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Fluorinated polyether siloxane and preparation method of same

A technology of fluorinated polyether siloxane and fluorinated polyether, which is applied in the field of fluorinated polyether siloxane and its preparation, can solve the problem that the compound coating does not show sufficient oil repellency and lubricity, and affects the substrate adhesion. Bond strength, unfavorable industrial production and other issues, to achieve full cross-linking and curing, easy control of the preparation process, and good antifouling effect

Inactive Publication Date: 2017-12-22
QUZHOU FLUORIDE & SILICON RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 3M Company has published many patents on the synthesis and application of fluorinated polyether siloxane (such as CN1998813320.2, CN200480025773.X, CN200780030231.5, etc.), but the polyfluoropolyether group of the above-mentioned fluorinated polyether siloxane The molecular weight is low and the molecular chain is short, so that the compound coating does not show sufficient oil repellency and lubricity
However, in order to obtain compounds with polysiloxane groups, the synthesis process of the fluorine-containing alkylene polymers with terminal hydrolyzable groups needs to use polysilicone hydrogen bond compounds, and the reaction is difficult to control due to the large number of active groups. , easy to produce by-products; secondly, the siloxane groups are all bonded to the polysilicon hydrogen bond groups, due to steric barriers, it is difficult for these hydrolyzable groups to fully hydrolyze and cross-link, which affects the adhesion to the substrate. In addition, the polysilicon-hydrogen bonded compounds described in the patent are mostly unused substances, the raw materials are not easy to obtain, and the cost is high, which is not conducive to industrial production

Method used

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  • Fluorinated polyether siloxane and preparation method of same

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preparation example Construction

[0033] The preparation method of fluorinated polyether siloxane includes the following steps:

[0034] (1): The polyfluoropolyether methyl monoformate is reacted with a multifunctional amino compound to prepare the amidation product of the polyfluoropolyether. A polyfunctional amino compound is an organic compound containing 1 to 2 primary amino groups and 2 hydroxyl groups in one molecule or an organic compound containing 1 to 2 primary amino groups and 2 secondary amino groups in one molecule, and among them, 2- Amino-1,3-propanediol, 2-amino-2-methyl-1,3-propanediol and trivinyltetraamine, etc. When the reactant is a monoprimary amine compound, the molar amount can be 1 to 1.2 times the polyfluoropolyether monoformate to complete the reaction of the polyfluoropolyether monoester; when the reactant is a diprimary amine compound, The molar amount of ether methyl ester is preferably controlled at 1:2. The reaction is preferably carried out under the protection of nitrogen, and ...

Embodiment 1

[0043] Example 1 (Synthesis of fluorinated polyether siloxane compound a-a-1)

[0044] Step (1): 103.16g (about 0.02mol) of polyfluoropolyether methyl monocarboxylate F (CF (CF 3 )CF 2 O)nCF(CF 3 )COOCH 3 , N=30 and 2.18g (about 0.024mol) of 2-amino-1,3-propanediol were added into the reaction flask, and under the protection of nitrogen, the temperature was raised to 75°C, and the reaction was stirred for 20h. FTIR analysis confirmed the ester group absorption peak (about 1790cm -1 ) Disappeared, and the amide group absorption peak (about 1710cm -1 ). The product was dissolved in 100 g of ethyl tert-butyl ether, and 10 ml of 1 mol / L HCl aqueous solution was added, stirred for 10 minutes, and then stood at room temperature for liquid separation, and the water phase was removed. After washing the organic phase with deionized water to neutrality, and then drying with magnesium sulfate, and then steaming the solvent with a rotary evaporator, the product F(CF(CF 3 )CF 2 O)nCF(CF 3 )CO...

Embodiment 2

[0047] Example 2 (Synthesis of fluorinated polyether siloxane compound a-a-2)

[0048] Step (1): In addition to polyfluoropolyether methyl monoformate, use 50.04g (about 0.02mol) of F(CF(CF 3 )CF 2 O)nCF(CF 3 )COOCH 3 , N=14 instead, 2-amino-1,3-propanediol was replaced with 2.52g (about 0.024mol) of 2-amino-2-methyl-1,3-propanediol, and the rest was the same as the step (1 ) Is the same, the resulting product F(CF(CF 3 )CF 2 O)nCF(CF 3 )CONHC(CH 2 OH) 2 CH 3 , N=14.

[0049] Step (2): Except that the polyfluoropolyether glycol is replaced by 38.63g (about 0.015mol) of the product obtained in the previous step, the rest is the same as the step (2) of Example 1, to obtain the product F(CF(CF) 3 )CF 2 O)nCF(CF 3 )CONHC(CH 2 OCONHCH 2 CH 2 OOCCH=CH 2 ) 2 CH 3 , N=14.

[0050] Step (3): Except that the double bond-containing polyfluoropolyether is replaced with 28.57g (about 0.01mol) of the product obtained in the previous step, the rest is the same as the step (3) of Example 1, to obtai...

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Abstract

The invention discloses a fluorinated polyether siloxane and a preparation method of same. The fluorinated polyether siloxane is represented as the formula (a1): PFPE-CONHCR1(CH2OCONHCH2CH2OCOCHR2CH2N(CH2CH2CH2Si(OR)3)2)2, or the formula (a2): {[PFPE-CONHCH2CH2]N[CONHCH2CH2OCOCHR2'CH2N(CH2CH2CH2Si(OR')3)2]CH2}2, wherein R1, R2 and R2' are respectively and independently H or CH3; and R and R' are respectively and independently C1-C4 alkyl groups; the PFPE- is a monovalent polyfluoropolyether group. The fluorinated polyether siloxane has high adhesion force on a base material and is good in scratch resistance. The preparation method employs easy-to-obtained raw materials and is easy to control.

Description

Technical field [0001] The invention relates to a fluorinated polyether siloxane and a preparation method thereof. Background technique [0002] The transparent optical devices of touch electronic display devices (such as mobile phone glass screens, etc.) are often in contact with fingers and are easily contaminated by fingerprints, sweat, oil stains, etc., and once the dirt is formed, it is difficult to remove without the use of solvents. There is a risk of damaging the display device; on the other hand, dirt also affects the visual perception of the display device. In order to prevent contamination of the display device by dirt and possible damage to the device in the process of removing the dirt, it is of great significance to develop a surface coating with anti-fouling and easy-to-decontamination functions. [0003] In order to achieve the above objectives, researchers have developed a variety of fluorinated siloxane antifouling products. The hydrolysis and condensation of si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/336C08G65/333
Inventor 李建裴金东郦聪
Owner QUZHOU FLUORIDE & SILICON RES INST
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