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Complexes of rare earth-beta-diketone-naphthisodiazine and synthetic method

A technology of phenanthroline and synthesis method, which is applied in the field of metal rare earth-β-diketone complexes and their synthesis, can solve the problems of low yield, and achieve the effects of high yield, simple operation, and high thermal decomposition temperature

Inactive Publication Date: 2005-10-26
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the synthesis of the above-mentioned novel rare earth-β-diketone-organic base ternary complexes with good light, thermal stability, spectroscopic properties and solubility properties, these common synthetic methods have low yields (

Method used

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  • Complexes of rare earth-beta-diketone-naphthisodiazine and synthetic method
  • Complexes of rare earth-beta-diketone-naphthisodiazine and synthetic method
  • Complexes of rare earth-beta-diketone-naphthisodiazine and synthetic method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Synthesis of rare earth gadolinium-β-diketone-phenanthroline complex:

[0016]

[0017] 0.36g (0.001mol) rare earth oxide gadolinium trioxide Gd 2 O 3 Dissolved in 10ml of 38% concentrated hydrochloric acid, slowly heated in a water bath for 60 minutes, the reaction temperature is 100℃, nearly dry, after cooling, the product gadolinium chloride GdCl 3 Dissolve in 20ml of double distilled water to obtain the inorganic salt of gadolinium chloride GdCl 3 Aqueous solution

[0018] Dissolve 1.35g (0.006mol) 1,3-diphenyl-1,3-propanedione and 0.36g (0.002mol) 1,10-phenanthroline in 40ml 80% ethanol aqueous solution, and adjust the solution with NaOH The PH is 4-8, and the reaction is slowly dripped with GdCl under stirring 3 Control the reaction temperature between 40-90℃, and continue to stir for 1-10 hours to fully react. Then, the reaction solution is allowed to stand, cooled to room temperature, and the cooled reaction solution is suction filtered to obtain a crude product. ...

Embodiment 2

[0024] Synthesis of rare earth lanthanum-β-diketone-phenanthroline complexes:

[0025] The specific synthesis steps as in Example 1:

[0026] 0.33g (0.001mol) rare earth oxide lanthanum trioxide La 2 O 3 Dissolved in

[0027] In 10m138% concentrated hydrochloric acid, the water bath is slowly heated to nearly dry, and after cooling, the product lanthanum chloride LaCl 3 Dissolve in 20ml twice distilled water to prepare inorganic salt lanthanum chloride LaCl 3 Aqueous solution

[0028] Dissolve 1.35g (0.006mol) 1,3-diphenyl-1,3-propanedione and 0.36g (0.002mol) 1,10-phenanthroline in 40ml 80% ethanol aqueous solution, and adjust the solution with NaOH PH is 4-8, add LaCl under stirring 3 Control the reaction temperature between 40-90℃, and continue to stir for 1-10 hours to fully react. Then, the reaction solution is allowed to stand, cooled to room temperature, and the cooled reaction solution is suction filtered to obtain a crude product. Wash the crude product with a small amoun...

Embodiment 3

[0036] Synthesis of rare earth samarium-β-diketone-phenanthroline complexes:

[0037] The specific synthesis steps as in Example 1:

[0038] 0.35g (0.001mol) rare earth oxide samarium trioxide Sm 2 O 3 Dissolve in 10ml of 38% concentrated hydrochloric acid, slowly heat the water bath to nearly dry, after cooling, the product samarium chloride SmCl 3 Dissolve in 20ml of double distilled water to prepare the inorganic salt of samarium chloride SmCl 3 Aqueous solution

[0039] Dissolve 1.35g (0.006mol) 1,3-diphenyl-1,3-propanedione and 0.36g (0.002mol) 1,10-phenanthroline in 40ml 80% ethanol aqueous solution, and adjust the solution with NaOH PH is 4-8, add SmCl under stirring 3 Control the reaction temperature between 40-90℃, and continue to stir for 1-10 hours to fully react. Then, the reaction solution is allowed to stand, cooled to room temperature, and the cooled reaction solution is suction filtered to obtain a crude product. Wash the crude product with a small amount of ethano...

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Abstract

The rare earth-beta-diketone-naphthisodiazine complex and its synthess emthod relates to chemical product and preparation technology. Said invention also provides its structure general formula, and its synthesis method includes the following steps: dissolving rare earth oxide in organic acid, using secondary distilled water to dissolve product to obtain rare earth inorganic salt aqueous solution; dissolving 1,3-diphenyl-1,3-propanedione and 1,10-naphthisodiazine in ethyl alcohol aqueous solution, adding rare earth inorganic salt aqueous solution, constant temperature stirring, standing still, filtering, washing out solvent, high-temp, vacuum drying so as to obtain rare earth-beta-diketone-naphthisodiazine. Said complex has good resolubility, optical property and optical and thermal stability.

Description

Technical field [0001] The present invention relates to a novel rare earth-β-diketone-phenanthroline complex and its synthesis method, in particular to 1,3-diphenyl-1,3-propanedione and 1,10-dione A metal rare earth-β-diketone complex with azaphenanthrene as a binary ligand and a synthesis method thereof. Background technique [0002] Rare earth-β-diketone complexes are an important inorganic functional material. Due to the strong ultraviolet absorption of the β-diketone organic ligands and the effective energy transfer of the ligands to the rare earth ions that are not filled with 4f electrons, this type of The complex has unique physical and chemical properties, and has a wide range of applications in the fields of organic thin film photoluminescence and electroluminescence, optical fiber sensors, light-emitting diodes, polymer fluorescence, immunofluorescence analysis, chemical analysis, biochemistry, catalysis and other fields. Especially when β-diketones (such as 2-thenoyl t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/00
Inventor 马东哲吴谊群左霞
Owner HEILONGJIANG UNIV
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