Biquaternary ammonium salt type cation fluorocarbon gemini surfactant and preparation method thereof
A technology of gemini surface and double quaternary ammonium salt, applied in chemical instruments and methods, fire prevention equipment, dissolution, etc., can solve the problems of harsh synthesis conditions, poor surface tension performance, and expensive fluorocarbon surfactants, etc., and achieve simple process , The effect of easy access to raw materials
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Embodiment 1
[0034] a) Mix dipropylene glycol methyl ether, N,N'-dimethyl-1,3-propanediamine and triethylamine, stir well, slowly add perfluoro 2-5-dimethyl and 3-6 -Dioxynonanoyl fluoride lactone, reacted at 50°C for 14h, then distilled under reduced pressure to obtain the crude product of fluorocarbon gemini surfactant intermediate;
[0035] b) Add ethylene glycol butyl ether and ice-water mixture to the crude fluorocarbon gemini surfactant intermediate obtained in step a), recrystallize 5 times, and dry the obtained crystalline product in a vacuum drying oven at 70° C. for 10 h, Obtain fluorocarbon gemini surfactant intermediate;
[0036] c) Add ethanol to the fluorocarbon gemini surfactant intermediate obtained in step b) to dissolve, and after stirring evenly, slowly add 1,6-dibromohexane dropwise, reflux at 50°C for 15 hours, and then add ethyl alcohol The mixture of glycol butyl ether and ice water is recrystallized 4 times, and then the crystallized product is dried to obtain the ...
Embodiment 2
[0040] a) Mix dipropylene glycol methyl ether, N,N'-dimethyl-1,3-propanediamine and triethylamine, stir well, slowly add perfluoro 2-5-dimethyl and 3-6 -Dioxynonanoyl fluoride lactone, after reacting at 85°C for 5h, distilling under reduced pressure to obtain the crude product of fluorocarbon gemini surfactant intermediate;
[0041] b) Add ethylene glycol butyl ether and ice-water mixture to the crude fluorocarbon gemini surfactant intermediate obtained in step a), recrystallize 6 times, and dry the obtained crystalline product in a vacuum drying oven at 95° C. for 6 hours, Obtain fluorocarbon gemini surfactant intermediate;
[0042] c) Add ethanol to the fluorocarbon gemini surfactant intermediate obtained in step b) to dissolve, and after stirring evenly, slowly add 1,6-dibromohexane dropwise, react at reflux for 5 hours at 80°C, and then add ethyl alcohol The mixture of glycol butyl ether and ice water is recrystallized twice, and then the crystalline product is dried to o...
Embodiment 3
[0046] a) Mix dipropylene glycol methyl ether, N,N'-dimethyl-1,3-propanediamine and triethylamine, stir well, slowly add perfluoro 2-5-dimethyl and 3-6 -Dioxynonanoyl fluoride lactone, reacted at 60°C for 12h, then distilled under reduced pressure to obtain the crude product of fluorocarbon gemini surfactant intermediate;
[0047] b) Add ethylene glycol butyl ether and ice-water mixture to the crude fluorocarbon gemini surfactant intermediate obtained in step a), recrystallize 6 times, and dry the obtained crystalline product in a vacuum drying oven at 85° C. for 9 hours, Obtain fluorocarbon gemini surfactant intermediate;
[0048] c) Add ethanol to the fluorocarbon gemini surfactant intermediate obtained in step b) to dissolve, and after stirring evenly, slowly add 1,6-dibromohexane dropwise, react at reflux for 7 hours at 70°C, and then add ethyl alcohol Glycol butyl ether and ice-water mixture, recrystallized 3 times, and then dried the crystalline product to obtain formul...
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