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Rapid preparation method of MOF material

A fast, time-controlled technology, applied in chemical instruments and methods, other chemical processes, physical/chemical process catalysts, etc., can solve the problems of uncontrollable particle size, slow reaction process, incomplete crystal growth, etc., and achieve uniform particle size. , The effect of easy product and high industrial application value

Active Publication Date: 2020-06-02
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a rapid large-scale preparation method of MOF materials with convenient operation and fast response (<5min), so as to overcome the slow reaction process and crystallization in the traditional MOF material preparation methods. Disadvantages such as incomplete growth and uncontrollable particle size

Method used

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  • Rapid preparation method of MOF material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The MOF material Cu(H 2 oba):

[0039] In step (1), 100 mg of copper acetate was dissolved in 2 mL of water to obtain an aqueous solution of copper acetate, and 258 mg of 4,4'-diphenyl ether dicarboxylic acid was dissolved in 1.5 mL of N,N-dimethylformamide (DMF) to obtain an organic DMF solution of ligand;

[0040] In step (2), the DMF solution of the organic ligand obtained in step (1) is dropped into the copper acetate aqueous solution at 30°C, and the time of dropping is controlled at about 50s to obtain a suspension of the crude product of the MOF material;

[0041] In step (3), the suspension of the MOF material crude product obtained in step (2) is centrifuged, and the precipitate obtained by centrifugation is cleaned with DMF and methanol respectively, which is the MOF material Cu(H 2 oba).

Embodiment 2

[0043] The MOF material Zn(H) was prepared by the following steps 2 oba):

[0044] In step (1), 87.6 mg of zinc acetate was dissolved in 2 mL of water to obtain an aqueous solution of zinc acetate, and 258 mg of 4,4'-diphenyl ether dicarboxylic acid was dissolved in 1.5 mL of N,N-dimethylformamide (DMF) to obtain DMF solution of organic ligand;

[0045] In step (2), the DMF solution of the organic ligand obtained in step (1) is dropped into the zinc acetate aqueous solution at 30° C., and the time of dropping is controlled at 20 to 30 s to obtain a suspension of the crude product of the MOF material;

[0046] In step (3), the suspension of the MOF material crude product obtained in step (2) is centrifuged, and the precipitate obtained by centrifugation is cleaned with DMF and methanol respectively, which is the MOF material Zn(H 2 oba).

Embodiment 3

[0048] The MOF material Cd(H) was prepared by the following steps 2 oba):

[0049] In step (1), 133mg of cadmium acetate was dissolved in 1mL of water to obtain an aqueous solution of cadmium acetate, and 258mg of 4,4'-diphenyl ether dicarboxylic acid was dissolved in 1.5mL of N,N-dimethylformamide (DMF) to obtain an organic DMF solution of ligand;

[0050] In step (2), the DMF solution of the organic ligand obtained in step (1) is dropped dropwise into the cadmium acetate aqueous solution at 35°C, and the time of dropping is controlled at 20-30s to obtain a suspension of the crude product of the MOF material ;

[0051] In step (3), the suspension of the MOF material crude product obtained in step (2) is centrifuged, and the precipitate obtained by centrifugation is cleaned with DMF and methanol respectively, which is the MOF material Cd(H 2 oba).

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Abstract

The invention provides a rapid preparation method of an MOF material. The method comprises the following steps: at 25-35 DEG C, adding an organic ligand solution into a metal acetate aqueous solutionin a dropwise manner to obtain the MOF material. According to the invention, an organic ligand solution is added into a metal acetate aqueous solution at room temperature in a dropwise manner to obtain a MOF material, so that the method can overcome the technical prejudice that long-time solvothermal reaction needs to be carried out at high temperature in preparation of a MOF material in the field, the MOF material with complete crystal growth and controllable particle size can be rapidly prepared within 1 minute, the preparation reaction can be continuously carried out, the product is easy toseparate, and the method has higher potential industrial application value.

Description

technical field [0001] The invention relates to the field of organic-inorganic composite materials, in particular to a rapid preparation method of MOF materials. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, referred to as MOF), is a porous crystal material formed by the self-assembly of transition metal ions and organic ligands through coordination bonds, which has more unsaturated metal active sites, higher With the advantages of large specific surface area and high thermal stability, it can be prepared in various fields such as gas separation, gas storage, chemical catalysis, chemical sensing or drug release. [0003] MOF materials are usually prepared by solvothermal or hydrothermal methods. When the above methods are used to prepare MOF materials, the reaction process usually takes hours or days to obtain MOF materials of a certain scale. In addition, the crystal structure of the product obtained by the above synthesis method is not ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J31/28B01J31/26B01J31/32
CPCB01J20/22B01J31/28B01J31/26B01J31/32
Inventor 唐智勇李国栋司马锐夕邱雪英
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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