Preparation of hybrid fluorine-containing surfactant and application in weak cationic fabric three-proof finishing agent
A surfactant and solvent technology, applied in the field of weak cationic fabric three-proof finishing agent, can solve the problems of refractory degradation, no signs of perfluorooctyl decomposition, hazards, etc.
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[0054] Preparation of "hybrid" type fluorosurfactant
[0055] 1. According to the percentage by weight, pour 30%-65% solvent into the reaction kettle, heat up to 110-150°C, and reflux the solvent for 30min; at the same time, add 15%-30% F(CF 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 After mixing OH, 30%-45% hydrogen iodide and 1%-10% catalyst evenly, carry out solution polymerization at 110-150°C for 6-12h, solid F(CF 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 I yield is higher than 90%;
[0056] 2. Synthesis, by weight percentage, first pour 30%-65% solvent into the reaction kettle, heat up to solvent reflux temperature; simultaneously add 15%-30% F(CF 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 I, 30%-45% N (C 2 h 5 ) 2 (CH 2 ) m After the OH is uniformly mixed, the solution polymerization is carried out for 24-72 hours, and the yield of the solid product hybrid fluorine-containing surfactant is higher than 80%.
Embodiment 1
[0058] Preparation of "hybrid" type fluorosurfactant
[0059] First, pour 50% by weight of the solvent into the reactor, heat up to about 120°C, and reflux the solvent for 30 minutes; simultaneously add 15% by weight of F(CF 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 OH, after the hydrogen iodide of 30% by weight and the catalyst of 5% by weight are mixed uniformly, carry out solution polymerization 6-12h at 120 ℃ of temperature, solid F (CF 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 I yield is 94.5%; The second step is synthetic, at first the solvent of 55% by weight is poured in the reactor, is warming up to solvent reflux temperature; Adds the F(CF of 15% by weight successively simultaneously) 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 I, 30% by weight of N (C 2 h 5 ) 2 (CH 2 ) m After the OH was uniformly mixed, the solution polymerization was carried out for 24 hours, and the yield of the solid product hybrid fluorosurfactant was 85.2%.
Embodiment 2
[0061] Preparation of "hybrid" type fluorosurfactant
[0062] First, 35% by weight of the solvent is poured into the reactor, the temperature is raised to 110° C., and the solvent is refluxed for 30 min; simultaneously, 15% by weight of F(CF 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 OH, after the hydrogen iodide of 45% by weight and the catalyst of 5% by weight are mixed uniformly, carry out solution polymerization 6-12h under the temperature of 110 ℃, solid F (CF 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 I yield is 95.2%; The second step is synthesized, first the solvent of 40% by weight is poured in the reactor, is warming up to solvent reflux temperature; Adds the F(CF of 15% by weight successively simultaneously) 2 ) n SO 2 N(C 2 h 5 )(CH 2 ) 2 I, 45% by weight of N (C 2 h 5 ) 2 (CH 2 ) m After the OH was uniformly mixed, the solution polymerization was carried out for 24 hours, and the yield of the solid product hybrid fluorosurfactant was 89.4%.
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