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Inorganic/organic fluorine-containing microspheres with strawberry structure and its preparation method and application

A strawberry-shaped, microsphere technology, applied in the direction of coating, can solve the problems of harsh process, complex process, difficult industrial production and application, etc., and achieve the effect of improving durability

Active Publication Date: 2016-03-16
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method also has the problem of insufficient bonding strength or easy damage to the surface
Patent CN1379128A proposes a chemical vapor deposition method to prepare an array structure film with super-amphiphobic properties, but the process is relatively harsh and it is not easy for industrial production and application
[0007] Patent 201110266897.9 proposes a method of blending fluorine-containing silicon-containing copolymers and silicon dioxide to form a film on the surface containing active groups, which can endow the surface with good super-amphiphobic properties. This method is widely used Fluorine-containing silicon-containing copolymers, and blending and assembly reactions are required when used, and the process is relatively complicated
[0008] In recent years, there have been many literatures and patents on the use of fluoropolymers to construct superhydrophobic and superoleophobic interfaces. However, most of the fluoropolymers reported in the literature currently have weak adhesion between the surface of the substrate, which leads to the construction of superhydrophobic and superoleophobic interfaces. The superhydrophobic / superoleophobic interface has the disadvantages of being weak, friction-resistant, and washing-resistant, and it is not effective for constructing a superamphiphobic surface with a smooth surface such as glass as a substrate.
In addition, the fluoropolymers used to construct superhydrophobic and superoleophobic are mainly oil-soluble. This oil-soluble fluoropolymer requires a large amount of organic solvents. On the one hand, organic solvents will pollute the environment and are expensive. It will also endanger the health of construction workers

Method used

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  • Inorganic/organic fluorine-containing microspheres with strawberry structure and its preparation method and application
  • Inorganic/organic fluorine-containing microspheres with strawberry structure and its preparation method and application
  • Inorganic/organic fluorine-containing microspheres with strawberry structure and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0063] (1) Preparation of silica microspheres: A typical example is to add 50ml of absolute ethanol and 2mL of ammonia water to a 100mL round bottom flask, then add 3mL of tetraethyl orthosilicate dropwise, and react at 35°C for 24h. The product was centrifuged and washed three times with absolute ethanol, and the obtained silica microspheres were lyophilized and vacuum-dried. The final particle size of the obtained silica microspheres was 80±5nm. In addition, by adjusting the feeding ratio of ammonia water and tetraethyl orthosilicate, the obtained 250±5nm and 350±5nm silicon dioxide are used in Example 2 and Example 3 respectively.

[0064] (2) Preparation of inorganic microspheres modified by coupling agent containing amino groups: In anhydrous toluene, add inorganic microspheres, ultrasonically disperse for 30 minutes (ultrasonic power is 300W, temperature is 35°C), then add silane coupling agent, Reflux at 110°C for 12 hours, wash the product with acetone and toluene seve...

Embodiment 2

[0079] Step 1 and step 2 are the same as embodiment 1;

[0080] (3) Synthesis of composite microspheres with strawberry structure: disperse the modified silica microspheres prepared in step (2) in water, ultrasonicate for 30 minutes (ultrasonic power is 300W, temperature is 35°C), and then add trigger Pre-emulsify agent C and macromer D by stirring at room temperature for 14 hours, and deoxidize with nitrogen for 30 minutes, then raise the temperature to 70°C, then slowly add epoxy group-containing double bond monomer A, continue to react for 5 hours, and then slowly add Hydrophilic monomer B, continue to react for 6 hours, cool to room temperature after the reaction, the product is washed with water and THF, centrifuged and redispersed twice, and dried at 40°C for 24 hours in a vacuum. The product is a white powder, which is a composite of strawberry structure. Microspheres.

[0081] where H 2 O, initiator C, macromonomer D, the mass ratio of double bond monomer A containin...

Embodiment 3

[0094] Step 1 and step 2 are the same as embodiment 1;

[0095] (3) Synthesis of composite microspheres with strawberry structure: disperse the modified silica microspheres prepared in step (2) in water, ultrasonicate for 30 minutes (ultrasonic power is 300W, temperature is 35°C), and then add trigger Pre-emulsify agent C and macromer D by stirring at room temperature for 24 hours, and deoxidize with nitrogen for 30 minutes, then raise the temperature to 90°C, then slowly add epoxy group-containing double bond monomer A, continue to react for 2 hours, and then slowly add Hydrophilic monomer B, continue to react for 3 hours, cool to room temperature after the reaction, the product is washed with water and THF, centrifuged and redispersed twice, and dried in vacuum at 40°C for 24 hours. The product is a white powder, which is a composite of strawberry structure. Microspheres.

[0096] where H 2 O, initiator C, macromonomer D, the mass ratio of double bond monomer A containing ...

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Abstract

The invention belongs to the field of a super-amphiphobic material and discloses inorganic / organic fluorine-containing microspheres with strawberry-shaped structures as well as a preparation method and application thereof. According to the invention, firstly, inorganic microspheres are modified by an amino-containing silane coupling agent to prepare inorganic microspheres of which the surfaces comprise amino; then the modified inorganic microspheres are prepared into composite microspheres with the strawberry-shaped structures through emulsion polymerization; finally, the composite microspheres with the strawberry-shaped structures and a fluorine-containing compound F are prepared into the inorganic / organic fluorine-containing microspheres with the strawberry-shaped structures under the action of a catalyst E. The fluorine-containing microspheres prepared by the invention have double coarse structures; the surfaces of the microspheres comprise an epoxy group and also comprise fluorine-containing chain segments, so that two necessary conditions of constructing the super-amphiphobic structure are met and the super-hydrophobic / oleophobic performance of the surfaces of most of base materials can be directly implemented; besides, the fluorine-containing microspheres have good hydrophilicity and can avoid using an organic solvent harmful for the environment; moreover, the obtained super-amphiphobic surface has good washing resistance and corrosion resistance.

Description

technical field [0001] The invention belongs to the field of super amphiphobic materials, and in particular relates to an inorganic / organic fluorine-containing microsphere with a strawberry structure and a preparation method and application thereof. Background technique [0002] The most important characterization 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. A surface can be considered a superoleophobic surface if it has a contact angle of greater than 150° for oil. If the surface has both superhydrophobic and superoleophobic properties, it is called a superamphiphobic surface. [0003] Due to its unique hydrophobic and oleophobic properties, superhydrophobic surfaces can be applied in many aspects. The superamphiphobic surface has a self-cleaning function...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/32C08F220/28C08F8/34C08F8/18C08F8/32C08K9/06C08K3/36C08K3/22C09D151/08C09D7/12
Inventor 胡继文李妃邹海良林树东吴艳杨洋刘国军
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI