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Method of preparing metal organic frame compound by using ultrasonic waves

A metal-organic framework and compound technology, which is applied in the preparation of organic compounds, zinc organic compounds, and 2/12 group organic compounds without C-metal bonds, etc., to achieve mild reaction conditions, lower reaction temperature, and simple operation.

Inactive Publication Date: 2014-05-14
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although there are many synthetic methods for the preparation of metal-organic framework compounds, there is no report on the method of efficiently synthesizing metal-organic framework compounds through ultrasonic waves.

Method used

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  • Method of preparing metal organic frame compound by using ultrasonic waves
  • Method of preparing metal organic frame compound by using ultrasonic waves
  • Method of preparing metal organic frame compound by using ultrasonic waves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Copper acetate provided metal ions to synthesize metal organic framework compound MOF-199.

[0029] Under ultrasonication, copper acetate monohydrate (1.72g, 8.62mmol) was dissolved in a mixed solvent of water (16mL) and DMF (8mL), trimesic acid (1.00g, 4.76mmol) was dissolved in ethanol (16mL) and In the mixed solvent of DMF (8mL), mix the two solutions, stir for 10min, add triethylamine (1.0mL), stir evenly, and intermittently sonicate at the ultrasonic frequency of 400-800W for 30min (ultrasound for 2s, stop for 3s) , The reaction temperature is 20°C to 50°C. After suction filtration, the obtained product was replaced twice with water, three times with DMF, and soaked in a certain amount of DMF for 12 hours; suction filtered, replaced with dichloromethane three times, and the product was soaked in dichloromethane for 12 hours; The sample was dried under vacuum for 24 hours to obtain the metal organic framework compound MOF-199 (1.43 g, yield 99.1%).

[0030] The pr...

Embodiment 2

[0032] Copper sulfate provided metal ions to synthesize metal organic framework compound MOF-199.

[0033] Dissolve copper sulfate pentahydrate (2.12g, 8.48mmol) in a mixed solvent of water, DMF and ethanol (24mL, the volume ratio of water, DMF and ethanol is 1:1:1) under the action of ultrasonic waves, trimesic acid (1.00mg, 4.76mmol) was dissolved in the same mixed solvent (20mL, the volume ratio of water, DMF, and ethanol was 1:1:1), after mixing the two solutions, add triethylamine (0.8mL), stir Evenly, continue to intermittently sonicate at a frequency of 400-800W for 20min (set the ultrasonic conditions, sonicate for 2s, stop for 3s), and the reaction temperature is 20°C-50°C. After suction filtration, the obtained product was replaced twice with water, three times with DMF, and soaked in a certain amount of DMF for 12 hours; suction filtered, replaced with dichloromethane three times, and the product was soaked in dichloromethane for 12 hours; The sample was dried unde...

Embodiment 3

[0036] Copper chloride provided metal ions to synthesize metal organic framework compound MOF-199.

[0037] Copper chloride dihydrate (1.44g, 8.45mmol) was dissolved in a mixed solvent of water (16mL) and DMF (8mL), trimesic acid (1.00g, 4.76mmol) was dissolved in ethanol (16mL) and DMF (8mL ) in a mixed solvent, mix the two solutions, stir for 1min, add triethylamine (1.0mL), stir evenly, and intermittently sonicate at an ultrasonic frequency of 100-400W for 60min (ultrasound for 3s, stop for 2s), the reaction temperature 20℃~50℃. After suction filtration, the obtained product was replaced twice with water, three times with DMF, and soaked in a certain amount of DMF for 12 hours; suction filtered, replaced with dichloromethane three times, and the product was soaked in dichloromethane for 12 hours; The sample was dried under vacuum for 24 hours to obtain a relatively pure MOF-199 metal organic framework (1.35 g, yield 93.6%).

[0038]The prepared samples were analyzed by po...

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Abstract

The invention provides a method of preparing a metal organic frame compound by using ultrasonic waves. The method comprises the following steps: dissolving copper salt or zinc salt in a way of stirring or ultrasonication in an organic solvent or a mixed solution of water and the organic solvent; dissolving an organic ligand in the organic solvent or the mixed solution of water and the organic solvent to form an organic ligand solution; then, mixing the organic ligand solution and saline liquor, adding a proton removal agent triethylamine or diethylamine, carrying out reaction under an ultrasonic intermittent effect, and repeatedly replacing by using the solvent to obtain the metal organic frame compound. The reaction temperature is reduced by an ultrasonic synthesis method, the crystallization time is shortened, and the yield of the metal organic frame compound is greatly improved. The method has the advantages of simple operation, mild reaction condition, environmental friendliness, low cost, high reaction yield and the like, and can be put into industrial production easily.

Description

technical field [0001] The invention relates to a method for preparing metal-organic framework compounds by ultrasonic waves. Background technique [0002] Metal-organic framework compounds (Metal-organic Framework, referred to as MOFs) is a new type of porous coordination compound with a highly regular network structure formed by metal ions or metal clusters and organic ligands through coordination bonds and other weak interaction methods. Compared with traditional porous materials (such as zeolite, molecular sieve, etc.), it has many characteristics such as larger specific surface area and lower density, designable and diverse skeleton structure, and adjustable potential channel size. At the same time, MOFs have both the functional characteristics of metals and organic ligands, and have a wide range of applications in the fields of gas storage, separation and purification, and catalysis, and have become a research hotspot in recent years. The current synthesis methods of ...

Claims

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Application Information

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IPC IPC(8): C07C63/307C07C51/41C07F3/06
CPCC07C51/418C07F3/003C07C63/307
Inventor 刘艳凤张天永李彬姜爽
Owner TIANJIN UNIV
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