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Hydrophobic POSS (Polyhedral Oligomeric Silsesquioxane)-based hybridization fluorinated acrylate resin as well as preparation method and application thereof

A fluorine-containing acrylate, hydrophobic technology, applied in the direction of polyurea/polyurethane coatings, coatings, etc., can solve the problems of insufficient hydrophobic effect, complex preparation process, cumbersome process, etc., and achieves favorable adhesion, simplified preparation process, Simple effect of raw materials

Inactive Publication Date: 2013-12-11
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the atom transfer radical polymerization method used in this invention is cumbersome, and the fluorine-containing POSS preparation process is relatively complicated, and the maximum static water contact angle achieved at the same time is only 120°
The Chinese invention patent applications with publication numbers CN103012700A and CN102775567A are all constructed by reversible addition-fragmentation chain transfer radical polymerization (RAFT) with low surface energy, the preparation process is relatively complicated, and the hydrophobic effect is not significant enough

Method used

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  • Hydrophobic POSS (Polyhedral Oligomeric Silsesquioxane)-based hybridization fluorinated acrylate resin as well as preparation method and application thereof
  • Hydrophobic POSS (Polyhedral Oligomeric Silsesquioxane)-based hybridization fluorinated acrylate resin as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In the first step, when equipped with an electric mixer, N 2 Add 11g of butyl acetate as a solvent to the four-necked flask with air duct, condensing reflux tube and constant pressure funnel, heat up to 85°C and reflux for 30min, and feed N2, then add 1.9g of methyl methacrylate, 2.8g of butyl acrylate , 1.9g of methacrylic acid-β-hydroxyethyl ester, 0.14g of azobisisobutyronitrile and 4g of butyl acetate were mixed evenly and then added to the constant pressure funnel, stirred at a speed of 350 rpm, and dripped continuously within 2.5h. After the dropwise addition, continue the insulation reaction for 3.5h;

[0038] In the second step, 1.4g of 2-(perfluorooctyl)ethyl methacrylate, 0.03g of azobisisobutyronitrile and 2g of solvent are mixed evenly and then added to the constant pressure funnel, and added dropwise to the reaction of the first step at a constant speed In the system, drop continuously within 0.5h, and continue to keep warm for 2h after the dropwise additi...

Embodiment 2

[0042] In the first step, add 10 g of xylene as a solvent in a four-neck flask equipped with an electric mixer, N2 gas guide tube, condensing reflux tube, and constant pressure funnel, raise the temperature to 80 ° C and reflux for 30 min, and feed N2, then 1.2 g of formazan Isopropyl acrylate, 1.7g butyl acrylate, 2.1g hydroxypropyl methacrylate, 0.1g azobisisobutyronitrile and 2g solvent were mixed evenly and then added to the constant pressure funnel, stirred at a speed of 350 rpm, 2.5 Continuously drip within h, and continue the insulation reaction for 3 hours after the dropwise addition;

[0043] In the second step, add 0.9g of dodecafluoroheptyl methacrylate, 0.02g of azobisisobutyronitrile and 2g of solvent into the constant pressure funnel, drop them into the reaction system of the first step at a constant speed, and drop them continuously within 2h After finishing the dropwise addition, continue the insulation reaction for 3h;

[0044] In the third step, take 4.1g PO...

Embodiment 3

[0047] In the first step, 11 g of xylene was added as a solvent in a four-neck flask equipped with an electric mixer, N2 gas guide tube, condensing reflux tube, and constant pressure funnel, and the temperature was raised to 90 ° C for 45 minutes to reflux, and N2 was introduced, and then 2.4 g of formazan tert-butyl acrylate, 3.6g isooctyl acrylate, 2.4g hydroxybutyl methacrylate, 0.18g benzoyl peroxide and 4g solvent are mixed evenly and then added to the constant pressure funnel, stirred at a speed of 350 rpm, 1.5 Continuously drip within h, and continue the insulation reaction for 2 hours after the dropwise addition;

[0048] In the second step, mix 1.3g of tridefluorooctyl methacrylate, 0.03g of benzoyl peroxide and 2g of solvent evenly, then add them to the constant pressure funnel, and drop them into the reaction system of the first step at a uniform speed, and continue within 1h After dropping, continue the insulation reaction for 1h after the dropwise addition;

[00...

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Abstract

The invention discloses a hydrophobicPOSS (Polyhedral Oligomeric Silsesquioxane)-based hybridization fluorinated acrylate resin as well as a preparation method and an application thereof. The formula of the hydrophobic POSS-based hybridization fluorinated acrylate resin comprises the following raw materials in percentage by weight: 2-12% of POSS-based monomer, 2-11% of hard monomer, 3-16% of soft monomer, 1.5-7% of fluoroacrylate monomer, 3-11% of crosslinking monomer, 0.4-1.3% of triggering agent and 50-79% of solvent. The application of the hydrophobic POSS-based hybridization fluorinated acrylate resin is characterized in that a crosslinking-type copolymer is mixed with a curing agent, the hydrophobic POSS-based hybridization fluorinated acrylate resin aggregates and is self-assembled in a film-forming solvent so as to form a micellar solution, then a phase isolation technology is used for ensuring that the solvent volatilizes on filter paper or a metal screen to form a film so as to construct a composite multi-scale structure, so that a super-hydrophobic coating is prepared. The preparation method has the advantages that a free radical solution polymerization method is adopted, synthetic conditions are simple, reaction routes are simple, raw materials are simple and easy to get, and the preparation technological processes of organic / inorganic hybrid materials are greatly simplified; the hydrophobic POSS-based hybridization fluorinated acrylate resin has wide application prospect in the field of waterproof and dampproof coating and the like.

Description

technical field [0001] The invention relates to a fluorine-containing acrylate resin, in particular to a hydrophobic POSS-based hybrid fluorine-containing acrylate resin and its preparation method and application; it belongs to the preparation technology of organic / inorganic hybrid materials. The resin is a fluorine-containing acrylate superhydrophobic material containing a polyhedral oligomeric silsesquioxane structure prepared by free radical solution polymerization. Background technique [0002] Polyhedral Oligomeric Silsesquioxane (Polyhedral Oligomeric Silsesquioxane, referred to as POSS) is a new type of nanomaterial that has emerged in recent years. Its molecular formula can be expressed as (RSiO 1.5 ) n (n can generally be 6, 8, 10, etc.), which is an organic / inorganic hybrid composed of a rigid, structurally determined nanoscale inorganic core composed of silicon and oxygen and an organic group R connected by a covalent bond. molecular. It can be combined with t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/18C08F220/14C08F220/28C08F220/24C08F220/22C08F8/42C09D175/04
Inventor 皮丕辉廖达刘超文秀芳蔡智奇徐守萍程江
Owner SOUTH CHINA UNIV OF TECH
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