Aminophenol type bidentate Schiff base ligand functional polymer-rare earth complex luminescent material and preparation method thereof
A technology of bidentate Schiff bases and rare earth complexes, applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of uneven dispersion of rare earth complexes, poor performance of polymer matrix, etc.
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[0052] The preparation method of the aminophenol type bidentate Schiff base ligand functionalized polymer-rare earth complex luminescent material comprises the following steps:
[0053] In the first step, add 0.40-0.50 g of polymer to 50 mL of solvent to fully dissolve, then add 0.85-0.95 g of p-chloromethyl benzaldehyde and 0.14-0.16 mL of catalyst, heat up to 60-80 ° C, N 2 React at a constant temperature for 10-12 h in the atmosphere. After the reaction, the polymer is precipitated with ethanol. The polymer is alternately washed with dilute hydrochloric acid, ethanol and distilled water, and dried in vacuum to constant weight to obtain the side chain bonded benzaldehyde (BA) ligand modified polymers;
[0054] In the second step, 0.40-0.50g of the modified polymer prepared in the first step with a side chain-bonded benzaldehyde (BA) ligand or directly using 0.40-0.50g of a side-chain-bonded acetaldehyde (AL) group The modified polymer (prepared according to the method descr...
Embodiment 1
[0062] Example 1: In a four-neck flask, add 0.4g modified polysulfone PSF-AL and 50 mL DMAC, after fully dissolved, then add 0.18g OAP, heat up to 70°C, N 2 React at a constant temperature in the atmosphere for 9 hours. After the reaction, the polymer is precipitated with ethanol. The polymer is washed alternately with ethanol and distilled water, and dried in vacuum until it reaches a constant weight. Polymer PSF-AO, the bonding amount of ligand AO is 1.15mmol / g.
[0063] Dissolve 0.3 g of the functionalized polymer PSF-AO in 50 mL of DMAC, adjust the pH to 7~8 with NaOH solution, then add 0.043 g of terbium trichloride crystals, raise the temperature to 65 °C, and react at constant temperature for 10 h. Precipitate the polymer with ethanol, wash the polymer with water, and dry to obtain the aminophenol-type bidentate Schiff base ligand functionalized polymer-rare earth binary complex luminescent material PSF-(AO) 3 -Tb(III).
[0064] Dissolve 0.35 g of the functionalized p...
Embodiment 2
[0065]Example 2: In a four-neck flask, add 50 mLDMAC and 0.44 g PSF to fully dissolve the PSF, then add 0.92 g p-chloromethylbenzaldehyde and 0.15 mL anhydrous tin tetrachloride, keep the temperature at 70 °C, 2 The reaction was stirred under atmosphere for 12h. After the reaction, the polymer was precipitated with ethanol, and the polymer was alternately washed with dilute hydrochloric acid, ethanol and distilled water, and dried in vacuum to constant weight to obtain the modified polysulfone PSF-BA with side chain bonded benzaldehyde (BA) ligand. The benzaldehyde bonded amount was 1.78 mmol / g.
[0066] In the four-neck flask, add 0.5 g modified polysulfone PSF-BA and 50 mL DMAC, after fully dissolved, add 0.19 g OAP, heat up to 65 °C, N 2 React at a constant temperature in the atmosphere for 8 hours. After the reaction, the polymer is precipitated with ethanol. The polymer is alternately washed with ethanol and distilled water, and dried in vacuum to a constant weight. Pol...
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