Process to prepare fluoropolymer dispersions and membranes
A polymer and dispersion technology, applied in the direction of solid electrolyte, final product manufacturing, sustainable manufacturing/processing, etc., can solve the problems that cannot be used as a large-scale solvent for dispersion casting medium, difficult to dissolve or disperse, etc.
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Embodiment 1-8
[0041] Poly(PSEPVE-co-TFE) and poly(PSEVE-co-TFE) partial hydrolysis and dispersion formation
Embodiment 1
[0043] 52.3 grams of poly(PSEPVE-co-TFE), which is a copolymer of tetrafluoroethylene (TFE) and perfluoro(3,6-dioxa-4-methyl-7-octenesulfonyl fluoride) (PSEPVE) material with an equivalent weight of 647 g / mol (80.8 mmol SO 2 F)) was divided into small portions and filled in dry 1 liter 3 neck round bottom (RB) flasks. The flask was equipped with mechanical stirring, a heating mantle, a reflux condenser with a nitrogen pad, and a thermocouple. Add approximately 185 ml of 2H-perfluoro(5-methyl-3,6-dioxanonane) ( E2) and slowly dissolve the polymer with stirring and heating to gentle reflux for 0.5 hours. Heat was reduced and the solution was cooled to 50-70°C. Then 60 mL of N,N-dimethylformamide (DMF) was slowly added via syringe (stirred at approximately 320-RPM), resulting in a translucent mixture. A solution of 4.90 g (48.4 mmol) triethylamine (TEA), 1.74 g water (96.7 mmol) and approximately 20 mL DMF was then added via syringe over 5 minutes. After 10 minutes, the mix...
Embodiment 2
[0045] 50.1 g of poly(PSEPVE-co-TFE) copolymer (77.4 mmol SO 2 F) Divide into small portions and fill in dry 500 ml 3 neck round bottom (RB) flasks. The flask was equipped with mechanical stirring, a heating mantle, and a reflux condenser with a nitrogen blanket. Add about 175ml E2 and slowly dissolve the polymer under stirring and moderate heating (50-60° C.) for 1-2 hours. With stirring at 320-RPM, 125 mL of DMF was slowly added via syringe. The mixture was homogenized with up to about 80 mL of DMF. Further addition of DMF provided a white emulsion. Then 4.73 g (46.7 mmol) TEA was added via pipette, followed by approximately 1.85 g (103 mmol) water. The emulsion was heated to gentle reflux and held at this temperature for about 1.5 hours. Reduce the heat and cool the emulsion below reflux temperature. The mechanical stirring was replaced with magnetic stirring and the reflux condenser was replaced with a short path distillation unit. The mixture was distilled under...
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