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Preparation method of metal organic framework material MIL-100 (Fe)

A metal-organic framework and organic ligand technology, applied in the direction of iron-organic compounds, can solve the problems of harsh synthesis conditions, low product yield, difficult industrial production, etc., achieve high quality, overcome low yield and reduce synthesis energy. consumption effect

Active Publication Date: 2013-08-14
湖州优研知识产权服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a mild synthesis condition and high product yield in view of the shortcomings of the above-mentioned harsh synthesis conditions, low product yield and difficulty in industrial production in the existing preparation process of MIL-100 (Fe). , the method of good product quality

Method used

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  • Preparation method of metal organic framework material MIL-100 (Fe)
  • Preparation method of metal organic framework material MIL-100 (Fe)
  • Preparation method of metal organic framework material MIL-100 (Fe)

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 2.02g Fe(NO 3 ) 3 .9H 2 O. Add 0.70g of 1,3,5-benzenetricarboxylic acid into a three-necked flask filled with 5mL of deionized water, stir it magnetically for about 30 minutes, reflux and condense, raise the temperature to 95°C and keep it at a constant temperature for 12 hours. The selected reactor is a three-necked flask Add a reflux condenser. After the reaction, the sample was filtered, washed with a sufficient amount of deionized water, and placed in a drying oven for constant temperature drying for 5 hours.

[0021] The dried samples were further purified with ethanol and ammonium fluoride, respectively. First, treat with absolute ethanol at 70°C for 10h, then treat with 30mmol / L ammonium fluoride solution at 80°C for 10h, and finally wash fully with deionized water. The drying temperature was 150°C, and the drying time was 10 hours to obtain a light orange powder. Through XRD analysis, its characteristic peak is consistent with the fitted MIL-100 (Fe) charac...

Embodiment 2

[0023] Sequentially add 0.81g FeCl 3 .6H 2 O. Add 0.51g of 1,3,5-trimethylbenzenetricarboxylate into a three-necked flask filled with 15mL of deionized water, stir it magnetically for about 30 minutes, reflux and condense, raise the temperature to 95°C and keep it at a constant temperature for 12 hours. The selected reactor Add a reflux condenser to the three-necked flask. After the reaction, the sample was filtered, washed with a sufficient amount of deionized water, and placed in a drying oven for constant temperature drying for 5 hours.

[0024] The dried samples were further purified with ethanol and ammonium fluoride, respectively. First, treat with absolute ethanol at 60°C for 15h, then treat with 40mmol / L ammonium fluoride solution at 70°C for 15h, and finally wash fully with deionized water. The drying temperature was 100°C, and the drying time was 10 hours to obtain a light orange powder. Through XRD analysis, its characteristic peak is consistent with the fitted ...

Embodiment 3

[0026] 2.02g Fe(NO 3 ) 3 .9H 2 O. Add 0.63g of 1,3,5-trimethylbenzenetricarboxylate into a three-necked flask filled with 5mL of deionized water, stir magnetically for about 30min, reflux and condense, heat up to 80°C and keep at constant temperature for 20h, the selected reactor Add a reflux condenser to the three-necked flask. After the reaction, the sample was filtered, washed with a sufficient amount of deionized water, and placed in a drying oven for constant temperature drying for 5 hours.

[0027] The dried samples were further purified with ethanol and ammonium fluoride, respectively. First, treat with absolute ethanol at 80°C for 20h, then treat with 50mmol / L ammonium fluoride solution at 60°C for 10h, and finally wash fully with deionized water. The drying temperature was 150°C, and the drying time was 5 hours to obtain a light orange powder. According to XRD analysis, its characteristic peaks are consistent with the fitted MIL-100(Fe) characteristic peaks, indi...

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Abstract

The invention relates to a preparation method of a metal organic framework material MIL-100 (Fe), which comprises the following steps: proportionally adding an organic ligand and an iron source into a certain amount of deionized water, and mixing for 30 minutes; mixing the mixture obtained in the step (1) at 80-95 DEG C under atmospheric pressure to react for 5-20 hours; and filtering the solid obtained in the step (2), washing with anhydrous ethanol at 60-80 DEG C for 10-20 hours, treating with a 30-60 mmol / L ammonium fluoride solution at 60-80 DEG C for 10-20 hours, sufficiently washing with deionized water, and finally, drying at 100-200 DEG C for 5-10 hours to obtain the pure MIL-100 (Fe). The method has the advantages of mild synthesis conditions, high product yield and high product quality.

Description

technical field [0001] The invention belongs to a preparation method of a metal organic framework material, in particular to a preparation method of a metal organic framework material MIL-100 (Fe). Background technique [0002] Metal-Organic Frameworks (MOFs) materials are new multifunctional porous materials with periodic network structures formed by self-assembly of organic ligands and transition metal ions. This type of material has the characteristics of large specific surface area, high porosity, uniform pore size distribution, and structural plasticity, and has great application potential in the fields of light, electricity, magnetism, catalysis, molecular recognition, adsorption, ion exchange, and gas storage. . [0003] Metal-organic framework material MIL-100 (Cr) (MIL: Materials of Institut Lavoisier) was first synthesized and reported by the French Férey research group in 2004. It is a Cr metal trimer and organic ligand trimesic acid The supertetrahedron formed ...

Claims

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Application Information

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IPC IPC(8): C07F15/02
Inventor 张富民石静钟依均朱伟东
Owner 湖州优研知识产权服务有限公司
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