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

Active Publication Date: 2016-07-27
河南索顿新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, aromatic carboxylic acid ligands and β-diketone ligands have their own advantages and disadvantages. The rare earth complexes formed by aromatic carboxylic acids have high thermal stability, but are not easy to sublimate; while β-diketone ligands are easy to sublimate. , but the thermal stability is relatively low

Method used

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  • Novel rare earth europium complex and preparation method thereof
  • Novel rare earth europium complex and preparation method thereof
  • Novel rare earth europium complex and preparation method thereof

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preparation example Construction

[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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Abstract

The invention discloses a novel rare earth europium complex and a preparation method thereof. The method includes the following steps of firstly, conducting acylation reaction with acetophenone and benzenedicarboxylic acid dimethyl ester as the raw materials to obtain beta-diketone ligand; secondly, using beta-diketone ligand obtained in the first step as the first ligand and phenanthroline as the second ligand to obtain the rare earth europium complex. The preparation method is easy to operate and implement, and the prepared novel rare earth europium complex is novel in structure, has high heat stability and meanwhile has the advantages of being high in fluorescent strength, long in fluorescent service life and the like.

Description

technical field [0001] The invention belongs to the field of rare earth complexes, in particular to a novel rare earth europium complex, in particular to a preparation method of the rare earth europium complex. Background technique [0002] Rare earth complexes have the advantages of high luminous intensity, low excitation energy required by organic substances, high fluorescence efficiency, and good solubility in organic solvents. Therefore, they are used in more and more fields and aspects. At the same time, it also has potential application value in a series of aspects such as optical fiber communication, fluorescence immunity, and rare earth analysis of anti-tumor activity. Synthesizing a new type of organic ligand and coordinating with rare earth ions to form rare earth complexes is a method to effectively improve the luminous efficiency of rare earth complexes. Generally, there are two types of organic ligands that can form complexes with rare earth ions, one is aromat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C09K11/06
CPCC07F5/003C09K11/06C09K2211/182
Inventor 陶栋梁金凤李世刚张开银
Owner 河南索顿新材料有限公司
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