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Hierarchical pore metal organic framework material as well as preparation method and application thereof

A metal-organic framework and hierarchical pore technology, which is applied in the fields of organic chemistry, chemical instruments and methods, and reductive alkylation preparation, etc., can solve the problems of difficult to control the etching/destruction of the parent MOF structure, and achieve the effect of a simple method.

Active Publication Date: 2022-08-02
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Furthermore, the etching / destruction of the parent MOF structure is difficult to control
Simple, rapid, mild and general synthetic methods to convert microporous MOFs into hierarchical porous structures have not yet been invented

Method used

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  • Hierarchical pore metal organic framework material as well as preparation method and application thereof
  • Hierarchical pore metal organic framework material as well as preparation method and application thereof
  • Hierarchical pore metal organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] The preparation of HP-UiO-66 by a reflux-assisted post-synthesis ligand replacement method is carried out as follows:

[0089] 1.1 Put 35 mg of ZrCl 4 Dissolved by sonication into 10 mL of DMF, followed by the addition of 25 mg of H 2 BDC. After the reaction solution was sonicated for 20 minutes, 0.7 mL of acetic acid was added, and then packaged into a 20 mL glass reaction vial, and reacted at 120° C. for 24 hours. After cooling to room temperature, the product was collected by centrifugation, washed with DMF and MeOH to remove unreacted raw materials, and then dried at 85°C for 12 hours for use.

[0090] 1.2 Add 656 mg of sodium acetate, 100 mg of PVP K30 and 20 mL of deionized water into a 100 mL round-bottomed flask, and ultrasonically dissolve it fully. Immediately, 100 mg of UiO-66 was dispersed therein, and the reactant was heated to 100° C. and refluxed with stirring for 12 hours. After cooling to room temperature, the product was collected by centrifugation...

Embodiment 2

[0095] The large-scale synthesis of HP-UiO-66 by a reflux-assisted post-synthesis ligand replacement method was carried out as follows (see appendix). Figure 4 ):

[0096] 2.1 Add 1 mL of concentrated hydrochloric acid and 150 mL of DMF to a 250 mL round-bottomed flask, and then add 2.33 g of ZrCl 4, 1.82g of H 2 BDC, 24.4 g of benzoic acid. The reaction solution was sonicated for 20 minutes to be fully dissolved, and then the reaction solution was heated and stirred at 120° C. for 2 to 3 days. After cooling to room temperature, the product was collected by centrifugation, washed with DMF and MeOH to remove unreacted raw materials, and then dried at 85°C for 12 hours for use. Synthesize in five batches and collect 10 g of UiO-66.

[0097] 2.2 Add 32g of sodium acetate, 4g of PVP K30 and 800mL of deionized water to a 1L round-bottomed flask, and stir to dissolve it fully. Then 10 g of the above UiO-66 was dispersed into it, and the reactant was heated to 100° C., stirred ...

Embodiment 3

[0102] The preparation of Pt@HP-UiO-66 by a reflux-assisted post-synthesis ligand replacement method was carried out as follows:

[0103] 3.1 Put 0.5mL of H with a concentration of 100mg / mL 2 PtCl 6 The solution and 222 mg of PVP (MW: 55000) were added to a round bottom flask containing 20 mL of ethylene glycol. The reaction was carried out at 180°C for 10 minutes. After cooling to room temperature, the product was collected by centrifugation, washed with n-hexane and acetone, and the obtained Pt NPs were dispersed in 20 mL of DMF for use.

[0104] 3.2 51 mg of ZrCl 4 Dissolved by sonication into 5 mL of DMF, and another 66.5 mg of H 2 BDC was sonicated into 5 mL of DMF. The above solution, 1 mL of DMF solution containing Pt NPs (1.0 mg / mL) and 1.2 mL of acetic acid were added to a 20 mL glass reaction flask, and reacted at 120° C. for 24 hours. After cooling to room temperature, the product Pt@UiO-66 was collected by centrifugation, washed with DMF and MeOH to remove un...

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Abstract

The invention provides a preparation method of a hierarchical pore metal organic framework material, which comprises the following steps: A) carrying out reflux reaction on a microporous metal organic framework material and a monocarboxylate compound in the presence of a surfactant; and B) treating a product obtained after the reaction in the step A) by using an acid solution to obtain the hierarchical pore metal organic framework material. The post-synthesis ligand substitution method provided by the invention is simple, rapid, mild and universal, and an end-capping reagent is used for replacing bridged ligands in microporous MOFs to form defective pores. Mesopores with different defective sizes are created by adjusting the concentration of an end-capping reagent, so that a hierarchical pore structure with ordered micropores and defective mesopores is formed. The method provided by the invention has relatively high universality and is suitable for various MOFs (Metal-Organic Frameworks). According to the method provided by the invention, one-pot large-scale preparation of the hierarchical porous metal organic framework material can be realized, and the HP-MOF can be favorably promoted to practical application.

Description

technical field [0001] The present invention relates to the technical field, in particular to a multi-level porous metal organic framework material and a preparation method and application thereof. Background technique [0002] How to solve the problems faced by the narrow pores in the traditional microporous metal-organic frameworks (MOFs) structure in the application of macromolecules has become an important research problem to further expand the application field of MOFs. A straightforward approach to address the above problems is to extend the length of bridging ligands to construct mesoporous MOFs. However, MOFs with high porosity are mostly thermodynamically unstable and it is difficult to avoid framework interpenetration. Moreover, long and complex organic ligands have low solubility and high synthesis cost. Based on this, the introduction of larger pores into parent microporous MOFs to generate hierarchically porous MOFs (HP-MOFs) is an effective solution. The inh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/28B01J35/10C08G83/00C07D317/36C07C249/02C07C251/24C07C209/26C07C211/45
CPCB01J31/1691B01J31/28C08G83/008C07D317/36C07C249/02C07C209/26B01J2531/48B01J2531/0213B01J35/23B01J35/60C07C251/24C07C211/45Y02P20/584
Inventor 江海龙蔡国瑞马杏
Owner UNIV OF SCI & TECH OF CHINA
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