Stabilized fluoropolymer and method for producing same
a technology of stabilized fluoropolymer and stabilized fluoride, which is applied in the direction of cell components, final product manufacturing, sustainable manufacturing/processing, etc., can solve the problems of insufficient rate of conversion of unstable groups to stable groups, contaminating the wastewater discharged from fuel cells, discoloration and freezing, etc., and achieves high-quality fuel cell membranes, excellent chemical stability, and low fluoride ion concentration
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example 1
(1) Polymer Synthesis
[0209]A 3000-ml stainless steel stirring autoclave was charged with 300 g of a 10% aqueous solution of C7F15COONH4 and 1170 g of pure water, followed by thorough evacuation and nitrogen substitution. After sufficiently evacuating the autoclave, tetrafluoroethylene [TFE] gas was fed to the autoclave until a gage pressure of 0.2 MPa, and the temperature was raised to 50° C. Then, 100 g of CF2═CFOCF2CF2SO2F was injected into the autoclave, and the gage pressure was raised to 0.7 MPa by introduction of TFE gas. Thereafter, an aqueous solution of 0.5 g of ammonium persulfate [APS] in 60 g of pure water was injected to start the polymerization. For supplementing the TFE consumed by polymerization, TFE was continuously fed to the autoclave so that the autoclave inside pressure might be maintained at 0.7 MPa. The polymerization was continued while continuously feeding CF2═CFOCF2CF2SO2F in an amount of 53% by mass relative to the TFE further fed.
[0210]After completion of...
example 2
[0228]The membrane obtained in Example 1 (2) was treated in a 20% aqueous solution of sodium hydroxide at 90° C. for 24 hours and then washed with water. It was then treated in 6 N sulfuric acid at 60° C. for 24 hours and then washed with water until the washings showed neutrality, to give a sulfonic acid form membrane.
[0229]This membrane was thoroughly dried at 110° C., and 3 g of the dried membrane was taken and subjected to stability testing by Fenton treatment 1. The fluoride ion concentration was 5 ppm.
example 3
(1) Polymer Synthesis
[0232]A 3000-ml stainless steel stirring autoclave was thoroughly evacuated, followed by nitrogen substitution. The autoclave was again thoroughly evacuated and, then, charged with 1530 g of perfluorohexane and 990 g of CF2═CFOCF2CF2SO2F, and the temperature was adjusted to 25° C. Then, tetrafluoroethylene [TFE] gas was introduced until arrival of the gage pressure at 0.30 MPa, followed by introduction under pressure of 13.14 g of a 10% (by mass) solution of the polymerization initiator (C3F7COO)2 in perfluorohexane to initiate the polymerization reaction. For supplementing the TFE consumed by polymerization, TFE was continuously fed to the autoclave so that the autoclave inside pressure might be maintained at 0.30 MPa. The polymerization was continued while further feeding a total of 47 g of CF2═CFOCF2CF2SO2F intermittently.
[0233]After completion of feeding of 73 g of TFE, the autoclave inside pressure was released and the polymerization was thereby terminated....
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