Complexes of rare earth-beta-diketone-naphthisodiazine and synthetic method
The technology of a phenanthroline and a synthesis method is applied in the field of metal rare earth-β-diketone complexes and their synthesis, and can solve the problems of low yield and the like, and achieve the effects of high yield, easy industrial production and simple operation.
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Embodiment 1
[0015] Synthesis of rare earth gadolinium-β-diketone-phenanthroline complexes:
[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 was 100 ° C, nearly dry, after cooling, the product gadolinium chloride GdCl 3 Dissolved in 20ml of double distilled water to obtain the inorganic salt gadolinium chloride GdCl 3 aqueous solution;
[0018] Dissolve 1.35g (0.006mol) of 1,3-diphenyl-1,3-propanedione and 0.36g (0.002mol) of 1,10-phenanthroline in 40ml of 80% ethanol aqueous solution, adjust the solution with NaOH The PH is 4-8, the reaction is slowly dripped with GdCl under stirring 3 the aqueous solution, control the reaction temperature between 40-90 ℃, continue to stir for 1-10 hours, and fully react. Then the reaction solution was allowed to stand, cooled to room temperature, and the cooled reaction solution was suctio...
Embodiment 2
[0025] Synthesis of Rare Earth Lanthanum-β-diketone-Phenanthrene Complexes:
[0026] Specific synthesis steps as in Example 1:
[0027] 0.33g (0.001mol) of rare earth oxide lanthanum trioxide La 2 O 3 Dissolved in 10ml of 38% concentrated hydrochloric acid, slowly heated in a water bath to near dryness, after cooling, the product lanthanum chloride LaCl 3 Dissolved in 20ml of secondary distilled water to obtain the inorganic salt lanthanum chloride LaCl 3 aqueous solution;
[0028] Dissolve 1.35g (0.006mol) of 1,3-diphenyl-1,3-propanedione and 0.36g (0.002mol) of 1,10-phenanthroline in 40ml of 80% ethanol aqueous solution, adjust the solution with NaOH The PH is 4-8, the reaction is added LaCl under stirring 3 the aqueous solution, control the reaction temperature between 40-90 ℃, continue to stir for 1-10 hours, and fully react. Then the reaction solution was allowed to stand, cooled to room temperature, and the cooled reaction solution was suction filtered to obtain a ...
Embodiment 3
[0037] Synthesis of rare earth samarium-β-diketone-phenanthroline complexes:
[0038] Specific synthesis steps as in Example 1:
[0039] 0.35g (0.001mol) rare earth oxide samarium trioxide Sm 2 O 3 Dissolved in 10ml of 38% concentrated hydrochloric acid, slowly heated in a water bath to near dryness, after cooling, the product samarium chloride SmCl 3 Dissolved in 20ml of secondary distilled water to obtain the inorganic salt samarium chloride SmCl 3 aqueous solution;
[0040] Dissolve 1.35g (0.006mol) of 1,3-diphenyl-1,3-propanedione and 0.36g (0.002mol) of 1,10-phenanthroline in 40ml of 80% ethanol aqueous solution, adjust the solution with NaOH The PH is 4-8, the reaction is added SmCl under stirring 3the aqueous solution, control the reaction temperature between 40-90 ℃, continue to stir for 1-10 hours, and fully react. Then the reaction solution was allowed to stand, cooled to room temperature, and the cooled reaction solution was suction filtered to obtain a crude ...
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