High-temperature-resistant fluorocarbon modified organic silicon resin as well as preparation method and application thereof

A fluorocarbon modification, silicone technology, used in coatings, polyester coatings, anti-corrosion coatings, etc., to achieve excellent high temperature resistance, improve hydrophobicity, and enhance impact resistance.

Active Publication Date: 2022-05-17
黄山佳杰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, when using the above-mentioned types of prior art to modify silicone resins, while improving several other performance aspects, they will all be affected to a certain extent Sacrifice the heat resistance of silicone resin, therefore, it is necessary to provide a new modified silicone resin with multiple properties

Method used

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  • High-temperature-resistant fluorocarbon modified organic silicon resin as well as preparation method and application thereof
  • High-temperature-resistant fluorocarbon modified organic silicon resin as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 2664g of D4H, 5760g of D4, and 972g of hexamethyldisiloxane into the reactor, add 94g of concentrated sulfuric acid as a catalyst, and continue the reaction at 35°C until the D4 content in the system is less than 10%.

[0041] Distill the unreacted D4 in the system, add 469g of sodium bicarbonate to remove the remaining acid value until the acid value is less than 0.3mgKOH / g, filter and remove the solid to obtain intermediate A1, divide intermediate A1 into two parts, and mark them as Aa1, Ab1;

[0042] Add 1270g of heptafluorobutyl acrylate to 3100g of intermediate Aa1, add 200ppm of platinum catalyst after raising the temperature to 70°C, add 174g of allyl alcohol after a period of reaction, and continue the reaction until the infrared spectrum detects that the Si-H bond is complete After disappearing, add 684g of caprolactone and react at 130°C until the caprolactone is detected by HPLC After the reaction is complete, add 300g of succinic anhydride and react at 1...

Embodiment 2

[0046] Add 2880g of D4H, 12432g of D4, and 972g of hexamethylsiloxane into the system, add 162g of concentrated sulfuric acid as a catalyst, and continue the reaction at 35°C until the D4 content in the system is less than 10%.

[0047] Distill the unreacted D4 in the system, add 814g of sodium bicarbonate to remove the remaining acid value until the acid value is less than 0.3mgKOH / g, filter and remove the solid to obtain intermediate A2, divide intermediate A2 into two parts, and mark them as Aa2, Ab2;

[0048] Add 762g of heptafluorobutyl acrylate to 5428g of intermediate Aa2, add 200ppm of platinum catalyst after heating up to 70°C, add 58g of allyl alcohol after a period of reaction, and continue the reaction until the infrared spectrum detects that the Si-H bond is complete After disappearing, add 114g of caprolactone and react at 130°C until HPLC detects that the reaction of caprolactone is complete, then add 100g of succinic anhydride and react at 110°C until the chang...

Embodiment 3

[0052] Add 2760g of D4H, 10104g of D4, and 972g of hexamethylsiloxane into the system, add 138g of concentrated sulfuric acid as a catalyst, and continue the reaction at 35°C until the D4 content in the system is less than 10%.

[0053] Distill the unreacted D4 in the system, add 692g of sodium bicarbonate to remove the remaining acid value until the acid value is less than 0.3mgKOH / g, filter and remove the solid to obtain intermediate A3, divide intermediate A3 into two parts, and mark them as Aa3, Ab3;

[0054] Add 762g of heptafluorobutyl acrylate to 4612g of intermediate Aa3, add 200ppm of platinum catalyst after heating up to 70°C, add 290g of allyl alcohol after a period of reaction, and continue the reaction until the Si-H bond completely disappears by infrared detection Finally, add 1140g of caprolactone and react at 130°C until HPLC detects that the reaction of caprolactone is complete, then add 500g of succinic anhydride and react at 110°C until the acid value change...

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Abstract

The invention relates to high-temperature-resistant fluorocarbon modified organic silicon resin and a preparation method and application thereof.The structure of the fluorocarbon modified organic silicon resin is shown in the general formula I. The organic silicon resin is modified through fluorocarbon chain segment grafting, so that the modified organic silicon resin has the excellent high-temperature-resistant effect, and the high-temperature-resistant performance of the organic silicon resin is improved; the water contact angle of a coating containing the high-temperature-resistant fluorocarbon modified organic silicon resin exceeds 105 degrees after the coating is cured, and the coating has excellent hydrophobicity. The invention also discloses a preparation method of the fluorocarbon modified organic silicon resin and an application of the fluorocarbon modified organic silicon resin in a coating.

Description

technical field [0001] The invention relates to the field of organosilicon materials, in particular to organosilicon resins modified by fluorocarbons and their preparation methods and applications. Background technique [0002] Silicone resin is a highly cross-linked network polyorganosiloxane, usually made of methyltrichlorosilane, dimethyldichlorosilane, phenyltrichlorosilane, diphenyldichlorosilane or methylbenzene In the presence of organic solvents such as toluene, various mixtures of dichlorosilanes are hydrolyzed at lower temperatures to obtain acidic hydrolyzates. The initial products of hydrolysis are a mixture of cyclic, linear and crosslinked polymers, usually also containing a considerable number of hydroxyl groups. The hydrolyzate is washed with water to remove the acid, and the neutral primary polycondensate is thermally oxidized in air or further polycondensed in the presence of a catalyst to form a highly cross-linked three-dimensional network structure. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/385C09D167/00C09D5/08
CPCC08G77/38C08G77/385C09D167/00C09D5/08C09D5/18C08L83/04
Inventor 俞介兵许俊杰曹汪洋
Owner 黄山佳杰新材料科技有限公司
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