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Method for rapidly synthesizing hierarchical pore ZIF-61 material from bimetal salt at normal temperature

A ZIF-61, bimetallic salt technology, applied in the field of rapid preparation of hierarchical porous metal-organic frameworks, can solve the problems of reduced stability of MOFs, penetration of pore channels, etc., and achieve the effects of mild conditions, energy saving and low price

Active Publication Date: 2018-10-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In principle, an ordered mesoporous structure can be formed by extending organic ligands and metal clusters, but excessive extension can easily penetrate the pores of the material, resulting in a decrease in the stability of MOFs.

Method used

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  • Method for rapidly synthesizing hierarchical pore ZIF-61 material from bimetal salt at normal temperature
  • Method for rapidly synthesizing hierarchical pore ZIF-61 material from bimetal salt at normal temperature
  • Method for rapidly synthesizing hierarchical pore ZIF-61 material from bimetal salt at normal temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 0.198g of zinc acetate dihydrate and 0.081g of zinc oxide in 1mL of N,N-dimethylformamide and 2mL of deionized water, and stir for 10h to obtain a (Zn-Zn) double metal salt solution; 0.402g of imidazole , 0.320g dimethylimidazole and 0.342g benzenesulfonic acid sodium salt were dissolved in 40mL methanol and stirred for 5 minutes to obtain a mixed solution of imidazole, dimethylimidazole and benzenesulfonic acid sodium salt; Add bimetallic salt solution to the benzenesulfonic acid sodium salt mixed solution, stir for 1 minute; then filter the obtained product with suction, activate at 90°C for 40h (soaked in ethanol), and finally put it in a vacuum oven at 110°C for 10 hours to dry. A hierarchically porous ZIF-61 material was obtained, marked as sample A.

Embodiment 2

[0033]Dissolve 0.220g of zinc acetate dihydrate and 0.090g of zinc oxide in 1mL of N,N-dimethylformamide and 2mL of deionized water, and stir for 11h to obtain a (Zn-Zn) double metal salt solution; 0.408g of imidazole , 0.328g dimethylimidazole and 0.36g benzenesulfonic acid sodium salt were dissolved in 40mL methanol, stirred for 7.5 minutes to obtain a mixed solution of imidazole, dimethylimidazole and benzenesulfonic acid sodium salt; Add bimetallic salt solution to the mixed solution of benzenesulfonic acid sodium salt, stir for 1 minute; then filter the obtained product with suction, activate at 95°C for 44h (soaked in ethanol); finally put it into a 115°C vacuum oven and dry for 11h to obtain Hierarchically porous ZIF-61 material, labeled Sample B.

Embodiment 3

[0035] Dissolve 0.241g of zinc acetate dihydrate and 0.098g of zinc oxide in 1mL of N,N-dimethylformamide and 2mL of deionized water, and stir for 12h to obtain a (Zn-Zn) double metal salt solution; 0.415g of imidazole , 0.337g dimethylimidazole and 0.378g benzenesulfonic acid sodium salt were dissolved in 40mL methanol and stirred for 10 minutes to obtain a mixed solution of imidazole, dimethylimidazole and benzenesulfonic acid sodium salt; Add bimetallic salt solution to the mixed solution of benzenesulfonic acid sodium salt, stir for 1 minute; then filter the obtained product with suction, activate at 100°C for 48h (soaked in ethanol); finally put it in a vacuum drying oven at 120°C for 12 hours, A hierarchically porous ZIF-61 material was obtained, designated as sample C.

[0036] The hierarchically porous ZIF-61 material prepared in Example 1 was used as a representative for analysis, and the analysis results of the hierarchically porous ZIF-61 material prepared in other ...

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Abstract

The invention discloses a method for rapidly synthesizing a hierarchical pore ZIF-61 material from a bimetal salt at normal temperature. The method successfully shortens the synthesis time to 1 min. The synthesis method comprises the following steps: 1, dissolving zinc acetate dihydrate and zinc oxide in a mixed solvent of N,N-dimethylformamide and water; 2, dissolving imidazole, dimethylimidazoleand sodium benzenesulfonate in methanol; 3, adding the above obtained imidazole, dimethylimidazole and sodium benzenesulfonate solution to the above obtained mixed solution of zinc acetate dihydrateand zinc oxide, and carrying out full stirring; 4, carrying out suction filtration on the obtained product, and activating the product with ethanol; and 5, carrying out vacuum drying to obtain the hierarchical ZIF-61 material. The (Zn-Zn) bimetal salt and sodium benzenesulfonate are added, so the method has the advantages of simplicity in operation, mild conditions, and great shortening of the synthesis time. The product simultaneously has micro-porous, meso-porous and macro-porous tunnels, has a high space-time yield, and has good application prospects in the fields of adsorption separation and catalysis of macromolecules.

Description

technical field [0001] The invention belongs to the field of rapid preparation of a hierarchical porous metal organic framework, and in particular relates to a method for rapidly synthesizing a hierarchical porous ZIF-61 material at room temperature using a bimetallic salt. Background technique [0002] Metal-organic frameworks (MOFs) are metal-organic hybrid network structures assembled and maintained by coordination bonds between metal ions or metal clusters and organic ligands [Kitagawa S, Kitaura R, Noro S. Functional porous coordination polymers[J]. Angewandte Chemie International Edition, 2004, 43(18): 2334-2375.]. These highly ordered frameworks have permanent porosity, and they can selectively build structural units to assemble the framework structure. Not only that, but their pore structures and functional groups are easy to adjust[Eddaoudi M, Kim J, Rosi N, et al. Systematic design of pore size and functionality inisoreticular MOFs and their application in methane...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 奚红霞张航段崇雄李非儿
Owner SOUTH CHINA UNIV OF TECH
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