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A kind of molecular sieve porous copper metal organic framework material and its preparation method and application

A metal-organic framework, porous copper technology, applied in separation methods, copper-organic compounds, chemical instruments and methods, etc., can solve the complex cost of ligands and other problems

Active Publication Date: 2017-10-03
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the ligands used in the existing porous copper metal organic framework materials are relatively complex and costly, and provide a molecular sieve-like porous copper metal organic framework material and its preparation method and application

Method used

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  • A kind of molecular sieve porous copper metal organic framework material and its preparation method and application
  • A kind of molecular sieve porous copper metal organic framework material and its preparation method and application
  • A kind of molecular sieve porous copper metal organic framework material and its preparation method and application

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preparation example Construction

[0032] The present invention also provides a method for preparing a molecular sieve-like porous copper metal-organic framework material, comprising:

[0033] Step 1: Copper iodide, organic ligand 3,5-pyridine dicarboxylic acid (C 7 h 5 NO 4 , 3,5-PDC) and triethylenediamine (C 6 h 12 N 2 , DABCO) was dissolved in an organic solvent, then added dilute nitric acid aqueous solution, and reacted at 75-105° C. for 12-72 hours to obtain a crude product of porous copper metal-organic framework material; the cuprous iodide, organic ligand 3,5 -The molar ratio of pyridinedicarboxylic acid and triethylenediamine is preferably 1:(0.66~1.33):(1.44~2.0); the organic solvent is N,N'-dimethylformamide, dimethylmethylene A mixed solution of one or more of sulfone or N,N'-dimethylacetamide and acetonitrile; there is no special limitation on the amount of organic solvent, it can be added according to the commonly used amount in this field, and the dilute nitric acid aqueous solution The c...

Embodiment 1

[0042] Convert 9.0×10 -5 mol cuprous iodide and 9.0×10 -5 mol of organic ligand 3,5-PDC dissolved in 3.9×10 - 2 mol N,N'-dimethylformamide and 3.9×10 -2 mol of acetonitrile mixed solvent, add 1.6×10 -4 mol of triethylenediamine, under stirring, add homemade 2mol / L dilute nitric acid aqueous solution until completely dissolved, put the solution at 85°C for 72 hours, and obtain the crude product of porous copper metal organic framework;

[0043] With the configured 3.9×10 -2 mol N,N'-dimethylformamide and 3.9×10 -2 The mixed solvent composed of mol acetonitrile washed the synthesized porous copper metal organic framework material and dried it at 80° C. for 10 h to obtain a green porous copper metal organic framework crystal with a yield of 89% (calculated based on the amount of metal);

[0044] Soak porous copper metal-organic framework crystals in acetonitrile for 2 days, replace with fresh acetonitrile and soak again, repeat this cycle twice, after filtration, vacuumize ...

Embodiment 2

[0050] Convert 9.0×10 -5 mol cuprous iodide and 6.0×10 -5 mol of organic ligand 3,5-PDC dissolved in 3.9×10 - 2 mol N,N'-dimethylformamide and 3.9×10 -2 mol of acetonitrile in the mixed solvent, add 1.3×10 -4 mol of triethylenediamine, under stirring, add homemade 2mol / L dilute nitric acid aqueous solution until completely dissolved, put the solution at 85°C for 72 hours, and obtain the crude product of porous copper metal organic framework;

[0051] configured with a 3.9×10 -2 mol N,N'-dimethylformamide and 3.9×10 -2 The mixed solvent composed of mol acetonitrile was washed with the crude porous copper metal organic framework material and then dried at 80° C. for 10 h to obtain a green porous copper metal organic framework crystal with a yield of 40% (calculated based on the amount of metal);

[0052] Soak porous copper metal-organic framework crystals in acetonitrile for 2 days, replace with fresh acetonitrile and soak again, repeat this cycle twice, after filtration, ...

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Abstract

The invention provides a molecular sieve-like porous copper metal organic framework material and its preparation method and application, which belong to the technical field of inorganic-organic hybrid porous materials. The method solves the problem that the ligands used in the existing porous copper metal organic framework materials are relatively complex and costly. The structure of the material is shown in Formula I. The porous skeleton is formed by the coordination of metal copper, iodine and 3,5-pyridinedicarboxylic acid. There are both monovalent and divalent copper ions in the compound structure. After solvent exchange and heating After activation treatment, metal active sites with strong force for CO2 gas adsorption can be obtained. The invention also provides a preparation method of a molecular sieve-like porous copper metal organic framework material. The invention also provides the application of the molecular sieve-like porous copper metal organic framework material in adsorbing N2 and CO2 gases. The molecular sieve-like porous copper metal organic framework material provided by the invention has good thermal stability, the ligands used are simple, and the cost is relatively low. Formula I.

Description

technical field [0001] The invention belongs to the technical field of inorganic-organic hybrid porous materials, and in particular relates to a molecular sieve-like porous copper metal-organic framework material and its preparation method and application. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOFs) are a new type of porous solid crystalline material with three-dimensional periodic expansion formed by connecting metal ions or metal clusters with organic ligands. It has a permanently ordered microporous structure (size less than 2 nanometers), and is called a new generation of molecular sieve materials. As a porous material, compared with traditional molecular sieve inorganic zeolite materials, metal-organic framework materials are characterized by larger surface area, adjustable pore shape and inner surface, and can be widely used in the field of gas adsorption and separation. [0003] In practical applications, the main factors l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/08B01D53/02
CPCB01D53/02B01D2253/204B01D2257/40B01D2257/504C07F1/08Y02C20/40Y02P20/151
Inventor 王春锐谢冀江潘其坤孙福兴贺鸿明
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI