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Method for preparing fluorine-containing waterproof and oil-proof agent through emulsifier-free emulsion polymerization

A technology of soap-free emulsion polymerization and water and oil repellent, which is applied in the preparation of fluorine-containing water and oil repellent, and in the field of preparation of fluorine-containing water and oil repellent by soap-free emulsion polymerization, which can solve the problems of large emulsion particle size, environmental problems, and film formation. To solve problems such as poor performance, achieve excellent water and oil repellency, improve adhesion fastness, and improve washability

Active Publication Date: 2014-02-12
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing fluorine-containing water and oil repellent by soap-free emulsion polymerization, which solves the problems of large particle size, poor film-forming property, gloss and water resistance of the existing emulsion in the water-soluble monomer copolymerization method. Poor stability, poor stability and low solid content of the emulsion, the addition of a co-solvent method will lead to an increase in the VOC value of the aqueous emulsion, and there are environmental problems and potential safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038]Step 1: Weigh 2.8g of fluorine-containing amphiphilic block copolymer, 81g of deionized water, 0.6g of potassium hydroxide, and 8.9g of 1.8% ammonium persulfate aqueous solution. Mix the above-mentioned components weighed, and stir and dissolve at room temperature in a reactor equipped with a stirrer, reflux device, feeding device and thermometer to obtain a mixed solution, then add the mixed monomers, and pass argon for 30 minutes under stirring conditions ; The mass ratio of the added mixed monomer to the mixed solution is 1:7.5;

[0039] Wherein the fluorine-containing amphiphilic block copolymer is polymethacrylic acid-b-polyhexafluorobutylmethacrylate containing thiocarbonate end groups, the number average molecular weight is 1650g / mol, and the molecular weight distribution is 1.2.

[0040] Step 2: Raise the temperature to 80°C, and within 80 minutes, drop the mixed monomer and initiator aqueous solution into the reactor again; the mass ratio of the mixed monomer ad...

Embodiment 2

[0057] Step 1: Weigh 3.5g of fluorine-containing amphiphilic block copolymer, 88g of deionized water, 1.1g of sodium carbonate, and 14.1g of an aqueous potassium persulfate solution with a mass concentration of 1.8%. Mix the above-mentioned components weighed, and stir and dissolve at room temperature in a reactor equipped with a stirrer, reflux device, feeding device and thermometer to obtain a mixed solution, then add the mixed monomers, and pass argon for 30 minutes under stirring conditions ; The mass ratio of the added mixed monomer to the mixed solution is 1:5.3;

[0058] Wherein the fluorine-containing amphiphilic block copolymer is polymethacrylic acid-b-polyhexafluorobutylmethacrylate containing thiocarbonate end groups, the number average molecular weight is 2040g / mol, and the molecular weight distribution is 1.4.

[0059] Step 2: Raise the temperature to 82°C, and within 150 minutes, add the mixed monomer and potassium persulfate aqueous solution with a mass concent...

Embodiment 3

[0069] Step 1: Weigh 3.2g of fluorine-containing amphiphilic block copolymer, 85g of deionized water, 0.9g of triethylamine, and 11.5g of an aqueous sodium persulfate solution with a mass concentration of 1.8%. Mix the above-mentioned components weighed, and stir and dissolve at room temperature in a reactor equipped with a stirrer, reflux device, feeding device and thermometer to obtain a mixed solution, then add the mixed monomers, and pass argon for 30 minutes under stirring conditions ; The mass ratio of the added mixed monomer to the mixed solution is 1:6.4;

[0070] Wherein the fluorine-containing amphiphilic block copolymer is polymethacrylic acid-b-polyhexafluorobutylmethacrylate containing thiocarbonate end groups, the number average molecular weight is 3210g / mol, and the molecular weight distribution is 1.3.

[0071] Step 2: Raise the temperature to 85°C, and within 120 minutes, drop the mixed monomer and an aqueous sodium persulfate solution with a mass concentratio...

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Abstract

The invention discloses a method for preparing fluorine-containing waterproof and oil-proof agent through emulsifier-free emulsion polymerization. The fluorine-containing polyacrylate fabric waterproof and oil-proof agent is prepared by taking thiocarbonate active end group-containing fluorine-containing amphiphilic block copolymer as an emulsifier. Compared with a micromolecular emulsifier, the fluorine-containing polyacrylate emulsifier-free emulsion prepared by adopting the amphiphilic block copolymers not only has high stability and high solid content, but also has excellent waterproof and oil-proof properties. Meanwhile, an organic solvent is not used in the method, so that the harm of the organic solvent on human health and environments can be avoided. In addition, a crosslinked monomer is selected to improve the washability, and enables the polymer to have reactive hydroxyl group which can be crosslinked with a reaction group on fiber or be self-crosslinked, so that the adhesion degree of a finishing agent on the fiber can be enhanced, and the washability can be improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of water and oil repellents, and relates to a preparation method of a fluorine-containing water and oil repellent, in particular to a method for preparing a fluorine-containing water and oil repellent by soap-free emulsion polymerization. Background technique [0002] Fluoropolymers are very attractive functional materials due to their high thermal stability, excellent chemical resistance, mechanical properties, aging resistance, and low surface energy. Fluoropolymer-modified polyacrylate not only maintains the good film-forming properties, flexibility and adhesion of polyacrylate, but also has the excellent performance of fluoropolymers, and is widely used in waterproof finishing and repellent of textiles. Oil finishing etc. [0003] In recent years, with people's increasing awareness of resources and environmental protection, water-based fluorinated polyacrylate emulsions have become a rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/18C08F220/14C08F220/22C08F220/28C08F2/24C08F287/00D06M15/277
Inventor 周建华段昊王海龙
Owner SHAANXI UNIV OF SCI & TECH
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