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High-dispersion fluorine-containing nanosphere and epoxy resin super-amphiphobic surface

A nano-microsphere, epoxy resin technology, applied in epoxy resin coatings, dyed polymer organic compound treatment, fibrous fillers, etc., can solve the problems of inability to disperse, weak adhesion, etc. The effect of weak adhesion and excellent hydrophobicity and oleophobicity

Inactive Publication Date: 2012-07-25
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

[0020] In order to overcome the shortcomings and deficiencies of existing superamphiphobic materials containing fluorine-containing solvents, poor adhesion, and inability to disperse in epoxy resin coatings, the primary purpose of the present invention is to provide a highly dispersed fluorine-containing nano-microsphere, The highly dispersed fluorine-containing nanospheres are grafted on the surface of ordinary fluorine-containing nanospheres with a high-dispersibility polymer that can be dispersed in epoxy resin, so that the fluorine-containing nanospheres can be processed without fluorine-containing solvents. To achieve its dispersion in epoxy resin

Method used

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  • High-dispersion fluorine-containing nanosphere and epoxy resin super-amphiphobic surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] The end group is the preparation method of the fluoropolymer of compound D, comprises the following steps:

[0082] (1) Synthesis of furan ring initiator (furyl bromoisobutyrate)

[0083] 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.

[0084] 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 bromide, 6H...

Embodiment 2

[0093] The end group is the preparation method of the fluoropolymer of compound D, comprises the following steps:

[0094] (1) Synthesis of furfuryl methacrylate

[0095] Disperse 1.23g of furyl alcohol (furfuryl alcohol) in 20ml of anhydrous tetrahydrofuran, add 2ml of triethylamine, slowly drop in 2.5ml of methacryloyl chloride under ice-water bath conditions, naturally warm up to room temperature and react for 24h, and then use saturated carbonic acid Wash it three times with sodium hydrogen solution, then wash it with pure water until neutral, then dry it with anhydrous magnesium sulfate, remove tetrahydrofuran, obtain a viscous liquid substance, and then distill under reduced pressure to obtain furfuryl methacrylate.

[0096] The spectral analysis of the product is as follows: 1 H-NMR (CDCl3 as solvent): 7.30, 6.25, 6.19 (hydrogen on the furan ring, 3H), 5.19 (hydrogen on the methylene on furfuryl alcohol, 2H), 1.78 (CH 3 , 3H); Infer that the product structure of the p...

Embodiment 3

[0103] Adopt anionic polymer hair synthesis end group to be the highly dispersed polymer of compound A, comprise the following steps:

[0104] (1) Synthesis of ρ-CPMIC initiator

[0105] Add 30mL of dimethylformamide to a 500mL three-necked flask equipped with stirring, and simultaneously add a DMF solution of p-aminobenzoic acid solution (14g, 0.1mol) and maleic anhydride (11g, 0.11mol) dropwise. React at ~20°C for 2 hours to obtain yellow needle-like crystals. After filtration and drying, the intermediate product ρ-CPMA is obtained, with a melting point of 208-210°C;

[0106] Add ρ-CPMA (20g, 0.85mol), anhydrous sodium acetate (2g, 0.016mol), and acetic anhydride (48mL, 0.5mol) into a 250mL three-neck flask in sequence, keep it warm at 60-80°C for 1h, and cool down to room temperature , poured into 800mL ice water, precipitated, suction filtered, washed with water until neutral, recrystallized with 95% ethanol by volume fraction, and vacuum dried at 60°C to obtain ρ-CPMIC, ...

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Abstract

The invention discloses a high-dispersion fluorine-containing nanosphere and an epoxy resin super-amphiphobic surface. The high-dispersion fluorine-containing nanosphere is obtained by grafting a fluorine-containing polymer with an end group of a compound D on the surface of the nanosphere and connecting a high-dispersion polymer with an end group of a compound A with the fluorine-containing polymer through a Diels-Alder reaction. The super-amphiphobic surface is prepared by the following steps that: the high-dispersion fluorine-containing nanosphere is dispersed in a low-boiling solvent, and then a liquid epoxy resin and an epoxy resin curing agent are added to obtain an epoxy resin coating with a super-amphiphobic effect; and then the epoxy resin coating is sprayed on a base material, and then is dried to obtain the super-amphiphobic surface. The poxy resin super-amphiphobic surface provided by the invention has excellent hydrophobic and oleophobic properties, the hydrophobic and oleophobic contact angle is greater than 150 degrees, and the rolling angle is less than 5 degrees. In the process of preparing the super-amphiphobic surface, a toxic fluorine-containing solvent is avoided being used, and the super-amphiphobic surface can be built on the surfaces of most materials by utilizing the excellent adhesive property of the epoxy resin coating.

Description

technical field [0001] The invention belongs to the field of macromolecule superamphiphobic materials, in particular to a fluorine-containing nano-microsphere grafted with a high-dispersibility polymer on the surface and a preparation method thereof, and a self-cleaning nano-microsphere prepared from the fluorine-containing nano-microsphere Functional epoxy superamphiphobic surfaces. Background technique [0002] Nanomaterials and micro-nano composite materials, especially micro-nano composite materials with special wettability, are important directions in the scientific research and practical application of nanomaterials. Superamphiphobic (hydrophobic and oleophobic) materials, as a kind of nanomaterials with special wettability, are a research hotspot today. Wherein, the superhydrophobic surface refers to those solid surfaces whose surface static contact angle is greater than 150°, and this special state (property) of the solid surface is called the superhydrophobic state...

Claims

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Application Information

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IPC IPC(8): C09D7/12C09D163/00C09C3/10C09C1/28C09C1/40C09C1/36C09C1/02C09C1/24C08J7/12
Inventor 胡继文邹海良候成敏张干伟何谷平李银辉涂园园刘国军胡攸卢汝烽李伟刘锋
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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