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Water-stabilized zinc-copper metal organic frame material and preparation method and application thereof

An organic framework and copper metal technology, applied in the chemical field, can solve instability and other problems, and achieve the effects of high water stability, high CO2 adsorption capacity, and high BET specific surface area

Inactive Publication Date: 2016-01-13
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it was found that this series of metal-organic framework materials is unstable under hydrothermal conditions and will be hydrolyzed into another phase, so further modification is needed to enhance its water stability

Method used

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  • Water-stabilized zinc-copper metal organic frame material and preparation method and application thereof
  • Water-stabilized zinc-copper metal organic frame material and preparation method and application thereof
  • Water-stabilized zinc-copper metal organic frame material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Zn 0.99 Cu 0.01 Preparation of BIms.

[0049] 883.49mg or 2.97mmol Zn (NO 3 ) 2· 6H 2 O, 7.248mg or 0.03mmol of Cu(NO 3 ) 2 Dissolve 564.6 mg, ie 3 mmol, of organic ligand BIm in 160 mL of DMF and 40 mL of ethanol, react at 100° C. for 72 h, and then cool to room temperature. Filter, wash with 60mL DMF, and dry to obtain the product, yield: 91.16%. structured as figure 1 Shown, has the general chemical formula Zn x Cu 1-x BIm (x0.99 Cu 0.01 The metal site of BIM has a helical icosahedral structure and contains three-dimensional channels with left-handed helix and right-handed helix as mirror images.

[0050] (2) Zn 0.95 Cu 0.05 Preparation of BIms.

[0051] 847.79mg or 2.85mmol of Zn(NO 3 ) 2· 6H 2 O, 36.24mg or 0.15mmol of Cu(NO 3 ) 2 Dissolve 564.6mg, ie 3mmol, of organic ligand BIm in 150mL DMF and 50mL ethanol, react at 100°C for 72h, and then cool to room temperature. Filter, wash with 60mL DMF, and dry to obtain the target product, yield: 9...

Embodiment 2

[0059] Zn prepared by different methods 0.99 Cu 0.01 BIm.

[0060] method 1:

[0061] 11.78mg or 0.0396mmol Zn (NO 3 ) 2· 6H 2 O, 0.09664mg that is 0.0004mmolCu (NO 3 ) 2 Dissolve 7.45 mg or 0.04 mmol of organic ligand BIm in 2 mL of DMF and 0.5 mL of ethanol, transfer the solution to a flask, seal it and put it in an oven, react at 140 °C for 24 h, then cool to room temperature at a rate of 5 °C / h . Filter and wash with DMF to obtain light green massive crystals, yield: 50.25%.

[0062] Method 2:

[0063] 11.78mg or 0.0396mmol Zn (NO 3 ) 2· 6H 2 O, 0.09664mg that is 0.0004mmolCu (NO 3 ) 2 Dissolve 7.45 mg of 0.04 mmol of organic ligand BIm in 2 mL of DMF and 0.5 mL of ethanol, transfer the solution to a hard glass tube with an inner diameter of 8 mm, seal it and put it in an oven, react at 100 ° C for 72 h, and then use 5 ° C / h to cool down to room temperature. Filter and wash with DMF to obtain light green massive crystals, yield: 51.68%.

[0064] Method 3...

Embodiment 3

[0074] Various properties of the zinc-copper mixed metal metal-organic framework material prepared in Example 1 and Example 2 were characterized.

[0075] 1. Powder diffraction characterization of purity:

[0076] Zn 0.99 Cu 0.01 Bim, Zn 0.95 Cu 0.05 BIm and Zn 0.90 Cu 0.10 The powder diffraction data collection of BIm samples was completed on a BrukerD8advance diffractometer. The operating voltage of the instrument was 40KV, the current was 40mA, and the copper target X-ray (CuK, λ=1.5418?) monochromated by graphite was used in the range of 5° to 40° Continuous scanning is completed. The simulation transformation of powder diffraction spectrum of single crystal structure was performed using Mercury software. From figure 2 According to the powder diffraction data of the present invention, the three materials are isomorphic.

[0077] 2. Determination of metal ion content in zinc-copper metal organic framework.

[0078] (1) Inductively coupled plasma atomic emission s...

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Abstract

The invention relates to a water-stabilized zinc-copper metal organic frame material and a preparation method and application thereof. The water-stabilized zinc-copper metal organic frame material has the chemical formula of ZnxCu1-xBIm, wherein x is smaller than 1. ZnxCu1-xBIm is shown as the structural formula (please see the formula in the specification), wherein zinc or copper occupies metal sites of ZnxCu1-xBIm. The preparation method includes the steps of firstly, mixing organic ligand BIm, Zn(NO3)2.6H2O and Cu(NO3)2 to be dissolved into DMF or the mixed solvent of DMF and ethyl alcohol with the volume ratio between 4 to 1 and 3 to 1, wherein the ratio of the molar weight ratio of BIm to the total molar weight of Zn(NO3)2.6H2O and Cu(NO3)2 is 1 to 1, the molar ratio of Zn(NO3)2.6H2O to Cu(NO3)2 is between 99 to 1 and 85 to 15; secondly, making the materials react for 24-72 h at a temperature of 100-140 DEG C or adding auxiliaries to react to generate solid products, cooling to the room temperature, and conducting filtering, DMF washing and drying. The water-stabilized zinc-copper metal organic frame material can be used as carbon dioxide adsorbent, has high water stability, acid stability and thermal stability, has a high porous property, has a high BET specific surface area and high CO2 adsorption capacity, and has potential application on the aspects of the greenhouse effect and the like.

Description

technical field [0001] The invention relates to the direction of coordination chemistry in the field of chemistry, and the main content is a metal organic framework material, especially a novel water-stable zinc-copper mixed metal metal organic framework material and its preparation method and application. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOFs) or porous coordination polymers are a type of crystalline framework material with permanent porosity formed by metal ions and organic ligands connected to each other through strong coordination bonds. The advantage of the material over traditional inorganic porous materials is that the framework topology, pore size, and surface properties can be changed by changing metal ions and ligands, and it has superior physical and chemical properties. [0003] Since American scientist Omar M. Yaghi synthesized and reported metal-organic framework materials (MOF-5) in 1999, this porous material wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06C07D233/64B01J20/22
CPCY02C20/40
Inventor 周小平李丹朱晓威
Owner SHANTOU UNIV
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