Catalyst-free method for preparing polysiloxane perfluoropolyether

A polysiloxane and perfluoropolyether technology, which is applied in the field of chemical materials and surface treatment of substrates, can solve the problems of low yield of hydrosilylation, easy to form gel, easy to be wiped off, etc., so as to save consumption , the effect of strong adhesion

Active Publication Date: 2016-04-13
TIANJIN RIJIN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN103665022A discloses a perfluoropolyether siloxane anti-fingerprint liquid prepared by catalysis of chloroplatinic acid, but the Pt catalyst is easily poisoned, and the reaction system is easy to form gel, resulting in low hydrosilylation yield
Easily wipes off during use

Method used

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  • Catalyst-free method for preparing polysiloxane perfluoropolyether
  • Catalyst-free method for preparing polysiloxane perfluoropolyether
  • Catalyst-free method for preparing polysiloxane perfluoropolyether

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preparation example Construction

[0026] A catalyst-free preparation method for polysiloxane perfluoropolyether, the steps of the method are as follows:

[0027] ⑴Preparation of perfluoropolyether acrylate

[0028] Add excess thionyl chloride dropwise to perfluoropolyether carboxylic acid in a three-necked flask, then add a certain amount of solvent, and react with magnetic stirring at 60-80°C for 4-7 hours. After washing, excess thionyl chloride is distilled off under reduced pressure to obtain perfluoropolyether acid chloride. According to the molar ratio of 1:1-1.5, add perfluoropolyether acid chloride and hydroxyl-containing acrylate compound into a three-necked flask, and react at room temperature for several hours under the protection of nitrogen. Washing, and distilling off excess acrylate compound under reduced pressure to obtain product 1, perfluoropolyether acrylate. The reaction equation is as follows:

[0029]

[0030] Rf is perfluoropolyether: CF 3 CF 2 CF 2 O(CF(CF 3 ) CF 2 O) n , n=1...

example 1

[0046] Synthesis 1. Rf-COOCH 2 C(CH 2 OCOCH 2 CH 2 NH(CH 2 ) 3 Si(OCH 3 ) 3 ) 3

[0047] Under nitrogen protection, PFPE-PETA (3 g, 0.000920 mol) and 3-aminopropyltrimethoxysilane (0.165, 0.000920 mol) were added to a 100 ml three-neck flask equipped with a magnetic stirring rotor, a nitrogen inlet and a reflux condenser. Stir at room temperature for 20 min, then stir at 55°C for 16 h, wash and distill under reduced pressure to obtain a yellow-brown viscous oil (PFPE-PETA-APS-3000).

example 2

[0049] Synthesis 2.

[0050] Rf-COOCH 2 C(CH 2 OCOCH 2 CH 2 N(CH 2 C(CH 3 )COO(CH 2 ) 3 Si(OCH 3 ) 3 )(CH 2 ) 3 Si(OCH 3 ) 3 ) 3

[0051] PFPE-PETA-APS-3000 (1.5 g, 0.000436 mol) was added to a 100 ml three-neck flask equipped with a magnetic stirring rotor, a nitrogen inlet and a reflux condenser under nitrogen protection. Gamma-(methacryloyloxy)propyltrimethoxysilane (0.1083 g, 0.000436 mol) was added dropwise to the flask over 20 min. Stir at room temperature for 30 min, then at 50 °C for 10 h. The peak associated with the secondary amine group was confirmed in FTIR analysis (~1546cm -1 ) to stop the reaction. After washing and reducing pressure, a yellow viscous oil (PFPE-PETA-APS-S3000) was obtained.

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Abstract

The invention belongs to a catalyst-free method for preparing polysiloxane perfluoropolyether. A synthetic method obtaining the polysiloxane perfluoropolyether by a reaction of perfluoropolyether carboxylic acid, a hydroxyl-containing acrylate compound and amino siloxane is characterized by comprising the following steps: (1) preparing the perfluoropolyether acrylate ester; (2) performing Michael addition reaction of the perfluoropolyether acrylate ester and siloxane and finally obtaining the polysiloxane perfluoropolyether. When the polysiloxane perfluoropolyether is prepared, the amino siloxane and alpha and beta unsaturated acrylate siloxane are added, a content ratio of silicon oxygen in polyether is improved, a content ratio of a silicon oxygen bond is higher, the silicon oxygen bond bonds with a hydroxyl at the surface of glass to form a Si-O-Si network structure is more, and the adhesive force of a film is higher.

Description

technical field [0001] The invention belongs to the field of chemical materials and substrate surface treatment, and relates to the preparation of polysiloxane-modified perfluoropolyether by a catalyst-free method, which can make the surface of hard substrates (glass, ceramics, metal and plastics) waterproof and oil-proof and antifouling properties. Background technique [0002] At present, touch-screen electronic equipment, ceramics, plexiglass and mirror material polycarbonate are more and more widely used in our lives. Touching and swiping with fingers for a long time during use will inevitably expose these substrates to water stains, Therefore, the requirements for the waterproof, anti-fouling and wear-resistant performance of these hard substrates are getting higher and higher. Therefore, there is an urgent need for a coating agent that can be coated on the surface of these substrates and has good waterproof, oil-proof, stain-proof and wear-resistant properties to solv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C08G65/332C08G65/336
CPCC08G65/3322C08G65/336C08G65/48
Inventor 唐旭东冯裕智毛占伟
Owner TIANJIN RIJIN TECH
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