A kind of binaphthol-based sulfonated polyarylether ketone sulfone compound and preparation method thereof
A technology for sulfonated polyaryletherketone and polyaryletherketone sulfone, which is applied in the field of sulfonated polyaryletherketone sulfone compounds and its preparation, can solve the problem of low polymer molecular weight and proton conductivity, low methanol permeability and anti-oxidation stability In order to achieve the effect of easy access and excellent proton conductivity
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Embodiment 1
[0032] The preparation of embodiment 1 ABA type oligomer
[0033] Mix 1.7519 g (7.0 mmol) 4,4'-dihydroxydiphenylsulfone, 12.2192 g (56.0 mmol) 4,4'-difluorobenzophenone, 2.2000 g potassium carbonate and 20 mL N,N-dimethylethyl The amide was added to a three-necked flask, and under the protection of argon, the temperature was raised to 80°C, and the reaction was performed under magnetic stirring for 12 hours. After the reaction, the reaction solution was poured into deionized water to precipitate a precipitate, and the precipitate was collected by filtration and dried, and then purified by a column. Obtain ABA type oligomer, productive rate is 98%, and its proton nuclear magnetic resonance spectrum data is: 1 H NMR (400 MHz, CDCl 3 , ppm), 7.12 (m, 8H), 7.83 (s, 4H), 7.85 (s, 4H), 7.95 (s, 4H), 7.97 (s, 4H).
Embodiment 2
[0034] Example 2 Preparation of binaphthol-based polyaryl ether ketone sulfone compound containing 50mol% binaphthyl groups
[0035] Add 0.5727 g (2 mmol) of 1,1'-bi-2-naphthol, 1.3733 g (2 mmol) of ABA-type oligomers and 16 mL of N,N-dimethylacetamide into a three-necked flask, dissolve, and then add 1.0000 g of potassium carbonate and 8 mL of toluene, under the protection of argon, first react at 140°C for 2 hours, then distill off the toluene, then raise the temperature to 160°C, react for 24 hours, then pour into deionized water to precipitate precipitation, The precipitate was collected and dried in an oven at 80 °C for 24 hours to obtain a binaphthol-based polyaryletherketone sulfone compound containing 50 mol% binaphthyl groups with a yield of 99%. After characterization, its number average molecular weight is 51kDa, and the data of its proton nuclear magnetic resonance spectrum are: 1 H NMR (400 MHz, CDCl 3 , ppm), 6.79 (d, 4H), 7.05 (s, 2H), 7.10 (s,2H), 7.25 (s, 2H...
Embodiment 3
[0036] Example 3 Preparation of binaphthol-based polyaryletherketone sulfone compounds containing 43mol% binaphthyl groups
[0037] In Example 2, the feeding amount of 1,1'-bi-2-naphthol was changed to 0.4075 g (1.72 mmol), and the feeding amount of ABA oligomer was changed to 1.5656 g (2.28 mmol). After adding these two At the same time as the compound, 0.3753 g (1.72 mmol) 4,4'-difluorobenzophenone was added, and the remaining operations were the same as in Example 2 to obtain a binaphthol-based polyaryletherketone sulfone containing 43mol% binaphthyl groups Compound, the yield is 98%. Characterized, its number average molecular weight is 35kDa.
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