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MDQ phenyl hydrogen-containing silicon resin and preparing method thereof

A technology of phenyl hydrogen-containing silicon and resin, which is applied in the field of polymer materials, can solve the problems of not being able to use LED packaging, low refractive index, and inability to add curing, etc., to achieve mild production process conditions, wide sources of raw materials, and high refractive index Effect

Inactive Publication Date: 2015-09-09
SHENZHEN CITY SQUARE SILICONE MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this phenyl MDQ silicone resin does not contain vinyl or silicon-hydrogen bonds, and cannot be cured by addition
[0008] 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
[0009] 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 hydrogen-containing silicon resin and preparing method thereof
  • MDQ phenyl hydrogen-containing silicon resin and preparing method thereof
  • MDQ phenyl hydrogen-containing silicon resin and preparing method thereof

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preparation example Construction

[0025] see figure 1 , The second embodiment of the present invention also provides a method for preparing the MDQ type phenyl hydrogen-containing silicone resin, which includes the following steps:

[0026] S101, mix and stir 50-1100 parts by mass of phenylalkoxy monomer, 10-500 parts of tetraethyl orthosilicate, and 50-500 parts of organic solvent, and dropwise add 20-300 parts of Water and 10-200 parts of acidic catalyst mixed solution with a mass concentration of 25%.

[0027] Specifically, 50-1000 parts by mass of diphenyldimethoxysilane monomer, 0-100 parts of dimethyldiethoxysilane monomer, 10-500 parts of ethyl orthosilicate , 50-500 parts of organic solvents are put into a three-necked flask, cooled in water bath, stirred, and 20-300 parts of water and 10-200 parts of hydrochloric acid catalyst mixed solution with a mass concentration of 25% are added dropwise thereto.

[0028] Specifically, the phenylalkoxy monomer includes at least one of diphenyldimethoxysilane an...

Embodiment 1

[0040] Add 256 parts of diphenyldimethoxysilane, 180 parts of ethyl orthosilicate, and 90 parts of dimethyldiethoxysilane to a 2L three-necked flask with 150 parts of methanol, and add 37 parts dropwise at 30°C. Parts of hydrochloric acid with a mass fraction of 25% and 133 parts of deionized water were fully stirred, and the dropwise addition was completed within half an hour, and then the temperature was raised to react for 5 hours, and then 76 parts of tetramethyldisiloxane capping agent was added, and the temperature was kept at 60~ 80°C, stop the reaction after 7 hours, cool to room temperature, then layered and wash with water until neutral, distill at 120°C for 3 hours under the condition of a vacuum of 0.9MPa~1.0MPa, remove low boiling point substances, and obtain colorless transparent benzene Base hydrogen-containing silicone resin 300g, viscosity 10000mPa.s / 25°C, refractive index 1.5214 / 25°C, hydrogen content 0.25% (m / m).

Embodiment 2

[0042] Add 350 parts of diphenyldimethoxysilane, 180 parts of ethyl orthosilicate, and 70 parts of dimethyldiethoxysilane to a 2L three-necked flask containing 150 parts of methanol, and add 42 parts dropwise at 30°C. Parts of hydrochloric acid with a mass fraction of 25% and 145 parts of deionized water were fully stirred, and the dropwise addition was completed within half an hour, and then the temperature was raised to react for 5 hours, and then 85 parts of tetramethyldisiloxane capping agent was added, and the temperature was kept at 60~ 80°C, stop the reaction after 7 hours, cool to room temperature, then layered and wash with water until neutral, distill at 120°C for 3 hours under the condition of a vacuum of 0.9MPa~1.0MPa, remove low boiling point substances, and obtain colorless transparent benzene Based on 350g of hydrogen-containing silicone resin, the viscosity is 30000mPa.s / 25°C, the refractive index is 1.52 / 25°C, and the hydrogen content is 0.24% (m / m).

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Abstract

The invention belongs to the technical field of polymer materials and provides MDQ phenyl hydrogen-containing silicon resin, having a general molecular formula: (Ph2SiO)a(Me2SiO)b(HMe2SiO0.5)c(Me3SiO0.5)d(SiO2)e. Ph is phenyl-C6H5, Me is methyl-CH3, (a+b) is valued from 0.2 to 1, a is greater than 0.2, (c+d) is valued from 0 to 0.1, c is greater than 0, and e is valued from 0 to 0.8. The invention further provides a preparing method of the MDQ phenyl hydrogen-containing silicon resin. The preparing method has the advantages that product viscosity, refractive index, hydrogen end plate agent content and the like can be controlled under the conditions such as monomer ratio, reaction time, temperature and pH, and thus the materials with the corresponding Phenyl vinyl silicone resin are made into products different in hardness and mechanical strength.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to an MDQ type phenyl hydrogen-containing 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/06
Inventor 李彦民罗建立
Owner SHENZHEN CITY SQUARE SILICONE MATERIALS
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