Separation method of carboxylic acid compound containing perfluoro(poly)ether group
A compound and ether group technology, which is applied in the field of separation of carboxylic acid compounds containing perfluoroether groups, can solve the problems of cumbersome manufacturing steps and heavy manufacturing equipment costs
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Embodiment 1～26 and comparative example 1～13
[0242] As a stationary phase for thin-layer chromatography, prepare a silica gel thin-layer plate (manufactured by Merck, 105715 TLC glass plate silica gel 60F) with a length of 5 cm and a width of 1.5 cm. 254 ).
[0243] CF as a monocarboxylic acid compound containing a perfluoro(poly)ether group 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CO 2 H0.1g, HO as a dicarboxylic acid compound containing a perfluoro(poly)ether group 2 CCF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CO 2 0.1 g of H was dissolved in 1 ml of m-xylene hexafluoride, which is a nonpolar solvent containing fluorine atoms, to prepare a sample solution.
[0244] The obtained sample solution was spotted at a position 5 mm from the lower end of the silica gel thin-layer plate using a glass microcapillary in an amount of 2 to 10 μl, and allowed to dry. This spotting position is used as the development start point (origin).
[0245] In the developing tank for thin-layer chromatography, the polar...
Embodiment 27
[0286] In a 50ml 3-necked flask equipped with a thermometer and a stirrer, the average composition CF 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CO 2 H. HO 2 CCF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CO 2 H. CF 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CF 3 7 g of the indicated perfluoropolyether carboxylic acid mixture, 35 ml of perfluorohexane, and 20 g of silica gel (manufactured by Fuji Silicone, PSQ-100B) were stirred at 25° C. for 1 hour. Thereafter, the silica gel in the reaction solution was filtered through Celite, the silica gel was washed with 100 ml of perfluorohexane, and the filtrate was concentrated under reduced pressure to obtain CF 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CF 3 1.69 g (24.1%).
[0287] Next, the silica gel was treated with Novec (商标) 7200 / CF 3 CH 2 After washing with 100ml of OH(6 / 4), the filtrate was concentrated under reduced pressure to obtain CF 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 C...
Embodiment 28
[0289] In a 50ml 3-necked flask equipped with a thermometer and a stirrer, the average composition CF 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CO 2 H. HO 2 CCF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CO 2 H. CF 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CF 3 7 g of the indicated perfluoropolyether carboxylic acid mixture, 35 ml of perfluorohexane, and 20 g of silica gel (manufactured by Fuji Silicone, PSQ-100B) were stirred at 25° C. for 1 hour. Thereafter, the silica gel in the reaction solution was subjected to Celite filtration, the silica gel was washed with 100 ml of perfluorohexane, and the filtrate was concentrated under reduced pressure to obtain CF 3 CF 2 CF 2 O(CF 2 CF 2 CF 2 O) 20 CF 2 CF 2 CF 3 1.69 g (24.1%).
[0290] Next, the silica gel was treated with Novec (商标) 7200 / CF 3 CF 2 CH 2 After washing with 100ml of OH(6 / 4), the filtrate was concentrated under reduced pressure to obtain CF 3 CF 2 CF 2 O(CF 2 CF 2 C...
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