Preparation method of perfluoropolyfluoroether fluorosilane with plurality of hydrolytically-active end groups

A perfluoropolyether-based, fluorosilane-based technology, used in biocide-containing paints, antifouling/underwater coatings, coatings, etc., can solve the problems of inflammability and explosion, difficult to obtain raw materials, low surface tension and other problems

Active Publication Date: 2017-09-29
太仓中化环保化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN104769009 discloses a method for simultaneously grafting four alkoxysilane functions at the end of the perfluoropolyether molecular chain. The treated surface has both extremely low surface tension and excellent wear resistance. However, the preparation of the compound The raw materials used are not easy to obtain and are flammable and explosive; therefore, it is very necessary to find a new method with mature, safe and easy-to-get raw materials, and mild and safe process conditions to prepare perfluoropolyfluorocarbons with multiple hydrolytically active end groups. Ether Fluorosilane

Method used

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  • Preparation method of perfluoropolyfluoroether fluorosilane with plurality of hydrolytically-active end groups
  • Preparation method of perfluoropolyfluoroether fluorosilane with plurality of hydrolytically-active end groups
  • Preparation method of perfluoropolyfluoroether fluorosilane with plurality of hydrolytically-active end groups

Examples

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Embodiment 1

[0075] This embodiment provides a method for preparing perfluoropolyfluoroether-based fluorosilane with multiple hydrolysis active end groups, comprising the following steps:

[0076] (1) In a four-neck flask equipped with a reflux condenser, nitrogen purging, strong stirring and temperature control device, add 100.0g vinyl-terminated perfluoropolyether (molecular weight: 1684g / mol, Taicang Sinochem Environmental Protection Chemical Co., Ltd. Provided, the general structural formula is: F(CFCF 3 CF 2 O) 9 CFCF 3 CH 2 OCH 2 CH=CH 2 ), 6.3g methyldimethoxyhydrogensilane and 110.0g m-ditrifluorotoluene, stirred evenly at room temperature, and added 1g Karstedt type platinum catalyst VM-23 (Pt content is 3000ppm, Zhejiang Quzhou Jiancheng Organic Silicon Material Co., Ltd. Provided by the company), gradually raise the temperature to 80°C, then keep the temperature for 8 hours, and finally remove the low boiling point for 2 hours under a vacuum of 0.2KPa to obtain the product...

Embodiment 2

[0089] This example provides a method for preparing a perfluoropolyfluoroether-based fluorosilane with multiple hydrolysis active end groups, referring to the method and steps in Example 1, the difference is that the vinyl-terminated perfluoropolyether in the formula The specification is changed to: the molecular weight is 3510g / mol, provided by Taicang Sinochem Environmental Protection Chemical Co., Ltd., and the general structural formula is: F(CFCF 3 CF 2 O) 20 CFCF 3 CH 2 OCH 2 CH=CH 2 , and the corresponding mass is replaced with 209g.

[0090] The perfluoropolyfluoroether fluorosilane prepared in this example is denoted as PFPE-FS-2, and its structural formula conforms to that shown in formula V, in formula V: a=1, b=4, c=4, d=3, e=20, g=3, X=CFCF 3 CH 2 OCH 2 CH 2 CH 2 , Y=CH 2 CH 2 CH 2 , R 1 =OC 2 h 5 .

Embodiment 3

[0092] This example provides a method for preparing a perfluoropolyfluoroether-based fluorosilane with multiple hydrolysis active end groups, referring to the method and steps in Example 1, the difference is that the vinyl-terminated perfluoropolyether in the formula The specification is changed to: the molecular weight is 5170g / mol, provided by Taicang Sinochem Environmental Protection Chemical Co., Ltd., and the general structural formula is: F(CFCF 3 CF 2 O) 30 CFCF 3 CH 2 OCH 2 CH=CH 2 , and the corresponding mass is replaced with 307g.

[0093] The perfluoropolyfluoroether fluorosilane prepared in this example is denoted as PFPE-FS-3, and its structural formula conforms to that shown in formula V, in formula V: a=1, b=4, c=4, d=3, e=30, g=3, X=CFCF 3 CH 2 OCH 2 CH 2 CH 2 , Y=CH 2 CH 2 CH 2 , R 1 =OC 2 h 5 .

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Abstract

The invention relates to a preparation method of perfluoropolyfluoroether fluorosilane with a plurality of hydrolytically-active end groups. The preparation method comprises the following steps: performing an addition reaction of vinyl-terminated perfluoropolyether and dialkoxyfluorosilane in the presence of a fluorine-containing solvent and a catalyst to obtain perfluoropolyether fluoroalkyl silane; performing a hydrolysis reaction on the perfluoropolyether fluoroalkyl silane to obtain a perfluoropolyether fluoroalkyl silane hydrolysate; reacting the perfluoropolyether fluoroalkyl silane hydrolysate with polyvinylsilicone oil in the presence of an alkali catalyst to obtain vinyl perfluoropolyether fluorosilicone oil; performing an addition reaction of the vinyl perfluoropolyether fluorosilicone oil and trialkoxyhydrosilane in the presence of a fluorine-containing solvent and a catalyst to obtain the perfluoropolyfluoroether fluorosilane. The preparation method has the advantages of adoption of readily-available raw materials and mild and safe process conditions; the defects that raw materials are difficult to obtain and are flammable and combustible in the prior art are overcome.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a preparation method of perfluoropolyfluoroether-based fluorosilane with multiple hydrolysis active end groups. Background technique [0002] Materials such as ceramics, glass, and metals contain a large number of polar functional hydroxyl groups (-OH) on the surface, so it is very easy to adhere to pollutants such as water droplets, oil stains, fingerprints, grease, and cosmetics, resulting in a serious decrease in their appearance and transparency. Especially when these materials are used in touch screens, displays and cameras of electronic products such as mobile phones, cameras and computers, optical lenses of glasses such as myopia, farsightedness and labor protection, front windshields and rearview mirrors of automobiles, high-rise building glass and When displaying windows, stainless steel handrails of stairs, and surfaces such as sanitary ceramics and shower r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C09D183/12C09D5/16
CPCC08G77/46C09D5/165C09D183/12
Inventor 徐涛吴克安王祎诚
Owner 太仓中化环保化工有限公司
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