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Ligand amination metal-organic framework-supported catalyst and its preparation method and application

A metal-organic framework and supported catalyst technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve active component leakage and uneven distribution , low loading of active components, etc., to achieve the effect of promoting uniform distribution, broadening the scope of application, and good industrial application potential

Active Publication Date: 2017-09-29
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a ligand-aminated metal-organic framework-supported catalyst for catalytic oxidation reactions and its preparation method and application. Inhomogeneity and excessive leakage of active components and other problems, the prepared catalytic material has high oxidation reaction activity and stability, expanding the scope of application of the reaction

Method used

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  • Ligand amination metal-organic framework-supported catalyst and its preparation method and application
  • Ligand amination metal-organic framework-supported catalyst and its preparation method and application
  • Ligand amination metal-organic framework-supported catalyst and its preparation method and application

Examples

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Effect test

Embodiment 1

[0025] (1) Ligand amination metal organic framework material NH 2 - Preparation of MIL-101(Al):

[0026] First, 0.5100g AlCl 3 ·6H 2 O, 0.56g 2-NH 2 -BDC was completely dissolved in 25mL of DMF, and the mixture was placed in a hydrothermal kettle and kept at 130°C for 3 days, after which the reaction liquid was centrifuged, and the centrifuged solid was washed with acetonitrile and activated with methanol, and finally heated at 80°C Vacuum drying for 12 hours, the ligand aminated metal-organic framework material NH 2 - MIL-101(Al) 0.5 g.

[0027] (2) Metal nickel-carbon oxide nanoparticles loaded with NH 2 - Preparation of MIL-101 (Al) (organic acid is oxalic acid OA):

[0028]NH after vacuum drying 2 -MIL-101(Al)(0.1g) was placed in 25mL OA and Ni(NO 3 ) 2 ·6H 2 In the mixed aqueous solution of O, soak at 80°C for 20h. The nickel ion concentration in the mixed aqueous solution is 7.14mmol / L, and the oxalic acid concentration is 21.42mmol / L. ℃ in a vacuum oven for 1...

Embodiment 2

[0031] (1) Ligand amination metal organic framework material NH 2 - Preparation of MIL-53(Al):

[0032] First, 0.1136g AlCl 3 ·6H 2 O, 0.5592g 2-NH 2 -BDC was completely dissolved in 16mL of DMF, and the mixture was placed in a hydrothermal kettle and kept at 150°C for 3 days. Reflux at ℃ for 8h, finally centrifuge, wash with DMF, and dry in vacuum at 150℃ for 12h to prepare the ligand-aminated metal-organic framework NH 2 - MIL-53(Al) 0.4 g.

[0033] (2) Metal nickel-carbon oxide nanoparticles loaded with NH 2 - Preparation of MIL-53 (Al) (organic acid is oxalic acid OA):

[0034] NH after vacuum drying 2 -MIL-53(Al)(0.1g) in 25mL OA and Ni(NO 3 ) 2 ·6H 2 In the mixed aqueous solution of O, soak at 80°C for 20h. The nickel ion concentration in the mixed aqueous solution is 7.14mmol / L, and the oxalic acid concentration is 21.42mmol / L. ℃ in a vacuum oven for 12 hours to obtain a metal-organic framework material Ni loaded with nickel ions and oxalic acid 2+ -OA-NH 2...

Embodiment 3

[0037] Metal nickel-cobalt-carbide nanoparticles loaded NH 2 - Preparation of MIL-101 (Al) (organic acid is oxalic acid OA):

[0038] NH after vacuum drying 2 -MIL-101(Al)(0.1g) was placed in 25mL OA and Ni(NO 3 ) 2 ·6H 2 O and Co(NO 3 ) 2 ·6H 2 In the mixed aqueous solution of O, immersed at 80°C for 20h, the nickel ion concentration in the mixed aqueous solution was 1.19mmol / L, the cobalt ion concentration was 5.95mmol / L, and the oxalic acid concentration was 21.42mmol / L. After impregnation, the mixture was centrifuged, washed with pure water, and dried in a vacuum oven at 60°C for 12 hours to obtain a metal-organic framework material Ni loaded with nickel-cobalt ions and oxalic acid. 2+ -Co 2+ -OA-NH 2 -MIL-101(Al), which was calcined at 200°C for 6h to obtain metallic nickel-cobalt-carbon oxide nanoparticles loaded NH 2 -MIL-101(Al) catalyst (Ni 2+ -Co 2+ -OA / NH 2 -MIL-101(Al)) 0.14g.

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Abstract

The present invention provides a ligand-aminated metal-organic framework-supported catalyst, which is prepared by the following method: AlCl3 6H2O and 2-NH2-BDC are added to N,N-dimethylformamide, and then Put the obtained mixed solution in a reaction kettle and react at 130-150°C for 24-72 hours, and then the reaction solution is post-treated to obtain a ligand-aminated metal-organic framework material; adding transition metal salts and organic acids to water to obtain impregnated Solution: Immerse the ligand-aminated metal-organic framework material in the impregnation solution, and immerse it at 40-90°C for 10-36 hours, then centrifuge the reaction solution, wash the solid obtained by centrifugation, and dry it in vacuum, and finally place it in a muffle furnace , calcined at 100-300° C. for 2-6 hours to obtain the catalyst; the catalyst of the invention can be applied to catalytic oxidation reactions, and has the characteristics of wide application range, high catalytic efficiency and good stability.

Description

(1) Technical field [0001] The invention relates to a ligand-aminated metal-organic framework-supported catalyst and its preparation method and application, in particular to a ligand-aminated Al-based metal-organic framework-supported metal-carbon oxide heterogeneous catalyst and its preparation method , and its application in catalytic oxidation reactions. (2) Background technology [0002] At present, hydrogen peroxide catalytic oxidation technology has been widely used in petrochemical, pharmaceutical, environmental protection, agriculture and other fields. However, the development of high-performance supported catalysts has become the key to accelerating catalytic oxidation reactions. In recent years, metal-organic framework materials are porous materials that have developed rapidly and received extensive attention in recent years. Compared with traditional porous materials, this porous material composed of organic ligands and inorganic metals has the following remarkab...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28A62D3/38A62D101/04A62D101/20
Inventor 张国亮秦磊李赵炆
Owner ZHEJIANG UNIV OF TECH