Crosslinking self-emulsifying cation full fluorine copolymer soap-free emulsion and preparation thereof
A perfluorinated copolymer and soap-free emulsion technology, applied in the field of polymer chemistry, can solve the problems of poor film-forming property, fluorine-containing emulsion waterproof and oil-proof performance and environmental protection, low conversion rate of fluorine monomer, etc., to achieve film-forming Good performance, improve storage stability and dilution stability, and eliminate adverse effects
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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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