Crosslinking self-emulsifying cation full fluorine copolymer soap-free emulsion and preparation thereof

A technology of perfluorinated copolymer and soap-free emulsion, applied in the field of polymer chemistry, can solve the problems of low conversion rate of fluorine monomer, poor film-forming property, water- and oil-repellent performance of fluorine-containing emulsion and unfavorable environmental protection, etc. effect, good film-forming properties, improved storage stability and dilution stability

Inactive Publication Date: 2009-08-19
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a cross-linked self-emulsifying cationic perfluorinated soap-free emulsion and its preparation method, to overcome the poor film-forming property

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: a kind of cross-linking type self-emulsifying cationic perfluorinated copolymer soap-free emulsion, is prepared by following method, and this method comprises the following steps successively:

[0036] (1) Preparation of monomer pre-emulsion mixture: 20 g of acryloyloxyethyltrimethylammonium chloride, 30 g of methyl acrylate, perfluoroalkyl (meth) acrylate (CH 2 =(R)C(O)CO(CH 2 ) 2 (CF 2 ) n CF 3 , where R is CH 3 , n is 5) 100g and 1.5g of hydroxyethyl acrylate, mix uniformly to prepare mixture solution A; then mix mixture solution A and azobisisobutyronitrile 0.755g to obtain mixture solution B, and mix solution B by mechanical stirring Mix well under pre-emulsification.

[0037](2) Preparation of water-soluble perfluoroalkyl acrylate prepolymer: Add solution B dropwise to 91 g of methyl ethyl ketone at 70°C for 0.5 hours, then continue polymerization for 2 hours to obtain perfluoroalkyl acrylate The methyl ethyl ketone solution C of the prepolyme...

Embodiment 2

[0039] Embodiment 2: a kind of crosslinking type self-emulsifying cationic perfluoro copolymer soap-free emulsion, is prepared by the following method, and this method comprises the following steps successively:

[0040] (1) Preparation of monomer pre-emulsion mixture: mix 35g of methacryloyloxyethyltrimethylammonium chloride with 36g of butyl acrylate, perfluoroalkyl (meth)acrylate (CH 2 =(R)C(O)CO(CH 2 ) 2 (CF 2 ) n CF 3 , R is H atom in the formula, n is 7) 100g and hydroxyethyl acrylate 1.8g, mix uniformly and make mixture solution A; Mix mixture solution A and azobisisoheptanonitrile 1.5g again and obtain mixture solution B, The mixture solution B was pre-emulsified and mixed uniformly under ultrasound.

[0041] (2) Preparation of water-soluble perfluoroalkyl acrylate prepolymer: Add solution B dropwise to 156 g of isopropyl acetate at 85°C for 1 hour, then continue to polymerize for 3 hours to obtain perfluoroalkane An isopropyl acetate solution C of an alkyl acryl...

Embodiment 3

[0043] Embodiment 3: a kind of cross-linking type self-emulsifying cationic perfluoro copolymer soap-free emulsion, is prepared by the following method, and this method comprises the following steps successively:

[0044] (1) Preparation of monomer pre-emulsion mixture: 30 g of acryloyloxyethyltrimethylammonium chloride, 45 g of butyl methacrylate, perfluoroalkyl (meth) acrylate (CH 2 =(R)C(O)CO(CH 2 ) 2 (CF 2 ) n CF 3 , where R is CH 3 , n is 11) 100g and 2.5g of hydroxyethyl methacrylate, mixed uniformly to obtain a mixture solution A; then mixed the mixture solution A and benzoyl peroxide 1g to obtain a mixture solution B, and the mixture solution B was ultrasonically Pre-emulsified and mixed evenly;

[0045] (2) Preparation of water-soluble perfluoroalkyl acrylate prepolymer: Add solution B dropwise to 200 g of tetrahydrofuran at 65°C for 2 hours, then continue to polymerize for 3 hours to obtain perfluoroalkyl acrylate THF solution C of the prepolymer; then add 300...

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Abstract

The invention belongs to the polymer chemistry field, in particular to a cross-linking self-emulsifying cationic perfluorocopolymer soap-free emulsion and a preparation method thereof. The soap-free emulsion overcomes the problems of the prior art such as poor film forming property, low conversion rate of fluoride monomer, and adverse impact on water resistance and oil resistance of fluorine-containing emulsion products and environmental protection. The technical proposal is as follows: the cross-linking self-emulsifying cationic perfluorocopolymer soap-free emulsion is prepared by the following method: (1) preparing a monomer pre-emulsion mixture: mixing a cationic monomer with vinyl monomer, perfluoroalkyl (methyl) acrylate and a functional monomer to obtain a mixture solution A; and then mixing the mixture solution A with an oil soluble initiator to obtain a mixture solution B, pre-emulsifying and evenly mixing the mixture solution B by ultrasonic agitation or mechanical agitation; (2) preparing a water soluble perfluoroalkyl acrylate prepolymer; and (3) preparing the perfluoroacrylate copolymer soap-free emulsion. The cross-linking self-emulsifying cationic perfluorocopolymer soap-free emulsion has the advantages of good stability, good film forming property of film coating, high conversion rate of the fluoride monomer, safety and environmental protection.

Description

technical field [0001] The invention belongs to the field of polymer chemistry, in particular to a cross-linked self-emulsifying cationic perfluoro copolymer soap-free emulsion and a preparation method thereof. Background technique [0002] Perfluoroalkyl acrylate copolymers have unique surface energy characteristics, so they can give fabrics, leather, paper and other substrates excellent water, oil, and antifouling effects, including solution type and emulsion type, but considering safety issues and the environment The problem is that this kind of polymer is mainly used in the form of water-dispersed emulsion. [0003] But judging from the current use situation, the perfluoroalkyl acrylate polymer also has the following problems: 1. The film-forming property is poor: the film-forming property is not good, and the crystallization performance of the film is not good, which leads to the polymer's crystallinity. Poor adhesion, defects in film flexibility, etc.; 2. Low conversi...

Claims

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Application Information

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IPC IPC(8): C08F220/24C08F220/12C08F2/22
Inventor 李培枝沈一丁杨晓武李刚辉唐新
Owner SHAANXI UNIV OF SCI & TECH
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