Preparation of covalent organic framework material and application of covalent organic framework material in rare earth separation
A technology of covalent organic framework and rare earth, which is applied in the direction of improvement of process efficiency, other chemical processes, chemical instruments and methods, etc., to achieve the effect of simple preparation process, mild reaction conditions, and avoiding the use of organic solvents
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Embodiment 1
[0045] (1) Preparation of a low eutectic solvent: oxalic acid dihydrate (0.1 M) and choline chloride (0.1 M), heated 0.5h at 60 ℃ for forming colorless transparent homogeneous solution, chlorine derived choline - oxalic acid dihydrate eutectic solvent.
[0046] Preparation covalent organic framework material (2): 0.0210 g (0.10 mM) among the three aldehyde phloroglucinol (Tp) and 0.0162g (0.15 mM) of p-phenylenediamine (Pa) was added to a volume of 50.0 mL plastic centrifuge tube, followed by addition of 200 μL choline chloride - oxalic acid dihydrate eutectic solvent as a reaction medium and the aqueous acetic acid (8μL, 12 M) as a catalyst. Thereafter, by way of vigorous stirring to fully dissolve the monomer and the three mixed. The mixture was subsequently kept 72 h at the temperature at 25 ℃. The resulting solid precipitate was centrifuged at 8500 rpm precipitate was washed with tetrahydrofuran and ethanol, respectively (15 mL × 3) used. Finally, the obtained powder was dried...
Embodiment 2
[0048] (1) preparing a solvent eutectic melt: oxalic acid dihydrate (0.1M) and choline chloride (0.1 M), heated at 60 ℃ for 1h of a colorless transparent homogeneous solution, to obtain the chloride choline - oxalic acid dihydrate eutectic solvent.
[0049] Preparation covalent organic framework material (2): 0.0105 g (0.05 mM) among the three aldehyde phloroglucinol (Tp) and 0.0081g (0.075 mM) of p-phenylenediamine (Pa) was added to a volume of 50.0 mL plastic centrifuge tube, followed by addition of 200 μL choline chloride - oxalic acid dihydrate eutectic solvent as a reaction medium and the aqueous acetic acid (8μL, 12 M) as a catalyst. Thereafter, by way of vigorous stirring to fully dissolve the monomer and the three mixed. The mixture was subsequently kept 72 h at the temperature at 25 ℃. The resulting solid precipitate was centrifuged at 8500 rpm precipitate was washed with tetrahydrofuran and ethanol, respectively (15 mL × 3) used. Finally, the obtained powder was dried fo...
Embodiment 3
[0051] (1) Preparation of a low eutectic solvent: lactic acid (0.2 M) and choline chloride (0.1 M), heated 1h at 60 ℃ for forming colorless transparent homogeneous solution, i.e. choline chloride to give - lactic eutectic solvent.
[0052] Preparation covalent organic framework material (2): 0.0105 g (0.05 mM) among the three aldehyde phloroglucinol (Tp) and 0.0145g (0.05mM) tris (4-aminophenyl) amine (TAPA) was added to a volume of to 50.0 mL plastic centrifuge tube, followed by addition of 1mL choline chloride - lactic eutectic solvent as a reaction medium and a 17.5 M aqueous solution of acetic acid as a catalyst 200μL. Thereafter, by way of vigorous stirring to fully dissolve the monomer and the three mixed. Then the mixture was kept at a constant temperature for 24 h at 25 ℃ of. The resulting solid precipitate was centrifuged at 8500 rpm precipitate was washed with tetrahydrofuran and ethanol, respectively (15 mL × 3) used. Finally, the obtained powder was dried for 24 h in a...
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