MDQ phenyl vinyl silicone resin and preparation method thereof

A phenyl vinyl silicon and vinyl technology, which is applied in the field of MDQ type phenyl vinyl silicone resin and its preparation, can solve the problems of difficult phenyl monomer to continue to react, cannot be encapsulated with LED, and affects the transparency of products, etc. The effect of stable quality, mild production process conditions and high refractive index

Active Publication Date: 2015-03-25
SHENZHEN CITY SQUARE SILICONE MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this phenyl MDQ silicone resin does not contain vinyl or silicon-hydrogen bonds, and cannot be cured by hydrosilylation
[0007] Japanese patent JP07228701A discloses a synthesis method of MDQ silicone resin containing silicon hydrogen in the D chain segment. The synthesis process is: dissolving methyl MQ silicone resin in an organic solvent, performing dehydration condensation under acidic catalyst strips, and then reacting with linear Hydrogen-containing silicone oil carries out equilibrium reaction, obtains the structure as (Me 3 SiO 1 / 2 ) a (MeHSiO 2 / 2 ) y (Me 2 SiO 2 / 2 ) z (SiO 4 / 2 )'s D-link hydrogen-containing MDQ silicone resin, which does not contain phenyl groups and has a low refractive index, so it cannot be used for LED packaging with high luminous flux requirements
[0008] Since tetraethyl orthosilicate that provides the source of Q chains is prone to gelation reaction under acidic conditions, and the reaction speed of various monomers in alcohol solvents is different, tetraethyl orthosilicate and head-capping agent are hydrolyzed to form formazan After base MQ silicone resin, it is not easy to continue to react with phenyl monomer, thus affecting the final transparency of the product

Method used

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  • MDQ phenyl vinyl silicone resin and preparation method thereof

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preparation example Construction

[0024] The embodiment of the present invention also provides a preparation method of the above-mentioned MDQ type phenyl vinyl silicone resin, which includes the following steps:

[0025] S01: Mix 100-1000 parts by mass of diphenyldimethoxysilane and / or diphenyldiethoxysilane, 10-300 parts by mass of tetraethyl orthosilicate, and 50-500 parts by mass of organic solvent , stirred at room temperature to obtain a mixed solution;

[0026] S02: Add dropwise 20-300 parts by mass of an acidic aqueous solution to the mixed solution, heat up to 60°C-70°C for 4-6 hours after the dropwise addition, and then add 20-200 parts of vinyl capping agent and / or methyl capping agent, the temperature is maintained at 60°C-70°C for 6-8 hours to obtain a reaction solution, wherein the mass concentration of the acidic catalyst solution is 5%-15%;

[0027] S03: the reaction solution is left to stand for stratification, after removing the acid solution in the upper layer, adding alkali to adjust the ...

Embodiment 1

[0035] In a 2L three-necked flask filled with 200 parts by mass of methanol, add 444 parts by mass of diphenyldimethoxysilane and 189 parts by mass of ethyl orthosilicate, and dropwise add 45 parts by mass of A mixed solution composed of 25% hydrochloric acid and 150 parts by mass of deionized water was stirred thoroughly, and the dropwise addition was completed within half an hour, then the temperature was raised to 60-80°C and reacted for 5 hours, and then 111.6g of divinyltetramethyldisilica was added Oxygen capping agent, keep the temperature at 60-80°C, stop the reaction after 7 hours, cool to room temperature and then separate layers, add 5g sodium hydroxide to neutralize, wash to neutral, at 150°C, vacuum degree 0.9MPa~ Distilled under the condition of 1.0MPa for 3 hours to remove low-boiling point substances to obtain 512.0g of colorless and transparent MDQ type phenylvinyl silicone resin, with a viscosity of 7800mPa·s / 25°C, a refractive index of 1.5495 / 25°C, and a viny...

Embodiment 2

[0037] In a 1L three-neck flask containing 100 parts by mass of methanol, add 148 parts by mass of diphenyldimethoxysilane and 63 parts by mass of ethyl orthosilicate, and dropwise add a mass fraction of 30 parts by mass at 30°C. It is a mixed solution of 25% hydrochloric acid and 100 parts by mass of deionized water, fully stirred, and the dropwise addition is completed within half an hour, then the temperature is raised to 60-80°C for 5 hours, and 56.5g of divinyltetramethyldisiloxane is added Alkane head-capping agent, keep the temperature at 60-80°C, stop the reaction after 7 hours, cool to room temperature and then separate layers, remove the upper acid solution, add 2.5g sodium hydroxide to neutralize, wash with water until neutral, at 150°C, Distill for 3 hours under the condition of vacuum degree 0.9MPa~1.0MPa, remove low boiling point substances, and obtain 186g of colorless and transparent MDQ type phenylvinyl silicone resin, viscosity is 20000mPa·s / 25℃, refractive in...

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Abstract

The invention relates to MDQ phenyl vinyl silicone resin. The MDQ phenyl vinyl silicone resin has the structure shown in the following general formula: (Ph2SiO)a(ViMe2SiO0.5)b(Me3SiO0.5)c(SiO2)d, wherein Ph is phenyl, Me is methyl and Vi is vinyl; the a value ranges from 0.1 to 1, the (b+c) value ranges from 0 to 0.1, and b is larger than 0; the d value ranges from 0 to 0.8, and the sum of a, b, c and d is larger than 0; the value of (a/d) ranges from 1.6 to 2.5; and the value of [(b+c)/d] ranges from 1.6 to 2.5. The invention further provides a preparation method of the MDQ phenyl vinyl silicone resin. According to the method, the viscosity, the refractive index and the vinyl content of a product are controlled through conditions of monomer raw material ratio, the reaction time, temperature and pH value and the like, the manufacturing conditions are mild, simple and feasible, the raw material source is wide, and the repeatability is good.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to an MDQ type phenylvinyl silicone resin and a preparation method thereof. Background technique [0002] Silicone polymer materials such as silicone gel, silicone rubber, and silicone resin have the advantages of aging resistance, high and low temperature resistance, and ultraviolet radiation resistance, and are currently ideal packaging materials. Among them, phenyl silicone resin has been widely used in packaging processes such as LED SMT and Molding due to its high refractive index, good air permeability and water permeability, direct infusion, no need for plastic shells, and easy use. [0003] Phenyl silicone resin and organosilicon polymer containing silicon-hydrogen bonds undergo hydrosilation addition reaction under the action of platinum, cobalt and other metal catalysts to cross-link and vulcanize. The vulcanization conditions are mild and can be vulcanized rap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06
CPCC08G77/06C08G77/20
Inventor 李彦民罗建立
Owner SHENZHEN CITY SQUARE SILICONE MATERIALS
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