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Nitrogenous carboxylic acid transition metal macropore complex, preparation method and application thereof

A technology of transition metal and nitrogen carboxylic acid, which is applied in the field of fluorescent materials, and achieves the effect of simple preparation method

Inactive Publication Date: 2019-06-14
YANAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no organic ligand (2-(pyrid-4`-yl)-benzimidazole-5-carboxylic acid, that is, 2-(4-pyridyl)benzimidazole-5-carboxylic acid) with transition metals (Zn and Cd ) Synthetic complexes

Method used

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  • Nitrogenous carboxylic acid transition metal macropore complex, preparation method and application thereof
  • Nitrogenous carboxylic acid transition metal macropore complex, preparation method and application thereof
  • Nitrogenous carboxylic acid transition metal macropore complex, preparation method and application thereof

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preparation example Construction

[0030] The preparation method of the nitrogen-containing carboxylic acid transition metal macroporous complex of the present invention, the specific operation process comprises the following steps:

[0031] Step 1, add 2-(4-pyridyl)benzimidazole-5-carboxylic acid, metal salt solution and auxiliary ligands into a small glass bottle in sequence according to a certain proportion, add dimethyl sulfoxide, N,N- Add dimethylformamide into the above-mentioned small glass bottle sequentially according to a certain proportion, stir at room temperature, add tetrafluoroboric acid during the stirring process until the solution becomes clear to obtain a mixed solution A;

[0032] In step 1, the metal salt is any one of cadmium nitrate, cadmium acetate, zinc nitrate, zinc acetate or zinc chloride;

[0033] In step 1, the auxiliary ligand is 1,10'-phenanthroline;

[0034] The molar ratio between 2-(4-pyridyl)benzimidazole-5-carboxylic acid, metal salt solution and auxiliary ligand in step 1 ...

Embodiment 1

[0038] Add 0.2mmol of 2-(4-pyridyl)benzimidazole-5-carboxylic acid, 0.1mmol of cadmium nitrate and 0.2mmol of 1,10'-phenanthroline into the small glass bottle successively, and then add 5ml of Add N,N-dimethylformamide and 1ml dimethyl sulfoxide into the above-mentioned small glass bottle in turn, stir at room temperature, add tetrafluoroboric acid appropriately during the stirring process until the solution becomes clear, and let it stand at 90°C React in a constant temperature box for about a week, until a colorless massive crystal substance is found to be produced, cool to room temperature, filter, wash and dry to obtain a synthetic nitrogen-containing carboxylic acid transition metal cadmium pore complex material, and the calculated yield is 57%.

[0039] The structure of the prepared nitrogen-containing benzimidazole carboxylate cadmium fluorescent probe material is as follows: figure 1 As shown, after physical characterization tests, it is concluded that the structure o...

Embodiment 2

[0045] Add 0.4mmol of 2-(4-pyridyl)benzimidazole-5-carboxylic acid, 0.2mmol of cadmium acetate and 0.4mmol of 1,10'-phenanthroline into the small glass bottle successively, and then add 10ml of Add N,N-dimethylformamide and 2ml dimethyl sulfoxide into the above-mentioned small glass bottle in turn, stir at room temperature, add tetrafluoroboric acid appropriately during the stirring process until the solution becomes clear, and let it stand at 80°C React in a constant temperature box for about a week, until a colorless massive crystalline substance is found to be produced, cool to room temperature, filter, wash and dry to obtain a synthetic nitrogen-containing carboxylic acid transition metal cadmium pore complex material, and the calculated yield is 60%.

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Abstract

The invention discloses a nitrogenous carboxylic acid transition metal complex material with a three-dimensional macropore structure and a chemical formula of M(PBCA)2, wherein M=Cd or Zn, PBCA=2-(4-pyridyl) benzimidazole-5-carboxylic acid. The invention also discloses a preparation method of the complex. The preparation method comprises the following steps: successively adding 2-(4-pyridyl) benzimidazole-5-carboxylic acid, metal salt solution, auxiliary ligand, dimethyl sulfoxide and N,N-dimethyl formamide into a small glass bottle; stirring under room temperature; adding a certain amount oftetrafluoroboric acid while stirring till the solution becomes clear; standing by and reacting in an incubator till generating colorless massive crystal, and then cooling to room temperature; filtering and washing repeatedly, and drying, thereby acquiring the nitrogenous carboxylic acid transition metal macropore complex. The complex provided by the invention has strong luminescent property and can be used as an excellent fluorescence probe material. The preparation method disclosed by the invention is simple in operation and is suitable for extensive popularization and application.

Description

technical field [0001] The invention belongs to the technical field of fluorescent materials, and in particular relates to a nitrogen-containing carboxylic acid transition metal macroporous complex, a preparation method of the complex, and an application of the complex. Background technique [0002] Due to their unique pore structure, metal-organic framework complex functional materials determine their potential applications in gas storage and separation, photocatalysis, ion exchange, molecular recognition, substance adsorption, and fluorescent probe materials. In recent years, metal-organic framework complexes have become a research hotspot for researchers. In the research on the synthesis of metal-organic framework complexes, the research on the use of carboxylic acids and nitrogen-containing organic ligands to construct functional materials of metal-organic framework complexes has been relatively mature. However, there are relatively few studies on organic ligands contai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/08C07F3/06C09K11/06
Inventor 王潇韩友侯向阳
Owner YANAN UNIV
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