Fluorine-contained surfactant and preparation method thereof
A technology of surfactants and initiators, which is applied in the field of block polymers, fluorine-containing surfactants and their preparation, can solve problems such as difficulty in industrial production, impact on polymer performance, and complicated preparation process, and achieve excellent surface activity , fast polymerization speed and pure product
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Embodiment 1
[0037] Using diethyl ether as a solvent, 1'-ethoxyethoxy)propyl chloride and metal lithium undergo lithiation reaction in a high vacuum device to prepare (1'-ethoxyethoxy)propyllithium.
[0038] Polymerization adopts high vacuum (-3 Pa) and sealed anionic polymerization experiment technology. In the high vacuum polymerization device, 100 ~ 150mL THF is used as the polymerization solvent, 1.0mL 0.5mol / L 3 (1'-ethoxyethoxy) propyllithium is the initiator, and the initiator and C 3 f 7 CH 2 CH 2 CH 2 OCOCH=CH 2 (Molar ratio 1:1.2) After polymerization for 1 to 3 hours, quickly cool to -78°C with a liquid nitrogen / isopropanol bath, then slowly add 5.0 to 15.0 g of methyl styrene, and add 0.02 g of methyl styrene after polymerization for 0.5 to 1 hour. g CH 3 OH terminates the reaction. The reacted polymer is subjected to rotary evaporation at 60-70°C to remove the solvent, precipitation and purification with n-hexane, repeated three times, and finally dried in a vacuum oven...
Embodiment 2~4
[0040] Except for changing the type of fluorine-containing monomer in Example 1, the initiator, solvent, second monomer, and polymerization temperature are the same as those described in Example 1. Wherein the fluorine-containing monomers used are respectively: (CF 3 ) 2 CF(CF 2 ) 2 C(CH 3 ) 2 OCOCH=CH 2 , (CF 3 ) 3 CCF 2 CH 2 C(CH 3 ) 2 OCOCH=CH 2 、CF 3 CF 2 CF 2 (CF 3 ) CFCH 2 CH 2 CH 2 CH 2 OCOCH=CH 2 . The number average molecular weight of the obtained polymer is 9000-10000.
Embodiment 5~8
[0042] Except for changing the type of fluorine-containing monomer and the second monomer in Example 1, the initiator, solvent, and polymerization temperature are the same as those described in Example 1. Wherein the second monomer used is 4-cyanophenyl acrylate, and the first monomers containing fluorine are respectively: The number average molecular weight of the obtained polymer is 1000-100000.
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