METHOD FOR PREPARING A COMPOSITION COMPRISING PERFLUOROPOLYETHER HAVING A HYDROXYL GROUP AT ONE TERMINAL and method for increasing the content ratio of the compound
A technology of perfluoropolyether and manufacturing method, which is applied in chemical instruments and methods, separation methods, chemical/physical processes, etc., to achieve the effect of reducing the amount of use and the impact of environmental load.
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Embodiment 1
[0134] Make 10g of composition F60 in supercritical carbon dioxide as mobile phase, and filled with silica gel 60-NH 2 (manufactured by Kanto Chemical Co., Ltd., particle size: 40 μm to 50 μm, weakly alkaline: pH 9.5 (25° C., value in the state of 10% by weight aqueous suspension), dry-filled) in a 25 mL high-pressure vessel. The flow rate of the mobile phase was 5ml / min, and the temperature was 40°C. Change the pressure from 11MPa to 25MPa. In detail, first flow carbon dioxide adjusted to a supercritical state at 40°C and 11 MPa, fractionate components for 60 minutes at a mobile phase pressure of 11 MPa, then set the mobile phase pressure to 15 MPa and fractionate The components were separated for 60 minutes, then the pressure of the mobile phase was set to 25 MPa and the components were fractionated for 60 minutes. The ratio of the components contained in each component is shown in Table 2 below. The composition ratio is utilized 19 F-NMR to confirm.
[0135] [Table 2] ...
Embodiment 2
[0138] Make 10g of composition F70 in supercritical carbon dioxide as mobile phase, and filled with silica gel 60-NH 2 (manufactured by Kanto Chemical Co., Ltd., particle size: 40 μm to 50 μm, weakly alkaline: pH 9.5 (25° C., value in the state of 10% by weight aqueous suspension), dry-filled) in a 25 mL high-pressure vessel. The flow rate of the mobile phase was 5ml / min, and the temperature was 40°C. Change the pressure from 11MPa to 25MPa. Specifically, first, carbon dioxide adjusted to a supercritical state was passed through at 40° C. and 11 MPa, fractionated for 60 minutes at a mobile phase pressure of 11 MPa, and then the mobile phase pressure was set to 15 MPa and separated. The components were taken for 60 minutes, then the pressure of the mobile phase was set to 25 MPa and the components were taken for 60 minutes. The ratio of the components contained in each component is shown in Table 3 below. The composition ratio is utilized 19 F-NMR to confirm. In addition, ...
Embodiment 3
[0142] Make 10g of composition F80 in supercritical carbon dioxide as mobile phase, and filled with silica gel 60-NH 2 (manufactured by Kanto Chemical Co., Ltd., particle size: 40 μm to 50 μm, weakly alkaline: pH 9.5 (25° C., value in the state of 10% by weight aqueous suspension), dry-filled) in a 25 mL high-pressure vessel. The flow rate of the mobile phase was 5ml / min, and the temperature was 40°C. Change the pressure from 11MPa to 25MPa. In detail, first flow carbon dioxide adjusted to a supercritical state at 40°C and 11 MPa, fractionate components for 60 minutes at a mobile phase pressure of 11 MPa, then set the mobile phase pressure to 15 MPa and fractionate The components were separated for 60 minutes, then the pressure of the mobile phase was set to 25 MPa and the components were fractionated for 60 minutes. The ratio of the components contained in each component is shown in Table 4 below. The composition ratio is utilized 19 F-NMR to confirm. In addition, the co...
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