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Cross-linked fluorine-containing (meth)acrylic acid block copolymer and its preparation and application

A block copolymer and cross-linking technology, which is applied in polyurea/polyurethane coatings, coatings, etc., can solve the problems of coating film performance and hydrophobicity can not be taken into account at the same time, to improve poor performance, waterproof and moisture-proof Extensive effect of improving coating film properties

Inactive Publication Date: 2014-10-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the relative molecular weight of the fluorine-containing block copolymers prepared by the ATRP method cannot exceed 100,000, and most of them are prepared from a single (meth)acrylate monomer and a fluorine-containing monomer. better at the same time

Method used

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  • Cross-linked fluorine-containing (meth)acrylic acid block copolymer and its preparation and application
  • Cross-linked fluorine-containing (meth)acrylic acid block copolymer and its preparation and application
  • Cross-linked fluorine-containing (meth)acrylic acid block copolymer and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The preparation of macromolecular initiator: the methyl methacrylate of 3g, the isopropyl acrylate of 6g, the hydroxyethyl acrylate of 1.5g and 6.5g dimethylbenzene join together in the reaction eggplant bottle and mix and dissolve, then seal the reaction bottle, Freeze the system with liquid nitrogen-vacuumize-thaw three times; under the protection of argon, add 0.048g ruthenium dichloride, 0.02g copper powder and 0.12g tris(2-pyridylmethyl)amine to seal the reaction bottle, and then freeze the system with liquid nitrogen-vacuumize-thaw-argon, repeat three times; finally put the reaction eggplant bottle in a 30°C oil bath, add 0.06g of carbon tetrachloride, and electromagnetically stir for 6 hours. Then add tetrahydrofuran to dilute, and then go through neutral alumina column chromatography. After most of the solvent evaporates, the prepared polymer is precipitated with petroleum ether and vacuum-dried to obtain a macromolecular initiator.

[0046] Preparation of cross...

Embodiment 2

[0050] Preparation of macroinitiator: 3.5g of isopropyl methacrylate, 6g of butyl acrylate, 1.5g of hydroxypropyl acrylate and 6g of dimethylformamide were added to the reaction eggplant bottle for mixing and dissolving, then sealed Reaction bottle, freeze the system with liquid nitrogen-vacuumize-thaw, repeat three times; under the protection of argon, then add 0.12g nickelous chloride, 0.01g nickel powder and 0.25g 3,5 Picolidinedicarboxylic acid, seal the reaction bottle, and then freeze the system with liquid nitrogen-vacuumize-thaw, repeat three times; finally put the reaction eggplant bottle in a 50°C oil bath, add 0.15g α-bromopropionitrile, electromagnetically stir for 10 hours, then add tetrahydrofuran to dilute, and then go through neutral alumina column chromatography. After most of the solvent volatilizes, the prepared polymer is precipitated with petroleum ether and vacuum-dried to obtain a macromolecular initiator.

[0051] Preparation of cross-linked fluorine-c...

Embodiment 3

[0055] Preparation of macromolecular initiator: 4g of tert-butyl methacrylate, 6.5g of isoamyl acrylate, 2g of hydroxybutyl acrylate and 7.25g of anisole were added to the reaction eggplant bottle for mixing and dissolving, then sealed for reaction bottle, freeze the system with liquid nitrogen-vacuumize-thaw, repeat three times; under the protection of argon, then add 0.26g cuprous chloride, 0.05g copper powder and 0.5g 2,5-thiophenedicarboxylic acid, seal the reaction bottle , and then freeze the system with liquid nitrogen-vacuumize-thaw-argon, repeat three times; finally put the reaction eggplant bottle into a 70°C oil bath, add 0.3g of initiator α-iodoisobutyronitrile, electromagnetic Stir for 15 hours, then add tetrahydrofuran to dilute, and then go through neutral alumina column chromatography. After most of the solvent volatilizes, the prepared polymer is precipitated with petroleum ether and vacuum-dried to obtain a macromolecular initiator.

[0056] Preparation of cr...

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Abstract

The invention discloses a cross-linked fluorine (methyl)-containing acrylic segmented copolymer and its preparation method and use, and belongs to the field of chemical materials. The preparation method comprises that various (methyl) acrylate functional monomers are copolymerized into the cross-linked fluorine (methyl)-containing acrylic segmented copolymer by an atom transfer radical polymerization (ATRP) method. A structure, molecular weight and molecular weight distribution of the cross-linked fluorine (methyl)-containing acrylic segmented copolymer can be controlled. The molecular weight of the cross-linked fluorine (methyl)-containing acrylic segmented copolymer is in a range of 10000 to 35000 and the molecular weight distribution is less than 1.4. The cross-linked fluorine (methyl)-containing acrylic segmented copolymer is mixed with a curing agent according to a certain ratio and the mixture self-assembles in a selective solvent so that a micellar solution having an average particle size of about 100 to 450nm is formed. Through a solvent evaporation film-forming method, the micellar solution is prepared into a super-hydrophobic coating film having a contact angle of more than 150 degrees, hardness H and second-level adhesion. The preparation method has simple and feasible operation processes, a low cost and a wide application prospect in the field of water-proofing and moisture-proofing coatings.

Description

technical field [0001] The invention belongs to the field of chemical materials and relates to a fluorine-containing block copolymer, in particular to a cross-linked fluorine-containing (meth)acrylic acid block copolymer and its preparation method and application. Background technique [0002] Fluorine-containing (meth)acrylate polymer refers to a type of (meth)acrylate resin with a C-F bond structure among (meth)acrylate resins. Many of the excellent properties of fluoropolymers are due to the large number of C-F chemical bonds contained in them. Therefore, it has excellent weather resistance, corrosion resistance, stain resistance, heat resistance, chemical resistance, hydrophobicity and oil repellency, insulation and low coefficient of friction. It is widely used in textile, leather, optical fiber, packaging, coating and other fields. [0003] Since the Q and E values ​​of fluorine-containing (meth)acrylates are similar to those of methacrylates, they have good homopoly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F220/18C08F220/14C08F220/28C08F220/22C08F220/24C09D175/04
Inventor 文秀芳罗永乐皮丕辉蔡智奇徐守萍程江
Owner SOUTH CHINA UNIV OF TECH
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