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A kind of mdq type phenyl vinyl silicone resin and preparation method thereof

A technology of phenylvinylsilicon and diphenyldiethoxysilane, which is applied in the field of MDQ type phenylvinylsilicon resin and its preparation, can solve the problem that phenyl monomers are not easy to continue to react, cannot be packaged with LEDs, and affect Product transparency and other issues, to achieve the effect of stable quality, mild production process conditions, high refractive index

Active Publication Date: 2016-02-24
SHENZHEN CITY SQUARE SILICONE MATERIALS
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  • Summary
  • 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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  • A kind of mdq type phenyl vinyl silicone resin and preparation method thereof

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

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

[0026] S02: dropwise add 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 kept at 60°C to 70°C for 6 to 8 hours to obtain a reaction solution, wherein the mass concentration of the acidic catalyst solution is 5% to 15%;

[0027] S03: the reaction solution is left to stand for stratification, and after removing the upper layer of acid solution, an alkali is added to adjust ...

Embodiment 1

[0035] Into a 2L three-necked flask containing 200 parts by mass of methanol, 444 parts by mass of diphenyldimethoxysilane and 189 parts by mass of ethyl orthosilicate were added dropwise at 30°C from 45 parts by mass to A mixed solution composed of 25% hydrochloric acid and 150 parts by mass of deionized water was fully stirred, and the dropwise addition was completed within half an hour, and then the temperature was raised to 60-80 ° C for 5 hours, and then 111.6g of divinyltetramethyldisiloxane was added. Oxane head capping agent, keep the temperature at 60~80℃, stop the reaction after 7 hours, cool to room temperature and then layer, add 5g sodium hydroxide to neutralize, wash with water until neutral, at 150℃, vacuum degree 0.9MPa~ Distilled for 3 hours under the condition of 1.0MPa to remove low-boiling point substances to obtain 512.0g of colorless and transparent MDQ type phenyl vinyl silicone resin with viscosity of 7800mPa·s / 25℃, refractive index of 1.5495 / 25℃, vinyl ...

Embodiment 2

[0037] Into a 1L three-necked flask containing 100 parts by mass of methanol, 148 parts by mass of diphenyldimethoxysilane and 63 parts by mass of ethyl orthosilicate were added, and a mass fraction of 30 parts by mass was added dropwise 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, and then the temperature is raised to 60-80 ° C for 5 hours, and 56.5g of divinyltetramethyldisiloxane is added. Alkane capping agent, keep the temperature at 60 ~ 80 ℃, stop the reaction after 7 hours, cool to room temperature, then layer, remove the upper layer of acid, add 2.5g sodium hydroxide to neutralize, wash with water until neutral, at 150 ℃, Distilled for 3 hours under the condition of vacuum degree of 0.9MPa~1.0MPa to remove low boiling point substances to obtain 186g of colorless and transparent MDQ type phenyl vinyl silicone resin with viscosity of 20000mPa·s / ...

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Abstract

The present invention relates to MDQ phenyl vinyl silicone resin. The MDQ phenyl vinyl silicone resin has a structure represented by 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 value of a ranges from 0.1 to 1; the value of b+c ranges from 0 to 0.1, and b>0; the value of d ranges from 0 to 0.8, and a+b+c+d>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 present invention also provides a method for preparing 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 such as the monomer raw material ratio, the reaction time, the temperature and the pH value, 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 phenyl vinyl 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 the advantages of high refractive index, good air permeability and water permeability, direct infusion, no need for plastic shell, and convenient use. [0003] Phenyl silicone resin and silicone polymer containing silicon hydrogen bond undergo hydrosilation addition reaction under the action of platinum, cobalt and other metal catalysts to cross-link vulcanization. The vulcanization conditions are mild, and it can be quickly vulcanized at medium temperature. Low molecular weight and oth...

Claims

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Application Information

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Patent Type & Authority Patents(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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