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A kind of ester ring epoxy acrylate hybrid silicone resin, preparation method and application

A technology of ester ring epoxy acrylate and hybrid silicon, applied in the field of polymer coating materials, can solve problems such as good adhesion, and achieve the effects of good adhesion, high water contact angle and fast light curing speed

Active Publication Date: 2022-06-07
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a kind of ester ring epoxy acrylate hybrid silicone resin, preparation method and application, and the coating prepared after compounding with multifunctionality acrylate resin, not only has excellent Excellent wear resistance and scratch resistance, and the surface of the coating is not prone to defects, with high light transmittance and good adhesion

Method used

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  • A kind of ester ring epoxy acrylate hybrid silicone resin, preparation method and application
  • A kind of ester ring epoxy acrylate hybrid silicone resin, preparation method and application
  • A kind of ester ring epoxy acrylate hybrid silicone resin, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Preparation of acryloyloxy-containing siloxane

[0057] To a four-necked flask equipped with a stirrer, a reflux condenser and a thermometer, 24.6 g (0.1 mol) of 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 7.2 g (0.1 mol) of acrylic acid were added. ), 0.16 g of trimethylbenzyl ammonium chloride, 0.16 g of hydroquinone and 10 g of methyl ethyl ketone, stirred and reacted in an oil bath at 80°C for 6 hours, then washed with n-hexane three times, and distilled under reduced pressure. Acryloyloxy-containing siloxane (A1) was obtained.

[0058] (2) Preparation of Ester Ring Epoxy Acrylate Hybrid Silicone Resin

[0059] To a 100 mL four-necked flask equipped with a reflux condenser, a dropping funnel and a thermometer, add 31.8 g (0.1 mol) of acryloxy-containing siloxane (A1), 4.8 g ( 0.04 mol), 30.1 g (0.2 mol) of ethyltrimethoxysilane, 4.2 g (0.02 mol) of tetraethyl silicate, 10 g of isopropanol and 0.9 g of hydroquinone, the mixture was stirred uniformly and heate...

Embodiment 2

[0063] (1) Preparation of acryloyloxy-containing siloxane

[0064] Add 34.6g (0.12mol), 7.2g (0.1mol) acrylic acid, 0.38g triphenylphosphine, 0.38g p-benzoquinone and 12g xylene to a four-necked flask equipped with a stirrer, a reflux condenser and a thermometer. The reaction was stirred in an oil bath at 85° C. for 6.5 hours, then washed with n-hexane three times, and distilled under reduced pressure to obtain an acryloxy-containing siloxane (A2).

[0065] (2) Preparation of Ester Ring Epoxy Acrylate Hybrid Silicone Resin

[0066] To a 100 mL four-necked flask equipped with a reflux condenser, a dropping funnel and a thermometer, add 36.0 g (0.1 mol) of acryloxy-containing siloxane (A2), 8.9 g ( 0.06mol), methyltriethoxysilane 39.2g (0.22mol), tetraethyl silicate 6.3g (0.03mol), ethyl acetate 12g and p-benzoquinone 0.8g, the mixture was stirred well and heated to 45°C . A mixture of a small amount of concentrated sulfuric acid 0.18 g and distilled water 21.6 g (1.2 mol) wa...

Embodiment 3

[0070] (1) Preparation of acryloyloxy-containing siloxane

[0071] The acryloyloxy-containing siloxane (A1) was prepared by the procedure in Example 1.

[0072] (2) Preparation of Ester Ring Epoxy Acrylate Hybrid Silicone Resin

[0073] To a 100 mL four-necked flask equipped with a reflux condenser, a dropping funnel and a thermometer, add 31.8 g (0.1 mol) of acryloxy-containing siloxane (A1), 8.8 g (0.1 mol) of diethyldiethoxysilane ( 0.05mol), propyltriethoxysilane 30.9g (0.15mol), tetramethyl silicate 4.6g (0.03mol), xylene 11g and p-hydroxyanisole 0.6g, the mixture was stirred and heated to 40 °C. A mixture of a small amount of glacial acetic acid 0.18 g and distilled water 17.82 g (0.99 mol) was added dropwise to the flask within 1 h. The temperature of the reaction mixture was then increased to 60°C and the reaction was stirred for 8 hours. Then, 6.50 g (0.04 mol) of hexamethyldisiloxane was added to the flask, the temperature was raised to 70° C., and the reaction w...

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Abstract

The invention provides an ester ring epoxy acrylate hybrid silicone resin, a preparation method and its application, and belongs to the field of polymer coating materials. The preparation method of the ester ring epoxy acrylate hybrid silicone resin comprises: Add hexyl siloxane, acrylic acid, catalyst I, polymerization inhibitor and solvent I into the reaction vessel, heat up and stir for reaction, wash with n-hexane, and distill under reduced pressure to obtain acryloxy-containing siloxane; Mix acyloxy siloxane, difunctional siloxane, trifunctional siloxane, tetrafunctional siloxane, solvent II and polymerization inhibitor, drop the mixture of catalyst II and deionized water, heat up and stir After reacting for 2 to 8 hours, add hexamethyldisiloxane, continue to heat up and stir for 2 to 5 hours; then stand to separate layers, wash the oil layer with water until neutral, and distill under reduced pressure to remove small molecular substances to obtain the product. Applying it to plastic substrates can improve its service life, higher water contact angle, and better antifouling performance.

Description

technical field [0001] The invention relates to the field of polymer coating materials, in particular to an ester ring epoxy acrylate hybrid silicone resin, a preparation method and an application. Background technique [0002] Silicone resin has many excellent physical and chemical properties, such as high hardness, high and low temperature resistance, oxidation resistance, weather resistance, etc., and has a wide range of applications in electronic devices, construction, aviation, aerospace, medical materials and other fields. Although silicone resins have more excellent properties than polyurethane resins, epoxy resins, and acrylate resins, their high cost often limits their individual applications. Ultraviolet-curing (UV) coatings have attracted more and more attention due to their unique advantages such as room temperature curing, wide adaptability, low energy consumption, high efficiency and environmental protection, and are especially suitable for surface treatment of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/18C09D175/14C09D183/06C08J7/04C08L67/02C08L27/06C08L69/00C08L23/06
CPCC08G77/18C09D175/14C08J7/0427C08G2150/00C08J2367/02C08J2327/06C08J2369/00C08J2323/06C08J2475/14C08J2483/06C08L83/06
Inventor 李小杰吕朝龙顾正明徐健刘晓亚
Owner JIANGNAN UNIV