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Surface fluorine-containing nanosphere capable of crosslinking as well as preparation method and application thereof

A nano-microsphere and microsphere technology, applied in coating, silicon oxide, silicon dioxide and other directions, can solve the problems of complex process, harsh assembly conditions, etc., and achieve simple preparation method, good super-amphiphobic performance, and adjustable structure. The effect of sexual convenience

Inactive Publication Date: 2012-05-02
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires the preparation of block copolymers with complex processes and harsh assembly conditions
[0008] The Chinese patent application with the application number 201110266897.9 and titled "A Superamphiphobic Polymer and a Superamphiphobic Surface Constructed by It" provides a method of blending a fluorine-containing silicon-containing copolymer with silicon dioxide. Assembling a film on the surface containing active groups can endow the surface with good superamphiphobic properties. This method uses more fluorine-containing silicon-containing copolymers, and requires blending and assembly reactions when used, and the process is relatively complicated.

Method used

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  • Surface fluorine-containing nanosphere capable of crosslinking as well as preparation method and application thereof
  • Surface fluorine-containing nanosphere capable of crosslinking as well as preparation method and application thereof
  • Surface fluorine-containing nanosphere capable of crosslinking as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Preparation of silica microspheres: Add 100ml of absolute ethanol, 4ml of deionized water and 3ml of ammonia water in a 100ml round bottom flask, then add 4ml of tetraethyl orthosilicate dropwise, and react at 25°C for 24h. The product was centrifuged and washed three times with absolute ethanol, and the obtained silica microspheres were lyophilized and vacuum-dried, and the finally obtained silica microspheres had a particle diameter of 91±4nm.

[0062] (2) Preparation of cross-linkable surface fluorine-containing nano-microspheres: disperse 2 g of the silicon dioxide prepared in step (1) in 60 ml of anhydrous toluene, add 5 ml of aminopropyltriethoxysilane, and fill with nitrogen at 105 Reflux at ℃ for 48 hours, then wash with anhydrous toluene and anhydrous acetone in sequence, and dry in vacuum to obtain aminated silicon dioxide.

[0063] Disperse 1.5 g of aminated silicon dioxide in 30 ml of anhydrous toluene, add 4 ml of triethylamine, and slowly drop in 2 ml ...

Embodiment 2

[0070] (1) Preparation of silica microspheres: Add 50ml of absolute ethanol, 3ml of deionized water and 3ml of ammonia water in a 100ml round bottom flask, then add 2ml of tetraethyl orthosilicate dropwise, and react at 25°C for 24h, The product is centrifuged and washed three times with absolute ethanol, and the obtained silica microspheres are subjected to freeze-vacuum drying, and the finally obtained silica microspheres have a particle diameter of 350±10 nm.

[0071] (2) Preparation of cross-linkable surface fluorine-containing nano-microspheres: disperse 2.5 g of silica microspheres prepared in step (1) in 70 ml of anhydrous toluene, add 8 ml of methacryloxypropyl trimethoxy Silane, after filling with nitrogen, reflux at 105°C for 48 hours, then wash with anhydrous toluene and anhydrous acetone in sequence, and vacuum-dry to obtain vinyl-rich silicon dioxide on the surface.

[0072] In a 250ml round bottom flask, add 5g of the surface vinyl-rich silicon dioxide prepared a...

Embodiment 3

[0078] (1) Preparation of polymer nanospheres containing hydroxyl groups on the surface: under stirring, gradually add 130 ml of distilled water, 4.80 g (48.0 mmol) of methyl methacrylate and 0.4 g (2.0 mg mol) of ethylene glycol dimethacrylate, and 41 mg (0.15 micromol) of potassium peroxodisulfate in water (5 ml). Nitrogen was blown through the reaction system at 25°C for 15 minutes to remove oxygen in the system. Then heated to 90° C. in an oil bath, and reacted for 2 hours.

[0079] (2) Preparation of cross-linkable surface fluorine-containing nanospheres: take 43 ml of solution from the above system, add it to a 250 ml three-necked flask filled with nitrogen, and add 0.5 ml of 2.4 mg (14.6 micromoles) of Azadiisobutyronitrile tetrahydrofuran solution. After stirring for 15 minutes at 25°C, it was heated to 90°C. Then slowly add 2-chloropropionic acid ethylene glycol diester containing 0.4 gram (1.9 mmol) (prepared according to literature method: Bifunctional Core-Shell...

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Abstract

The invention provides a surface fluorine-containing nanosphere capable of crosslinking as well as a preparation method and application thereof. The surface fluorine-containing nanosphere capable of crosslinking has the structural formula I shown in the specification, wherein a structural unit A contains an alkoxysilane group or an acyloxy alkoxysilane group, and the alkoxysilane group can be bonded or crosslinked with a substrate after being hydrolyzed or enables nanospheres to crosslink; and a structural unit B contains a fluorine group and can be endowed with surface super hydrophobicity and oleophobicity. A material with a super hydrophobicity and oleophobicity surface is obtained through the steps: placing the surface fluorine-containing nanosphere capable of crosslinking into fluorine-containing solvent, adding tetrahydrofuran hydrochloric acid solution and water to mix, and then adding a preprocessed substrate material to react. The water contact angle of the super hydrophobicity and oleophobicity surface of the material is larger than 150 DEG, and the oil contact angle of the super hydrophobicity and oleophobicity surface of the material is larger than 150 DEG, thus, the material can be widely applied to all aspects of production and life, such as electricity, military, buildings, kitchen and toilet appliances and the like. (Formula I).

Description

technical field [0001] The invention belongs to the field of polymer superamphiphobic materials, in particular to a crosslinkable surface fluorine-containing nano-microsphere and its preparation method and application. The cross-linkable surface fluorine-containing nano-microsphere can be used to prepare a superamphiphobic surface . Background technique [0002] The most important characteristic parameter of surface wetting behavior is the contact angle. If the static contact angle of the surface to water is less than 10°, it is called a superhydrophilic surface; if the surface has a contact angle greater than 150°, it is called a superhydrophobic surface. If the surface has a contact angle greater than 150° for oil, it can be considered as a super-oleophobic surface; if the surface has both super-hydrophobic and super-oleophobic properties, it is called a super-amphiphobic surface. [0003] Due to its unique hydrophobic and oleophobic properties, superhydrophobic surfaces ...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F220/24C08F230/08C08F265/04C09D151/10C09D151/00C01B33/12
Inventor 张干伟邹海良李银辉刘国军涂园园何谷平胡盛逾
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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