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A kind of mesoporous metal-organic framework multi-site catalyst and its preparation method and application

A metal-organic framework and metal-organic technology, applied in organic compound/hydride/coordination complex catalysts, organic chemistry, chemical instruments and methods, etc., can solve high production costs, difficulty in catalyst recovery, high energy consumption of reactions, etc. question

Active Publication Date: 2021-08-17
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] (a) The current research mainly focuses on the reaction using high temperature, high pressure and homogeneous catalysts, the reaction consumes a lot of energy, the catalyst recovery is difficult, and the production cost is high;
[0005] (b) Due to the existence of multiple reaction by-products in the glucose conversion process, the current catalytic process has poor reaction selectivity, which increases the cost of product separation

Method used

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  • A kind of mesoporous metal-organic framework multi-site catalyst and its preparation method and application
  • A kind of mesoporous metal-organic framework multi-site catalyst and its preparation method and application
  • A kind of mesoporous metal-organic framework multi-site catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1, Synthesis of Metal Organic Framework (PCN-222(Co) or PCN-224(Co)).

[0034] Synthesis of PCN-222(Co): Dissolve benzoic acid (1.25 g) and zirconium oxychloride (50 mg) in 10 mLDEF, heat at 100 °C for 1 hour, and phenylcobalt porphyrin carboxylate (50 mg) in the above solution, ultrasonically dissolved, heated at 120 °C for 12 h, and washed with DMF and acetone to obtain 50 mg of purple-red solid. Yield 50%.

[0035] like figure 1 As shown, the scanning electron microscope (SEM) images of the as-prepared samples showed that the microscopic morphology of PCN-222(Co) was rod-like micron-sized crystals. The crystal structure of PCN-222(Co) ( figure 2) was verified by X-ray powder diffraction pattern (PXRD). N2 adsorption data ( image 3 ) shows that PCN-222(Co) is a mesoporous material with a pore size of 3.6 nm.

[0036] Synthesis of PCN-224(Co): Dissolve benzoic acid (1.5 g) and zirconium oxychloride (50 mg) in 10 mL of DMF, heat at 100 °C for 1 hour, and...

Embodiment 2

[0038] Example 2, Synthesis of Metal Organic Framework (PCN-222(Fe) or PCN-224(Fe)).

[0039] Synthesis of PCN-222(Fe): Dissolve benzoic acid (1.25 g) and zirconium oxychloride (50 mg) in 10 mLDEF, heat at 100 °C for 1 hour, and carboxylic acid phenyliron porphyrin (50 mg) in the above solution, ultrasonically dissolved, heated at 120 °C for 12 h, and washed with DMF and acetone to obtain 50 mg of a brown solid. Yield 50%.

[0040] As shown in the figure, the scanning electron microscope (SEM) images of the as-prepared samples showed that the microscopic morphology of PCN-222(Fe) was rod-like micron-scale crystals. The crystal structure of PCN-222(Fe) ( Image 6 ).

[0041] Synthesis of PCN-224(Fe): Dissolve benzoic acid (1.5 g) and zirconium oxychloride (50 mg) in 10 mL of DMF, heat at 100 °C for 1 hour, and carboxylic acid phenyliron porphyrin (25 mg) in the above solution, ultrasonically dissolved, heated at 120 °C for 12 h, and washed with DMF and acetone to obtain 40 ...

Embodiment 3

[0043] Example 3, Synthesis of Metal Organic Framework (PCN-222(Ni) or PCN-224(Ni)).

[0044] Synthesis of PCN-224(Ni): Dissolve benzoic acid (1.5 g) and zirconium oxychloride (50 mg) in 10 mL of DMF, heat at 100 °C for 1 hour, and phenylnickel porphyrin carboxylate (25 mg) in the above solution, ultrasonically dissolved, heated at 120 °C for 12 h, washed with DMF and acetone, and 40 mg of red solid was obtained. Yield 53%.

[0045] As shown in the figure, the scanning electron microscope (SEM) images of the as-prepared samples showed that the microscopic morphology of PCN-224(Ni) was micron-scale cubic crystals. The crystal structure of PCN-224(Ni) ( Figure 8 ).

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Abstract

The invention belongs to the field of porous composite material catalysis, in particular to a mesoporous metal-organic framework multi-center catalyst and its preparation method and application. The present invention uses zirconium oxygen clusters as nodes and tetracarboxylic metal porphyrins as organic chains to construct rod-like (hexagonal) or cubic crystals; the metal-organic framework material is composed of zirconium oxygen clusters and tetracarboxylic metal porphyrins through coordination Formed by self-assembly at a certain temperature; the metal-organic framework material has a large pore size, a high specific surface area, and excellent thermal and chemical stability; through the post-modification method, stannous chloride can be loaded on the zirconium oxygen cluster to A mesoporous metal-organic framework multi-catalytic center catalyst is obtained. The catalyst material can efficiently convert glucose into 2,5-furandicarboxylic acid under photothermal conditions.

Description

technical field [0001] The invention belongs to the technical field of porous composite material catalysis, and in particular relates to a mesoporous metal-organic framework multi-center catalyst, a preparation method thereof and an application in biomass conversion. Background technique [0002] As a non-renewable energy source, fossil fuels are expected to be exploited within 50-100 years, which seriously threatens global energy security. Therefore, finding green and recyclable alternatives to traditional fossil fuels has become the key to solving this problem. Biomass, as the largest recyclable carbon resource on earth, has the potential to solve this problem. Biomass is an important resource composed of organic matter such as cellulose, hemicellulose, and lignin. It has the characteristics of a wide range of sources, green, renewable, and contains a variety of oxygen-containing functional groups. Every year, 1.7×10 11 tons of biomass. It can meet the needs of human s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10C07D307/68C08G83/00
CPCB01J31/1691B01J31/183B01J31/2239B01J35/004B01J35/1004B01J35/1061B01J2531/025B01J2531/16B01J2531/42B01J2531/48B01J2531/842B01J2531/845B01J2531/847C07D307/68C08G83/008
Inventor 李鹏毕云波徐睿
Owner FUDAN UNIV
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