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Copper-based metal-organic framework-based crystalline catalyst for catalytically converting carbon dioxide to prepare carbonate, and preparation method and application thereof

A carbon dioxide and organic framework technology, applied in the field of coordination porous materials, copper-based metal-organic framework-based crystalline catalysts, and the preparation field, can solve the problems of poor catalyst stability, low activity, and variable structure, and achieve good selectivity and yield. The effect of high efficiency, simple preparation method and large specific surface area

Inactive Publication Date: 2019-02-01
SHANGHAI INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The present invention is based on the 5-(1H-1,2,4-triazol-1-yl) isophthalic acid ligand and the cheap and easy-to-obtain Cu(II) salt coordination assembly complex, and realizes the porous coordination compound Controllable assembly, obtained a porous catalytic material with a large specific surface area, effectively solved the uncontrollable assembly process of most MOFs in the prior art, the structure is variable, and the synthesis process is relatively unpredictable. Catalysts prepared by traditional methods have technical problems such as poor stability and low activity

Method used

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  • Copper-based metal-organic framework-based crystalline catalyst for catalytically converting carbon dioxide to prepare carbonate, and preparation method and application thereof
  • Copper-based metal-organic framework-based crystalline catalyst for catalytically converting carbon dioxide to prepare carbonate, and preparation method and application thereof
  • Copper-based metal-organic framework-based crystalline catalyst for catalytically converting carbon dioxide to prepare carbonate, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Synthesis of Cu(II)-based Metal Organic Framework Crystalline Catalysts

[0025] (1) Weighing according to the molar ratio of hydrated copper nitrate and 5-(1H-1,2,4-triazol-1-yl)isophthalic acid at 1:1;

[0026] (2) Mix 5-(1H-1,2,4-triazol-1-yl) isophthalic acid ligand and hydrated copper nitrate, dissolve in a mixture of N,N-dimethylformamide and water Solvent (volume ratio is 1:1), prepared as a precursor solution;

[0027] (3) Transfer the precursor solution into a hydrothermal reaction kettle for solvothermal reaction, the reaction temperature is 100°C, and the reaction time is 12 hours. Finally, suction filtration, washing, and drying are performed to obtain a copper-based metal-organic framework-based crystalline catalyst.

Embodiment 2

[0028] Example 2: Synthesis of Cu(II)-based Metal Organic Framework Crystalline Catalysts

[0029] (1) Weighing according to the mole of copper nitrate hydrate and 5-(1H-1,2,4-triazol-1-yl)isophthalic acid is 2:1;

[0030] (2) Mix 5-(1H-1,2,4-triazol-1-yl) isophthalic acid ligand and hydrated copper nitrate, dissolve in a mixture of N,N-dimethylformamide and water Solvent (volume ratio is 2:1), is prepared as precursor solution;

[0031] (3) Transfer the precursor solution into a hydrothermal reaction kettle for solvothermal reaction, the reaction temperature is 120°C, and the reaction time is 16 hours. Finally, suction filtration, washing, and drying are performed to obtain a copper-based metal-organic framework-based crystalline catalyst.

[0032] In the embodiment, the single crystal structure of the Cu(II)-based crystalline catalyst synthesized in Examples 1-2 of the present invention is as follows figure 1 shown. figure 2 It is a three-dimensional frame structure diag...

Embodiment 3

[0036] Embodiment 3: Catalytic cycloaddition reaction of propylene oxide and carbon dioxide

[0037] In the reaction of the cycloaddition of catalyzed propylene oxide and carbon dioxide, a quantitative amount of propylene oxide (40mmol) and tetrabutylammonium bromide (TBAB, 1.0g) were loaded into the flask, and 10mg of crystalline catalyst was added (Example 1 synthesis). The reaction mixture was in CO 2 Stirring was carried out under atmospheric conditions, and the reaction was maintained at 25° C. for 10 hours. After the reaction, the product was detected by a Bruker AVANCE III 500MHz nuclear magnetic resonance spectrometer. The conversion rate was 98.5%.

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Abstract

The invention discloses a copper-based metal-organic framework-based crystalline catalyst for catalytically converting carbon dioxide to prepare carbonate, and a preparation method and an applicationthereof. The catalyst adopts 5-(1H-1,2,4-triazol-yl)isophthalic acid as a ligand and Cu(II) as a central metal ion. The preparation method comprises the following steps: 1) dissolving copper nitrate hydrate and 5-(1H-1,2,4-triazole-1-yl) isophthalic acid in a mixed solvent of N,N-dimethylformamide and water in order to prepare a precursor solution; and 2) transferring the precursor solution into ahydrothermal reaction vessel, carrying out a solvothermal reaction, and carrying out suction filtration, washing and drying to obtain the copper-based metal-organic framework-based crystalline catalyst. The metal-organic framework-based crystalline material obtained in the invention has high catalytic activity to a cycloaddition reaction of epoxide and CO2, and has a good recycling effect.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and relates to a coordination porous material, in particular to a copper-based metal-organic framework-based crystalline catalyst for catalytic conversion of carbon dioxide to prepare carbonate, a preparation method and an application thereof. Background technique [0002] Metal-organic frameworks (MOFs) are crystalline materials with one-dimensional, two-dimensional or three-dimensional periodic infinite network structures. MOFs materials not only have a novel network topology, but also show great application value in gas adsorption and separation, catalysis, and sensing. Compared with traditional porous materials, MOFs porous materials have the advantages of plastic structure, high porosity, large specific surface area, and uniform pore size distribution. In addition, they are insoluble in most organic solvents, so they have great potential in the application of heterogeneous catalysi...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07D317/36
CPCB01J31/1691B01J2531/0213B01J2531/0241B01J2531/16C07D317/36
Inventor 张建勇邓维谷荣彩史军霞崔鹏辉
Owner SHANGHAI INSTITUTE OF TECHNOLOGY
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