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Method for preparing nano metal-organic framework material by using internal circulation rotating packed bed

A technology of rotating packed bed and nano metal is applied in the field of preparing nano metal-organic framework materials to achieve the effect of shortening reaction time and preventing contamination between batches

Active Publication Date: 2021-02-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although BASF already has a large-scale production line for MOFs (Basolite series), it is still prepared by solvothermal / hydrothermal methods, and the obtained micron-scale particles have a wide particle size distribution, while industrially related The large-scale preparation of NMOFs has not been reported

Method used

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  • Method for preparing nano metal-organic framework material by using internal circulation rotating packed bed
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  • Method for preparing nano metal-organic framework material by using internal circulation rotating packed bed

Examples

Experimental program
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Effect test

Embodiment 1

[0072] A method for preparing nano metal-organic framework materials using an internal circulation rotating packed bed, comprising the steps of:

[0073] 2.282g (14mmol) of ferric chloride was stirred and dissolved in 350mL of deionized water; 2.326g (14mmol) of terephthalic acid was stirred and dissolved in 350mL of N,N'-dimethylformamide; 100mL of the precursor solution (deionized Water: N,N'-dimethylformamide=1:1); Add the precursor solution into the internal circulation rotating packed bed through the feed port, open the internal circulation rotating packed bed device, and adjust the rotor speed to 1500rpm; Ferric chloride solution and terephthalic acid solution were simultaneously pumped into the internal circulation packed rotary bed for precipitation and crystallization reaction, and the feed rate on both sides was controlled to be 100mL / min, and the circulating water controlled the reaction temperature to 90°C; After the material is finished, wait for the material to r...

Embodiment 2

[0078] A method for preparing nano metal-organic framework materials using an internal circulation rotating packed bed, comprising the steps of:

[0079] Stir and dissolve 2.900g (9mmol) of zirconium oxychloride octahydrate in 300mL N,N'-dimethylformamide; stir and dissolve 1.495g (9mmol) of terephthalic acid in 300mL solvent (N,N'-dimethylformamide Formamide: formic acid=9:1); configure the precursor solution: stir and dissolve 0.967 g (3 mmol) of zirconium oxychloride octahydrate in 100 mL N, N'-dimethylformamide; pass the precursor solution through the feed Put it into the internal circulation rotating packed bed, turn on the internal circulation rotating packed bed device, and adjust the rotor speed to 1500rpm; pump zirconium oxychloride octahydrate solution and terephthalic acid solution into the internal circulation rotating packed bed at the same time for precipitation and crystallization React, and control the feed rate on both sides to be 100mL / min, and the circulatin...

Embodiment 3

[0084] Repeat Example 1, the difference is only: the soluble metal salt is selected from one or more of the following substances: ferric nitrate, ferric sulfate; the effect obtained is similar to that of Example 1.

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Abstract

The invention discloses a method for preparing a nano metal organic framework material by using an internal circulation rotating packed bed, which comprises the following steps: 1) stirring and dissolving a metal salt in a solvent to prepare a metal salt solution; stirring and dissolving an organic ligand in a solvent to prepare an organic ligand solution; 2) preparing a precursor solution; 3) adding the precursor solution into a cavity of the internal circulation rotating packed bed through a feeding hole to serve as a reaction substrate; starting a motor, respectively pumping the metal saltsolution and the organic ligand solution into the internal circulation rotating packed bed for circulation after the motor stably operates, continuously carrying out precipitation and crystallizationreaction for 0.01-5 h, and taking out a reaction material to prepare a suspension; and 4) filtering and washing to obtain a clean filter cake, and drying the filter cake to obtain the product. The particle size of the product prepared by the method is 1-100 nanometers, the particle size distribution is uniform, the morphology is regular, and the product is a nano metal-organic framework material with a determined crystal form structure.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation; more specifically, it relates to a method for preparing nanometer metal-organic framework materials using an internal circulation rotating packed bed. Background technique [0002] Metal-organic frameworks (Metal Organic Frameworks, MOFs) are a class of crystalline materials with a three-dimensional pore structure composed of metal atoms as the center and connected by organic molecules. Since Yaghi's group discovered the first metal-organic frameworks (MOFs) in 1995, MOFs have been a research hotspot at home and abroad. Using different organic ligands and different inorganic metal ions or metal ion clusters, different MOFs structures can be obtained; and the space matching of the metal atom center and various organic ligands makes the pore size of the material controllable, and has a unique physical and chemical properties. The ultra-high porosity and specific surface area make...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 王洁欣魏雁陈建峰
Owner BEIJING UNIV OF CHEM TECH
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