Chiral mononuclear nine-coordinated beta-diketone complex and preparation method thereof

A technology of diketones and complexes, applied in the field of chiral mononuclear nine-coordinated neodymium complexes and their preparation, can solve the problems of unpublished articles, publications, and no patents, and achieve the reduction of non-radiative transitions, simple process, and high production efficiency. high rate effect

Inactive Publication Date: 2015-01-07
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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Problems solved by technology

At present, only one case of mononuclear eight-coordinated chiral Nd β-diketone complex has been reported, and the

Method used

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  • Chiral mononuclear nine-coordinated beta-diketone complex and preparation method thereof
  • Chiral mononuclear nine-coordinated beta-diketone complex and preparation method thereof
  • Chiral mononuclear nine-coordinated beta-diketone complex and preparation method thereof

Examples

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Example Embodiment

[0025] Example 1

[0026] A preparation method of a chiral mononuclear nine-coordinate neodymium β-diketone complex, the steps are as follows:

[0027] (1) Intermediate Nd(tta) as raw material for reaction 3 ·2H 2 Preparation of O: Dissolve 2.2 g of 1-thiophenetrifluoromethyl 1,3-butanedione (manufactured by Alfa Reagent Company) in 25 mL of absolute ethanol and stir for 20 minutes to form a clear solution. Then add 10 mL of 1 M ammonia water, under slow stirring, add 20 mL dropwise to dissolve 1.1 g of NdCl 3 ·6H 2 Aqueous solution of O was allowed to stand overnight, and a colorless precipitate formed. After filtration, the precipitate was washed three times with a small amount of water and dried in vacuum to obtain a white product with a yield of about 86% (calculated by Nd). Elemental analysis: according to molecular formula C 24 H 16 O 8 F 9 S 3 Nd: calculated value (%) C 34.16, H 1.91; measured value (%) C 34.21, H 1.85. Infrared spectrum IR (KBr, cm -1 ): 1609(s), 1538(m), ...

Example Embodiment

[0034] Example 2

[0035] Chiral mononuclear nine-coordinate neodymium β-diketone complex Nd(tta) as a near-infrared luminescent material 3 Preparation method of L:

[0036] (1) Intermediate Nd(tta) as raw material for reaction 3 ·2H 2 Preparation of O: Dissolve 2.2 g of 1-thiophenetrifluoromethyl 1,3-butanedione (tta, produced by Alfa Reagent Company) in 30 mL of absolute ethanol and stir for 20 minutes to form a clear solution. Then add 7 mL of 1 M ammonia. Under slow stirring, add 20 mL dropwise to dissolve 1.1 g NdCl 3 ·6H 2 O aqueous solution, let stand overnight, a colorless precipitate is formed. After filtration, the precipitate is washed three times with a small amount of water and dried in vacuum to obtain a white product;

[0037] (2) Chiral mononuclear nine-coordinate neodymium β-diketone complex Nd(tta) 3 Preparation of L: add 15 mL Nd(tta) 3 ·2H 2 A solution of O (225 mg, 0.2 mmol) in acetonitrile was added with a tridentate nitrogen-containing chiral chelating organic...

Example Embodiment

[0040] Example 3

[0041] A preparation method of a chiral mononuclear nine-coordinate neodymium β-diketone complex, the steps are as follows:

[0042] (1) Intermediate Nd(tta) as raw material for reaction 3 ·2H 2 Preparation of O: Dissolve 7.5 mmol 1-thiophene trifluoromethyl 1,3-butanedione in 25 mL of absolute ethanol and stir for 24 minutes to obtain 1-thiophene trifluoromethyl 1,3 with a concentration of 0.3 mol / L -Butanedione ethanol solution, then add 7mL ammonia water, under slow stirring, add dropwise NdCl with a concentration of 0.12 mol / L 3 ·6H 2 20mL of O aqueous solution, precipitation immediately formed. After filtration, the precipitate was washed with water and dried in vacuum to obtain a white product called Nd(tta) 3 ·2H 2 O.

[0043] (2) Chiral mononuclear nine-coordinate neodymium β-diketone complex Nd(tta) 3 Preparation of L: Nd(tta) with a concentration of 0.02mol / L 3 ·2H 2 Add 10 mL of O acetonitrile solution to 5 mL of 0.02mol / L tridentate nitrogen-containing ...

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Abstract

The invention discloses a chiral mononuclear nine-coordinated beta-diketone complex which has a molecular formula of Nd(tta)3L, wherein L is [(-)-2,6-bis(4,5-pinene-2-pyridyl)pyridine]; tta is a 1-thiophene trifluoromethyl1,3-butanedione anion. The preparation method of the chiral mononuclear nine-coordinated beta-diketone complex comprises the following steps: dissolving the 1-thiophene trifluoromethyl1,3-butanedione in absolute ethyl alcohol, adding ammonium hydroxide and a NdCl3.6H2O aqueous solution to generate precipitates, filtering, washing and drying to obtain Nd(tta)3.2H2O, adding an acetonitrile solution of the Nd(tta)3.2H2O into an acetone solution in which a trident nitrogenous chiral chelation organism L, stirring and filtering to obtain pink crystals after 3 days, and filtering, washing and drying to obtain the target product. As the preparation process is simple and the reaction is carried out at a normal temperature, the complex has favorable near-infrared luminescence property and is expected to serve as a near-infrared luminescence material which has wide application prospect in the aspects of lasers and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic-organic hybrid rare earth functional materials and their preparation and application, and in particular relates to a chiral mononuclear nine-coordination neodymium complex with near-infrared luminescent properties and a preparation method thereof. Background technique [0002] Due to the special configuration of the f electron shell of rare earth neodymium ions, the complexes of neodymium have characteristic near-infrared luminescence properties. The characteristic near-infrared luminescence wavelengths are 890, 1060 and 1130 nm. Optical amplifiers and network communications have broad application prospects. However, the molar absorption coefficient of neodymium ion itself is very low, and its absorption ability to ultraviolet and visible light is weak. Therefore, to prepare neodymium complexes with excellent near-infrared luminescent properties, organic chromophores with strong absorption abili...

Claims

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Application Information

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IPC IPC(8): C07F5/00C09K11/06C07D401/14
CPCC07F5/003C09K11/06C09K2211/1029C09K2211/1092
Inventor 方少明李郤里靳淸贤王爱玲杜俊平周利明
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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