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A kind of single-end capping method of double-end perfluoropolyether alcohol

A perfluoropolyether alcohol and perfluoropolyether technology, which is applied in the field of preparation of single-ended perfluoropolyether alcohol, can solve the problem of unclear perfluoropolyether content, complicated preparation process, double-ended perfluoropolyether silicone Problems such as poor lubricity of alkanes

Active Publication Date: 2022-05-06
苏州东杏表面技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] WO099085 discloses a preparation of single-end Z-type perfluoropolyether siloxane with fluorine gas, and pointed out that the double-end perfluoropolyether siloxane has poor lubricity and the smoothness of K-type perfluoropolyether siloxane bad question
[0004] CN106146820A discloses a kind of use perfluoroalkyl iodide to capping double-end perfluoropolyether allyl ether, although the fluorine content of molecular chain can be increased, but the content of perfluoropolyether with single-end structure is not clear, and not separated
The preparation process of this method is complicated, and the end-capped compound needs to be separated to obtain a single-end active perfluoropolyether
[0006] CN108463482A discloses a preparation method and application of hydroxyl-terminated (per)fluoropolyether polymer derivatives containing carbamate moieties, but this end-capping method does not have unity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 1 g of the raw material Fomblin D2500 perfluoropolyether alcohol in 19 g of perfluorohexane, add 180 g of toluene, place it in a 250 ml flask, control the temperature at 5°C, stir vigorously to form an emulsion, add 10 g to dissolve 32 milligrams of acetyl chloride and continued stirring, keeping nitrogen flowing through the reaction flask, continuing the reaction for 10 minutes, standing to separate layers, obtaining the lower layer solution and evaporating the solvent to obtain the product.

Embodiment 2

[0025] Dissolve 1 g of the raw material Fomblin D2500 perfluoropolyether alcohol in 19 g of perfluorohexane, add 180 g of chloroform, place it in a 250 ml flask, control the temperature at 5°C, stir vigorously to form an emulsion, add 10 g to dissolve With 32 mg of acetyl chloride and continuous stirring, nitrogen gas was kept flowing through the reaction flask, the reaction was continued for 10 minutes, and the layers were left to stand to obtain the lower layer solution and evaporate the solvent to obtain the product.

Embodiment 3

[0027] Dissolve 1 g of the raw material Fomblin D2500 perfluoropolyether alcohol in 19 g of perfluorooctane, add 180 g of chloroform, place it in a 250 ml flask, control the temperature at 5°C, stir vigorously to form an emulsion, add 10 g to dissolve With 32 mg of acetyl chloride and continuous stirring, nitrogen gas was kept flowing through the reaction flask, the reaction was continued for 10 minutes, and the layers were left to stand to obtain the lower layer solution and evaporate the solvent to obtain the product.

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PUM

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Abstract

The invention discloses a single-end capping method of double-end perfluoropolyether alcohols, and belongs to the technical field of preparation of single-end perfluoropolyether alcohols. In this method, the double-terminal perfluoropolyether alcohol is dissolved in a fluorinated solvent, and an emulsion is formed with a second organic solvent, and the second organic solvent is immiscible with the fluorinated solvent; and then the acid chloride reagent solution is continuously added under nitrogen protection, The acid chloride reagent solution is a solution obtained by dissolving the metered ratio of the acid chloride reagent in the second organic solvent; after the reaction, a single-end perfluoropolyether alcohol capped by esterification at one end is obtained; the two-end perfluoropolyether alcohol is The concentration in the fluorine-containing solvent is 1wt.%-10wt.%, and the mass ratio of the fluorine-containing solvent to the poor second organic solvent is 1:5-1:20. The invention uses double-end perfluoropolyether alcohols as raw materials, and selectively esterifies acid chlorides with hydroxyl groups at one end by controlling its distribution in a solution, thereby obtaining single-end perfluoropolyether alcohols.

Description

technical field [0001] The invention belongs to the technical field of preparation of single-end perfluoropolyether alcohols, and in particular relates to a single-end capping method of double-end perfluoropolyether alcohols. Background technique [0002] The fluorine-containing siloxane compound can react with the hydroxyl groups on the surface of the substrate to form a film with amphiphobic properties (neither lipophilic nor hydrophilic), which can prevent dirt such as moisture or oil from adhering, And it increases the surface sliding property, thereby improving the surface wear resistance. It is a surface layer with anti-fouling and wear-resistant properties. It has been widely used in lenses, mobile phones and tablet computer displays. [0003] WO099085 discloses a preparation of single-end Z-type perfluoropolyether siloxane with fluorine gas, and pointed out that the double-end perfluoropolyether siloxane has poor lubricity and the smoothness of K-type perfluoropolyet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/331C08G65/48
CPCC08G65/331C08G65/48
Inventor 许波连何丽蓉王兴张黎斌张俊江
Owner 苏州东杏表面技术有限公司