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A chiral mononuclear nine-coordinate neodymium β-diketone complex and its preparation method

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 no patents, no articles, publications, etc., achieve high yield, reduce non-radiative transitions, The effect of simple process

Inactive Publication Date: 2016-08-24
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 there is no article published on mononuclear nine-coordinated chiral Nd β-diketone complex, let alone related patents

Method used

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  • A chiral mononuclear nine-coordinate neodymium β-diketone complex and its preparation method
  • A chiral mononuclear nine-coordinate neodymium β-diketone complex and its preparation method
  • A chiral mononuclear nine-coordinate neodymium β-diketone complex and its preparation method

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Experimental program
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Effect test

Embodiment 1

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

[0027] (1) Intermediate Nd(tta) as a reaction raw material 3 2H 2 Preparation of O: 2.2 g of 1-thiophenetrifluoromethyl 1,3-butanedione (manufactured by Alfa Reagents) was dissolved in 25 mL of absolute ethanol and stirred for 20 minutes to form a clear solution. Subsequently, 10 mL of 1 M ammonia water was added, and under slow stirring, 20 mL of 1.1 g of NdCl was added dropwise. 3 ·6H 2 The aqueous solution of O was allowed to stand overnight, and a colorless precipitate was 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 (%) C 34.16, H 1.91; Found (%) C 34.21, H 1.85. Infrared spectrum IR (KBr, cm -1 ): 1609(s), 153...

Embodiment 2

[0035] Chiral mononuclear nine-coordinated neodymium β-diketone complexes Nd(tta) as near-infrared luminescent materials 3 The preparation method of L:

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

[0037] (2) Chiral mononuclear nine-coordinate neodymium β-diketone complex Nd(tta) 3 Preparation of L: Dissolve 15 mL of Nd(tta) 3 2H 2 O (225 mg, 0.2 mmol) in acetonitrile solution was added dissolved tridentate nitrogen-containing ch...

Embodiment 3

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

[0042] (1) Intermediate Nd(tta) as a reaction raw material 3 2H 2 Preparation of O: 7.5 mmol of 1-thiophenetrifluoromethyl 1,3-butanedione was dissolved in 25 mL of absolute ethanol and stirred for 24 minutes to obtain 1-thiophene trifluoromethyl 1,3 at 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 O aqueous solution 20mL, a precipitate is formed immediately, after filtration, the precipitate is washed with water and dried in vacuum to obtain a white product which is 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 10mL of O acetonitrile solution into 5 mL of tridentate nitrogen-containing chiral ...

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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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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00C09K11/06C07D401/14
CPCC07F5/003C09K11/06C09K2211/1029C09K2211/1092
Inventor 方少明李郤里靳淸贤李凤彩王爱玲杜俊平周立明
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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