Method for preparing microemulsion of fluorinated ethylene propylene powder
A polyperfluoroethylene propylene and microemulsion technology is applied in the field of preparation of tetrafluoroethylene and hexafluoropropylene copolymer polyperfluoroethylene propylene, which can solve the problems of less research on monomer copolymerization and the like
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[0020] The microemulsion preparation method of above-mentioned polyperfluoroethylene propylene powder, concrete steps are as follows:
[0021] Add emulsifier and co-emulsifier into water, lower the temperature of the polymerization tank to -15~-18°C, and feed hexafluoropropylene gas to liquefy hexafluoropropylene to form O / W microemulsion. The tetrafluoroethylene and hexafluoropropylene monomers are fed into the initial mixed gaseous monomers and additional mixed gaseous monomers. An oil-soluble free radical initiator is injected to initiate polymerization. Under stirring conditions, the polymerization temperature is 25-45°C and the pressure is 1.1-1.5MPa. After the reaction is completed, the product is separated by raising the temperature. First, the temperature is raised to 45-65° C. to separate and recover the liquefied hexafluoropropylene. After evacuation, the water is released, and the obtained powder is heated in another airtight container at 120-200°C under vacuum fo...
Embodiment 1
[0025]Add 2500g of deionized water, 60g of ammonium perfluorooctanoate and 20g of n-amyl alcohol in a 5-liter reactor, vacuumize and cool to -18°C, then add 200g of hexafluoropropylene to the reactor, and feed 600g of the initial monomer mixture, where The mass ratio of tetrafluoroethylene to hexafluoropropylene is 15:85. Heating to 48° C. was carried out with stirring, and then 3 g of bis(perfluorobutyryl) peroxide dissolved in R113 at a concentration of 15% was injected. At this point, the reactor pressure was 1.5Mpa. Continue to feed additional monomer mixture to maintain this pressure, the mass ratio of tetrafluoroethylene to hexafluoropropylene is 80:20. The addition amount of the oil-soluble radical initiator is 0.04% of the total mass of the monomers. The copolymerization was carried out until 800 g of mixed monomers were added. Heating to 58°C under stirring conditions, the unreacted monomers were recovered. After 1 hour, the pressure is 0.1Mpa. Evacuate and repla...
Embodiment 2
[0027] Add 2500g of deionized water, 60g of ammonium perfluorooctanoate and 20g of cetyl alcohol in a 5-liter reactor, vacuumize and cool to -18°C, then add 200g of hexafluoropropylene into the reactor, and feed 600g of the initial monomer mixture , wherein the mass ratio of tetrafluoroethylene to hexafluoropropylene is 15:85. Heating to 48° C. was carried out with stirring, and then 4 g of perfluorobutyl peroxide dissolved in R113 with a concentration of 15% was injected. At this point, the reactor pressure was 1.5Mpa. Continue to feed additional monomer mixture to maintain this pressure, the mass ratio of tetrafluoroethylene to hexafluoropropylene is 80:20. The addition amount of the oil-soluble radical initiator is 0.03% of the total mass of the monomers. The copolymerization was carried out until 800 g of mixed monomers were added. Heating to 58°C under stirring conditions, the unreacted monomers were recovered. After 1 hour, the pressure is 0.1Mpa. Evacuate and repla...
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