Fluorine-containing nanoparticles with high dispersibility and bonding property and superamphiphobic surface

A nano-microsphere, high-dispersion technology, applied in the direction of coating, etc., can solve the problems of expensive, toxic, unfavorable construction and environmental protection of fluorine-containing solvents, and achieve excellent hydrophobicity and oil repellency, and broad application prospects

Active Publication Date: 2012-07-18
中科瑞丽分离科技无锡有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the fluorine-containing nano-microspheres in this patent need to be dispersed in a fluorine-containing solvent, and there are no adhesive groups on the surface, so the adhesion is not very strong
[0013] In short, although the articles and patents published in the world have mentioned that the performance of super-amphiphobic materials is very good, there is no real large-scale industrialized product in related fields, mainly because some basic problems have not been solved: (1) fluorine-containing nano-micro Dispersion of spheres: Due to the low surface energy of fluoropolymers, it is difficult to dissolve in most non-fluorinated solvents, so it is necessary to use fluorinated solvents to realize the dispersion of fluorinated nanospheres
However, fluorine-containing solvents are not only expensive, but also toxic, which is not conducive to construction and environmental protection.
(2) Adhesion problem of fluorine-containing nano-microspheres: the surface of the super-amphiphobic nano-microspheres prepared in the current reported patents and literatures are all fluorine-containing polymers, and there is no adhesive functional group, so the prepared super-amphiphobic nano-microspheres Amphiphobic nanospheres have the disadvantage of poor adhesion

Method used

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  • Fluorine-containing nanoparticles with high dispersibility and bonding property and superamphiphobic surface
  • Fluorine-containing nanoparticles with high dispersibility and bonding property and superamphiphobic surface
  • Fluorine-containing nanoparticles with high dispersibility and bonding property and superamphiphobic surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] The end group is the preparation method of the fluoropolymer of compound D, comprises the following steps:

[0072] (1) Synthesis of Hydroxyl ATRP Initiator (HEBI)

[0073] Add 4ml of triethylamine to 25g of ethylene glycol (furfuryl alcohol), place it in an ice-water bath, slowly drop in 2.5ml of 2-bromoisobutyryl bromide, naturally warm up to room temperature and react for 4h, and then use saturated sodium bicarbonate solution to It was washed 3 times, then washed to neutrality with pure water, then dried with anhydrous magnesium sulfate, removed dichloromethane to obtain a viscous liquid substance, and then distilled under reduced pressure to obtain the ATRP initiator (HEBI) with hydroxyl ,

[0074] Nuclear magnetic spectrum analysis is: 1H NMR (CDCl 3 , δ, ppm): 4.35(q, 1H, J=6.89Hz), 4.19(t, 2H, J=4.75Hz), 3.75(t, 2H, J=4.75Hz), 3.00(s, 1H, OH) , 1.75 (d, 3H, J=6.96Hz).13C NMR (CDCl 3 , δ): 170.53, 67.18, 60.35, 39.93, 21.50. Therefore, it can be deduced that i...

Embodiment 2

[0085] The end group is the preparation method of the fluoropolymer of compound D, comprises the following steps:

[0086] (1) Synthesis of maleimido methacrylate

[0087] Dissolve 1.25g of ρ-CPMIC in 50ml of anhydrous dichloromethane, add 2.1ml of triethylamine, and slowly drop into 1.21ml of ATRP initiator hydroxyethyl methacrylate with hydroxyl groups under ice-water bath conditions. Naturally warm up to room temperature and react for 10 h, then wash it with saturated sodium bicarbonate solution 3 times, then wash with pure water until neutral, then dry with anhydrous magnesium sulfate, remove dichloromethane, and obtain viscous liquid material, and then distilled under reduced pressure to obtain an acrylic monomer with a maleic anhydride functional group, that is, maleamidomethacrylate (ρ-CPMIC-HEMA).

[0088] The spectral analysis of the product is as follows: 1H-MR (CDCl3 as solvent): 6.94 (hydrogen on maleimide, 2H), 7.85, 7.95 (hydrogen on phenyl, 4H), 1.93 (CH3, 3H);...

Embodiment 3

[0095] End group is the preparation method of the epoxy resin type polymer of compound A, comprises the following steps:

[0096] (1) Synthesis of furan ring initiator (furyl bromoisobutyrate)

[0097] Disperse 1.5g of furyl alcohol (furfuryl alcohol) in 30ml of anhydrous dichloromethane, add 4ml of triethylamine, slowly drop in 2ml of 2-bromoisobutyryl bromide under ice-water bath conditions, naturally warm up to room temperature and react for 4h, then Then wash it 3 times with saturated sodium bicarbonate solution, then wash it with pure water to neutrality, then dry it with anhydrous magnesium sulfate, remove dichloromethane, obtain a viscous liquid substance, and then distill under reduced pressure to obtain the furan ring Initiator.

[0098] The spectral analysis of the product is as follows: 1 H-NMR (CDCl 3 solvent): 7.30, 6.25, 6.19 (hydrogen on the furan ring, 3H), 5.19 (hydrogen on the methylene on furfuryl alcohol, 2H), 2.02 (hydrogen on the dibromoisobutyryl brom...

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Abstract

The invention discloses fluorine-containing nanoparticles with high dispersibility and bonding property and a superamphiphobic surface prepared from the nanoparticles. The fluorine-containing nanoparticles with high dispersibility and bonding property are prepared by the steps of grafting a fluorine-containing polymer with an upper terminal group to be a compound D on the surfaces of the nanoparticles, and reacting an epoxy resin polymer with a terminal group to be a compound A with the fluorine-containing polymer through a heat-breaking Diels-Alder reaction. The superamphiphobic surface disclosed by the invention is prepared by the steps of dispersing the fluorine-containing nanoparticles with high dispersibility and bonding property in a low-boiling-point fluorine-free solvent, uniformly mixing with an epoxy resin curing agent, carrying out spray coating on the surface of a substrate material, and carrying out vacuum drying. According to the fluorine-containing nanoparticles disclosed by the invention, the epoxy resin polymer with high dispersibility is introduced, as the epoxy functional group contained in the dispersing polymer can take place a curing reaction with the epoxy group by using the epoxy resin curing agent in the solvent to fix the fluorine-containing nanoparticles on the surfaces of most substrates, the bonding problem of the fluorine-containing nanoparticles on the substrate surface is solved.

Description

technical field [0001] The invention belongs to the field of macromolecular superamphiphobic materials, and in particular relates to a fluorine-containing nano-microsphere with high dispersibility and cohesiveness, a preparation method thereof, and a super-amphiphobic surface prepared from the fluorine-containing nano-microsphere. Background technique [0002] Superhydrophobic surfaces refer to those solid surfaces with surface static contact angles greater than 150°. This special hydrophobic state (property) is called superhydrophobic state (property). If the static contact angles of water and oil on a surface are both greater than 150° and the rolling angles are both less than 5°, the interface can be called a superamphiphobic interface. [0003] Superamphiphobic materials can be widely used in all aspects of production and life such as building materials, electricity, military, textiles, leather, packaging materials, kitchen and bathroom utensils, oil pipelines, and meta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02C09D187/00C09D7/12C09D5/00
Inventor 胡继文邹海良张干伟候成敏何谷平李银辉涂园园刘国军胡攸卢汝烽李伟刘锋
Owner 中科瑞丽分离科技无锡有限公司
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