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A kind of magnetic hierarchical porous metal organic framework catalyst and its preparation method and application

A technology of metal-organic frameworks and hierarchical pores, which is applied in the fields of organic compound/hydride/coordination complex catalysts, organic chemistry, catalytic reactions, etc. To solve the problems of poor quality and performance, to achieve the effect of magnetic controllability, wide application range, and reduced diffusion resistance

Active Publication Date: 2020-06-26
山西立铂隆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, a single metal-organic framework material has only micropores and mesopores, the catalytic mass transfer performance is not good, and the catalyst regeneration process is complicated, which greatly limits the application of metal-organic framework catalysts.

Method used

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  • A kind of magnetic hierarchical porous metal organic framework catalyst and its preparation method and application
  • A kind of magnetic hierarchical porous metal organic framework catalyst and its preparation method and application
  • A kind of magnetic hierarchical porous metal organic framework catalyst and its preparation method and application

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Embodiment 1

[0047] A method for preparing the magnetic multi-stage porous metal organic framework catalyst of the present invention, the specific steps are as follows:

[0048] (1) Weigh 15.33 g acrylamide, 3.11 g N,N'-methylenebisacrylamide and 2.25 g polyvinyl alcohol (molecular weight 10000 g / mol), and dissolve them in 40 mL distilled water to form a mixed aqueous solution ;

[0049] (2) Take 4 mL of the mixed aqueous solution prepared in step (1), 0.4 mL Triton X-405 and 0.2g Fe 3 O 4 Nano particles, stir evenly with a mechanical stirrer at 1500 rpm, and then add 6 mL xylene and 200 mL ammonium persulfate solution (10 wt%) drop by drop, continue stirring for 10 minutes, and then add 30 mL tetraethyl ethyl Diamine

[0050] (3) The resulting system was reacted at 60 ℃ for 24 hours, and the resulting product was cut into 0.3 cm × 0.3 cm × 0.3 cm block particles, washed three times with deionized water and acetone, and dried in vacuum at 60 ℃ for 12 h, to obtain magnetic macroporous polyacryla...

Embodiment 2

[0054] A method for preparing the magnetic multi-stage porous metal organic framework catalyst of the present invention, the specific steps are as follows:

[0055] The preparation method of magnetic macroporous polyacrylamide is the same as the step (1), step (2) and step (3) of Example 1;

[0056] Dissolve 1.732 g of zinc nitrate hexahydrate and 0.3217 g of terephthalic acid into 11 mL of N,N'-dimethylformamide, take 4 mL of the prepared solution into a polytetrafluoroethylene-lined reactor and add Several pieces of magnetic macroporous polyacrylamide were reacted at 105 ℃ for 24 h. After magnetic separation and repeated washing with ethanol for three times, the product was vacuum dried in a vacuum oven at 60 ℃ for 12 h to obtain a magnetic hierarchical porous MOF-2 composite catalyst .

[0057] Figure 7 with Figure 8 Is the scanning electron microscope image of the internal cross-section of the obtained magnetic multi-porous MOF-2 composite catalyst (different magnification), b...

Embodiment 3

[0059] A method for preparing the magnetic multi-stage porous metal organic framework catalyst of the present invention, the specific steps are as follows:

[0060] The preparation method of magnetic macroporous polyacrylamide is the same as the step (1), step (2) and step (3) of Example 1;

[0061] Dissolve 0.080 g of zirconium tetrachloride and 0.057 g of terephthalic acid into 10 mL of N,N'-dimethylformamide, take 4 mL of the prepared solution in a polytetrafluoroethylene lined reactor, and add Several pieces of magnetic macroporous polyacrylamide were reacted at 120 ℃ for 24 h. After magnetic separation and repeated washing with ethanol for three times, the product was vacuum dried in a vacuum oven at 60 ℃ for 12 h to obtain a magnetic hierarchical porous UiO-66 composite catalyst .

[0062] Picture 9 Is a scanning electron microscope image of the internal cross-section of the obtained magnetic multi-porous UiO-66 composite catalyst. Picture 9 It can be seen that UiO-66 grows ...

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Abstract

The invention discloses a preparation method of a magnetic hierarchical porous metal-organic framework catalyst, which includes the following steps: (1) Dissolve soluble metal salts and multidentate organic ligands in a solvent to obtain a mixed solution of metal salt-organic ligands; ( 2) Take the magnetic macroporous polyacrylamide and place it in the reaction kettle, then add the metal salt organic ligand mixed solution obtained in step (1) into the reaction kettle, heat the reaction, and after the reaction is completed, perform magnetic separation, washing and drying of the product in sequence , that is, a magnetic hierarchical porous metal-organic framework catalyst is obtained. The preparation method is simple to operate and has wide application range. The invention also discloses a magnetic hierarchical porous metal-organic framework catalyst, which has high catalytic activity, good mass transfer performance, and can be magnetically regenerated. The invention also discloses the application of the catalyst in catalyzing organic synthesis reactions.

Description

Technical field [0001] The invention relates to the technical field of catalysts, in particular to a magnetic multi-stage porous metal organic framework catalyst and a preparation method and application thereof. Background technique [0002] The metal organic framework material has a very high specific surface area and pore volume, and the pore size in the framework is highly ordered and adjustable, which is expected to realize the selective permeability of the substrate. Unsaturated metal sites in the framework are used as Lewis acid sites and can be used as catalytic centers. They are now used in cyanation reactions, oxidation reactions of hydrocarbons and alcohols, esterification reactions, Diels-Alder reactions, and many other reactions. Has high activity. [0003] However, a single metal-organic framework material has only micropores and mesopores, the catalytic mass transfer performance is not good, and the catalyst regeneration process is complicated, which greatly limits t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J31/22C07C45/58C07C47/225
CPCC07C45/58B01J31/2239B01J31/28B01J2231/52B01J2531/842B01J2531/16B01J2531/48B01J2531/26B01J35/33C07C47/225
Inventor 霍甲金硼陈兰君王双印
Owner 山西立铂隆新材料有限公司