packaging adhesive

A technology of LED encapsulation and methylphenyldimethoxysilane is applied in the field of preparation of methylphenyl hydrogen-containing silicone oil for LED encapsulation glue, which can solve the difficulty and cost of increasing production, poor repeatability and controllability, The preparation process is complicated and the operation is complicated, and the post-processing process is simple, the repeatability and controllability are good, and the process operation is simple.

Inactive Publication Date: 2017-03-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process requires the use of organic solvents, and the repeatability and controllability are poor, so there are disadvantages of complex synthesis process and pollution and energy consumption in the production process
[0004] Chinese patent CN104672455A discloses a method for preparing methylphenyl hydrogen-containing silicone oil by ring-opening polymerization of cyclosiloxane catalyzed by strong acid, but the raw materials (methylphenylcyclosiloxane) used in this method are mostly passed through chlorosilane It is produced by hydrolysis and condensation. The preparation process is complicated to operate, and the high-temperature cracking process and separation and purification process included in it greatly increase the difficulty and cost of production.

Method used

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  • Preparation method of methyl phenyl hydrogen-containing silicone oil for LED packaging adhesive

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Experimental program
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Effect test

Embodiment 1

[0025] (1) Take 40g of hydrochloric acid with a mass fraction of 2.0% and add it to a four-necked flask equipped with mechanical stirring and temperature controller to preheat to 60°C, then add 50g of methylphenyldimethoxysilane at 60°C React for 2 hours. After the reaction is over, wash the product with distilled water for 3-4 times to neutrality, then transfer the product to a round-bottomed distillation flask and remove the water in the system at 80°C / -0.096MPa to obtain a colorless and transparent methyl phenyl hydroxyl terminated silicone oil.

[0026] (2) Take 30g of the above-prepared methyl phenyl hydroxyl-terminated silicone oil and add it to a three-necked flask equipped with mechanical stirring and a temperature controller to preheat to 60°C, and then add 0.89gMM H The end-capping agent and 0.31g CH-01 type acidic cationic resin were reacted at 60°C for 4 hours. After the reaction is over, remove the CH-01 type acidic cationic resin catalyst by suction filtration,...

Embodiment 2

[0028] (1) Take 40g of hydrochloric acid with a mass fraction of 2.0% and add it to a four-necked flask equipped with mechanical stirring and temperature controller to preheat to 60°C, then add 50g of methylphenyldimethoxysilane at 60°C React for 2 hours. After the reaction is over, wash the product with distilled water for 3-4 times to neutrality, then transfer the product to a round-bottomed distillation flask and remove the water in the system at 80°C / -0.096MPa to obtain a colorless and transparent methyl phenyl hydroxyl terminated silicone oil.

[0029] (2) Get 30g of the above-mentioned prepared methyl phenyl hydroxyl-terminated silicone oil and 15g of D 4 H Add it into a three-necked flask equipped with mechanical stirring and a temperature controller and preheat it to 60°C, then add 1gMM end-capping agent and 0.46gCH-01 type acidic cationic resin and react at 60°C for 4 hours. After the reaction is over, remove the CH-01 type acidic cationic resin catalyst by suction...

Embodiment 3

[0031] (1) Take 40g of hydrochloric acid with a mass fraction of 2.0% and add it to a four-necked flask equipped with mechanical stirring and temperature controller to preheat to 60°C, then add 50g of methylphenyldimethoxysilane at 60°C React for 2 hours. After the reaction is over, wash the product with distilled water for 3-4 times to neutrality, then transfer the product to a round-bottomed distillation flask and remove the water in the system at 80°C / -0.096MPa to obtain a colorless and transparent methyl phenyl hydroxyl terminated silicone oil.

[0032] (2) Take 30g of the above-mentioned prepared methyl phenyl hydroxyl-terminated silicone oil and 15g of D 4 H Add it to a three-necked flask equipped with mechanical stirring and a temperature controller, preheat to 60°C, and then add 1gMM H The end-capping agent and 0.46g CH-01 type acidic cationic resin were reacted at 60°C for 4 hours. After the reaction is over, remove the CH-01 type acidic cationic resin catalyst by...

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Abstract

The invention discloses a preparation method of methyl phenyl hydrogen-containing silicone oil for LED packaging adhesive. The method takes methyl phenyl dimethoxy silaneas raw material and hydrochloric acid or acid cationic resin as catalyst, and performs hydrolytic condensation reaction under the heating and stirring condition, and prepares methyl phenyl hydroxyl silicone oil; the prepared methyl phenyl hydrogen-containing silicone oil and tetramethyl tetralin cyclotetrasiloxane (D4H) as raw materials, hexamethyl disiloxane (MM) or hydrogen-containing dual-sealing end (MMH) as the end-capping reagent, and acid cationic resin as the catalyst; the reaction is carried out under the heating and stirring conditions; after finishing the reaction, catalyst is filtered and removed; and then the methyl phenyl hydrogen-containing silicone oil is obtained after depressurizing and distilling the product and removing the low-boiling-point substance. The prepared hydrogen-containing silicone oil is colorless and transparent thick fluid; the light transmittance, refractive index and activated hydrogen content are high, the thermal stability is good; besides, the methyl phenyl hydrogen-containing silicone oil can be used as the LED packaging material.

Description

technical field [0001] The invention relates to the technical field of LED packaging glue, in particular to a method for preparing methylphenyl hydrogen-containing silicone oil for LED packaging glue. Background technique [0002] Light-emitting diodes (LEDs) have a series of advantages such as stable performance, energy saving and high efficiency, safety and environmental protection, and are widely used in daily lighting, automotive lighting, mobile phones and televisions, and have become the trend and trend of future lighting technology. The selection of packaging materials is very important to the performance of LEDs. Silicone materials have become a key research direction for LED packaging materials at home and abroad due to their excellent thermal stability, aging resistance, mechanical properties, optical properties and moisture resistance. Therefore, the development of silicone packaging materials with excellent performance is of great significance to the improvement ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/08
CPCC08G77/12C08G77/08
Inventor 潘朝群袁强康英姿
Owner SOUTH CHINA UNIV OF TECH
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