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Hierarchical pore MOFs material as well as preparation method and application thereof

A technology of multi-level pores and ligands, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve the problems of complex material synthesis and low adsorption capacity, and achieve simple preparation methods, good technical effects, and wide applications foreground effect

Active Publication Date: 2020-09-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is the problem of complicated material synthesis and low adsorption capacity in the prior art, and a new multi-level porous MOFs material is provided, which has the advantages of high adsorption capacity and fast adsorption rate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh a certain amount of ZrCl 4 (233mg, 1.0mmol), monodentate alkyl carboxylic acid ligand acetic acid (1.8g, 30.0mmol) in a reaction flask, add organic solvent 20mL DMF, ultrasonically mix well, then add bidentate aromatic carboxylic acid ligand 4,4 '-(1,2-ethynediyl)dibenzoic acid (266mg, 1.0mmol) was again ultrasonically mixed. The uniformly mixed reaction solution was transferred to a high-pressure reactor and heated in an oven at 120° C. for 12 h. After the reaction, the sample was cooled to room temperature and centrifuged. The obtained sample was washed 3 times with N,N-dimethylformamide DMF, and washed 3 times with ethanol under reflux to remove residual unreacted organic ligands and high boiling point solvents. Finally, the solid was heated and activated in a vacuum oven at 150° C. for 12 h to obtain a hierarchically porous Zr(IV)-MOF (BUT-30) material. The structural parameters of the material and the saturated adsorption capacity of benzene vapor are show...

Embodiment 2

[0021] Weigh a certain amount of ZrCl 4 (466mg, 2.0mmol), monodentate alkyl carboxylic acid ligand n-butyric acid (2.64g, 30.0mmol) in a reaction flask, add organic solvent 20mL N,N-dimethylacetamide DEF, ultrasonically mix evenly, and then add The bidentate aromatic carboxylic acid ligand 4,4'-(1,2-ethynediyl)dibenzoic acid (266mg, 1.0mmol) was again ultrasonically mixed. The uniformly mixed reaction solution was transferred to a high-pressure reactor and heated in an oven at 150° C. for 24 h. After the reaction, the sample was cooled to room temperature and centrifuged. The obtained sample was washed 3 times with DMF and washed 3 times with dichloromethane under reflux to remove residual unreacted organic ligands and high boiling point solvent. Finally, the solid was heated and activated in a vacuum oven at 180° C. for 18 h to obtain a hierarchically porous Zr(IV)-MOF (BUT-30) material. The structural parameters of the material and the saturated adsorption capacity of ben...

Embodiment 3

[0023] Weigh a certain amount of ZrCl 4 (700mg, 3.0mmol), monodentate alkyl carboxylic acid ligand n-octanoic acid (4.32g, 30.0mmol) in a reaction flask, add organic solvent 20mL DMF, ultrasonically mix evenly, then add bidentate aromatic carboxylic acid ligand 4, 4'-(1,2-ethynediyl)dibenzoic acid (266mg, 1.0mmol) was again ultrasonically mixed. The uniformly mixed reaction solution was transferred to a high-pressure reactor and heated in an oven at 180° C. for 36 h. After the reaction, the sample was cooled to room temperature and centrifuged. The obtained sample was washed 3 times with DMF and refluxed with chloroform for 3 times to remove residual unreacted organic ligands and high boiling point solvent. Finally, the solid was heated and activated in a vacuum oven at 150 °C for 24 h, and the hierarchically porous Zr(IV)-MOF (BUT-30) material was obtained. The structural parameters of the material and the saturated adsorption capacity of benzene vapor are shown in Table 1...

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Abstract

The invention relates to a hierarchical pore MOFs material as well as a preparation method and application thereof, and mainly solves the problems of simple material synthesis and low adsorption capacity in the prior art. The hierarchical pore MOFs material is prepared from zirconium salt, a monodentate alkyl carboxylic acid ligand and a bidentate organic carboxylic acid ligand, wherein the zirconium salt is ZrCl4, the monodentate alkyl carboxylic acid ligand is acetic acid, n-butyric acid, n-octyl carboxylic acid, dodecanoic acid and hexadecanoic acid, and the bidentate organic carboxylic acid ligand is 4,4'-(1,2-ethynediyl)dibenzoic acid; the molar ratio of the zirconium salt, the monodentate alkyl carboxylic acid ligand to the bidentate organic carboxylic acid ligand is (1-3):(10-50):1.The technical scheme can solve the problems very well, and the material can be used for preparation and application of adsorbing materials.

Description

technical field [0001] The invention relates to a hierarchically porous MOFs material, a preparation method and application thereof. It specifically relates to the preparation of a hierarchically porous Zr(IV)-MOF modified adsorption material and its adsorption to benzene series in the environment, and belongs to the field of adsorption material preparation and application. Background technique [0002] In recent years, the increasingly serious environmental pollution has attracted widespread attention at home and abroad, and how to effectively control environmental pollution has become a research hotspot in today's society. Volatile organic compounds (VOCs) are an important factor leading to environmental pollution. VOCs include benzene series (benzene, toluene, xylene, ethylbenzene, etc.), alkanes, aldehydes, ketones, and chlorinated hydrocarbons. During transportation and use, it will diffuse into the environment due to volatilization, thereby causing environmental pollu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30C08G83/00B01D53/02
CPCB01J20/226C08G83/008B01D53/02B01J2220/4812B01J2220/4806B01D2253/204B01D2257/7027B01D2257/708Y02A50/20
Inventor 李莹杨静怡胡绪尧林雨张红星肖安山
Owner CHINA PETROLEUM & CHEM CORP