Rare earth complex and process for preparing the same
A technology of rare earth complexes and complexes, applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc., can solve the problem of low luminous efficiency, inability of ligands to convert light, and short luminous lifetime and other problems, to achieve the effect of simple preparation process
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Embodiment 1
[0027] Embodiment 1: 3, the synthesis of 5-dihydroxybenzoic acid methyl ester
[0028] In a 250ml three-necked bottle, add 50g of chemically pure 3,5-dihydroxybenzoic acid to a 100ml solution of methanol with a concentration of 99.7% by weight, that is, 3,5-dihydroxybenzoic acid with a weight percentage of 99.7% The molar ratio of methanol is 1:10, then add 0.1g of catalyst p-toluenesulfonic acid, the reaction temperature is 70°C, and the reaction time is 10 hours, the prepared liquid is then dissolved with 100ml of deionized water to dissolve its unreacted (3,5-dihydroxybenzoic acid and methanol), after stirring for 20 minutes, the layers were separated, and the lower oil layer was taken to obtain 3,5-dihydroxybenzoic acid methyl ester with a yield of 95%.
Embodiment 2
[0029] Example 2: Ligand M 1 Synthesis
[0030]Put the above-mentioned 14mmol of 3,5-dihydroxybenzoic acid methyl ester and 28mmol of chemically pure terephthaloyl chloride into 99.7% by weight concentration of N,N-dimethylformamide solvent 50ml, and dropwise add React with 2.5ml of chemically pure pyridine liquid, the reaction temperature is 95°C, and the reaction time is 8 hours, until no HCl is released; the reaction solution is cooled to room temperature and then poured into deionized water, and the stirring time is 15 minutes to obtain a white powder; The white powder was repeatedly washed with deionized water for 3 times, filtered and dried to obtain the ligand M 1 .
Embodiment 3
[0031] Embodiment 3: rare earth europium complex [Eu 2 m 1 (M 2 ) 2 Preparation of R]
[0032] A. the oxide of rare earth metal europium is dissolved in HCl, and the mol ratio with the oxide of rare earth europium and hydrochloric acid is 1: 15, and dissolution temperature is 40 ℃, and the time is 20 minutes, makes europium trichloride solution, will It is dried; 6 millimoles of europium trichloride is added to 30 ml of ethanol solution with a concentration of 99.7% by weight to form solution 1;
[0033] B. Dissolving 6 mmoles of chemically pure 1,10-phenanthroline in 20 ml of ethanol solution with a concentration of 99.7% by weight to obtain solution 2;
[0034] C. Add 3 mmol of ligand M 1 Mix with solvent dimethyl sulfoxide 40ml of 99.7% ligand by weight, and stir for 15 minutes until the ligand M 1 Completely dissolved, and with alkaline solution ammonia, the P H The value was adjusted to 7 to obtain solution 3.
[0035] D. Mix 30ml of solution 1 and 20ml of solutio...
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