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A kind of preparation method of room temperature moisture curing silicone resin

A moisture-curing, silicone resin technology, applied in the field of silicone resins, to achieve the effect of easy availability, excellent adhesion and hardness, and improved storage stability

Active Publication Date: 2020-09-18
CHENGDU GUIBAO SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, there is no report on alkoxy-terminated and room-temperature moisture-curable silicone resins

Method used

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  • A kind of preparation method of room temperature moisture curing silicone resin
  • A kind of preparation method of room temperature moisture curing silicone resin
  • A kind of preparation method of room temperature moisture curing silicone resin

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preparation example Construction

[0031] A preparation method of room temperature moisture curing silicone resin, comprising the following steps:

[0032] Step A: Add the mixed solution of acidic catalyst and water to the mixed solution of difunctional siloxane monomer, trifunctional siloxane monomer and solvent, hydrolyze and react for 2-6 hours at a temperature of 25-70°C, and then raise High temperature to reflux reaction for 2-8 hours; then stand for stratification, wash the pre-polysilicone resin until neutral, then heat and rotary steam under reduced pressure to remove small molecular substances, and obtain pure pre-polysilicone resin;

[0033] Step B: adding solvent, alkoxy monomer and end-blocking catalyst to the pre-polysilicone resin, reacting at a temperature of 70-100° C. for 1-10 hours, and heating under reduced pressure to remove the catalyst and small molecules to obtain the silicone resin.

[0034] The following is a preference for the above scheme, wherein the difunctional siloxane monomer in ...

Embodiment 1

[0052] Add 35 parts of methyltrimethoxysilane, 55 parts of phenyltrimethoxysilane, 20 parts of dimethyldimethoxysilane and 30 parts of methylphenyldimethoxysilane into the three-necked flask, and stir for 10 minutes at room temperature ; Slowly add 120 parts of sulfuric acid aqueous solution with a mass fraction of 2% and 100 parts of isopropanol mixture dropwise under stirring at room temperature, and drop it for 60 minutes. After dropping, raise the temperature to 60°C and stir for 3 hours, then heat up to reflux for 6 hours After the reflux reaction is finished, cool to room temperature, and add 200 parts of toluene to stir and mix evenly, pour into a separatory funnel and add a large amount of deionized water, wash with water, leave to stand for layering, get the toluene phase and continue washing until the washing liquid is until neutral; after washing with water, add anhydrous magnesium sulfate to the toluene phase to further remove water, pour it into a single-necked fla...

Embodiment 2

[0056] Add 30 parts of methyltrimethoxysilane, 40 parts of phenyltrimethoxysilane, 30 parts of dimethyldimethoxysilane and 40 parts of methylphenyldimethoxysilane into the three-necked flask, and stir for 10 minutes at room temperature ; Slowly add 120 parts of sulfuric acid aqueous solution with a mass fraction of 2% and 100 parts of isopropanol mixture dropwise under stirring at room temperature, and drop it for 60 minutes. After dropping, raise the temperature to 60°C and stir for 3 hours, then heat up to reflux for 6 hours After the reflux reaction is finished, cool to room temperature, and add 200 parts of toluene to stir and mix evenly, pour into a separatory funnel and add a large amount of deionized water, wash with water, leave to stand for layering, get the toluene phase and continue washing until the washing liquid is until neutral; after washing with water, add anhydrous magnesium sulfate to the toluene phase to further remove water, pour it into a single-necked fla...

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Abstract

The invention discloses a preparation method for room-temperature moisture curable silicone resin. The method comprises the following steps: adding an acidic catalyst to a mixed solution of a difunctional organic siloxane monomer, a trifunctional organic siloxane monomer and a solvent, performing a hydrolysis reaction for 2-6h at the temperature of 25-70 DEG C, then raising the temperature, and performing a reflux reaction for 2-8h; then allowing the obtained material to stand for layering, washing pre-polymerization silicon resin until the resin is neutral, performing decompression and heating, and performing rotary evaporation to remove small-molecular matter to obtain pure pre-polymerization silicon resin; and adding a solvent, an alkoxy monomer and an end-capping catalyst into the pre-polymerization silicon resin, performing a reaction for 1-10h under the conditions of the reflux temperature, performing washing with water to remove the catalyst, performing decompression and heating, and performing rotary evaporation to obtain the silicone resin. The room-temperature moisture curable silicone resin provided by the invention has high reaction activity, can be quickly cured in a curing agent and a moisture environment, has high hardness and good adhesion after being cured at the surface of a cold rolled steel plate, and can effectively protect a substrate.

Description

technical field [0001] The invention relates to the technical field of silicone resins, in particular to a method for preparing room temperature moisture-cured silicone resins. Background technique [0002] For a long time, silicone resin has different properties from other silicone products due to its special molecular structure, such as high hardness, weather resistance, oil resistance, hydrophobicity and other excellent properties. It is widely used in aerospace, food industry and construction industry. , Electronic appliances and other fields have a wide range of applications. [0003] The silicone resins that are widely used in industry today are mainly methyl silicone resin, methyl phenyl silicone resin and phenyl silicone resin. Some silicone resins, but most of these silicone resins use heat curing to cross-link the silicone resin into a film or make industrial products; some substrates will deform or change in performance when heated, and large workpieces will be h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06
CPCC08G77/06C08G77/80
Inventor 陈良兵陈贵荣王玉坤黄强王有治
Owner CHENGDU GUIBAO SCI & TECH