Novel rare earth europium complex and preparation method thereof
A europium complex and rare earth technology, applied in the field of rare earth complexes, can solve the problems of difficult sublimation and low thermal stability, and achieve the effects of easy realization, simple operation and high fluorescence intensity
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[0041] According to one aspect of the present invention, a kind of preparation method of rare earth europium complex is provided, and the method comprises the following steps:
[0042] Step 1. Synthesis of β-diketone ligands: acetophenone and dimethyl terephthalate are used as raw materials for acylation reaction to obtain β-diketone ligands;
[0043] Step 2. Preparation of rare earth europium complex: the β-diketone ligand obtained in step 1 is used as the first ligand, and o-phenanthroline is used as the second ligand to prepare the rare earth europium complex.
[0044] Wherein, the reaction process of the step 1 is carried out as follows, (1) is a β-diketone ligand, (2) is a by-product, and the β-diketone ligand is also called methyl terephthalate Benzoylmethane.
[0045]
[0046] Step 1 includes the following sub-steps:
[0047] Step 1.1, adding dimethyl terephthalate into an organic solvent, adding sodium methoxide into methanol, and then mixing the above solutions t...
Embodiment 1
[0086] The synthesis of embodiment 1β-diketone ligand
[0087] Dissolve 9.7 g of dimethyl terephthalate in 100 mL of THF. Dissolve 2.7g of sodium methoxide solid in 6.4g of methanol to prepare a 30% sodium methoxide solution. The two were added together in a 500mL single-necked flask.
[0088] Dissolve 3.96g of acetophenone solid in 25mLTHF, and control the temperature of the oil bath at 75°C. After the liquid in the flask starts to boil, add the acetophenone solution into the flask. The reaction process is carried out under anhydrous conditions. For reflux, add a drying tube above, and the drying tube is filled with anhydrous CaCl 2 , the reaction time is 6 hours. Then keep it warm at 65°C for 4 hours, and it can be seen that the solution gradually changes from the original milky white to yellowish brown. After incubation, the solution turned dark yellow-brown. At this time, the flask was removed from the oil bath and placed in an ice-water bath at 5° C., and continued t...
Embodiment 2
[0090] The synthesis of embodiment 2β-diketone ligands
[0091] Dissolve 9.7 g of dimethyl terephthalate in 100 mL of THF. Dissolve 2.7g of sodium methoxide solid in 10.8g of methanol to prepare a 20% sodium methoxide solution. The two were added together in a 500mL single-necked flask.
[0092] Dissolve 1.2 g of acetophenone solid in 15 mL of THF, control the temperature of the oil bath at 70° C., and add the acetophenone solution into the flask after the liquid in the flask starts to boil. The reaction process is carried out under anhydrous conditions, and the condenser is used for reflux, and a drying tube is added above, and anhydrous CaCl is installed in the drying tube. 2 , the reaction time is 4 hours. Then keep it warm at 50°C for 2 hours, and it can be seen that the solution gradually changes from the original milky white to yellowish brown. After incubation, the solution turned dark yellow-brown. At this time, the flask was removed from the oil bath and placed i...
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