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Preparation method of hydrophobic MIL-101 chromium organometallic skeleton material

A technology of organic framework and chromium metal, which is applied in the field of preparation of hydrophobic MIL-101 chromium metal organic framework material, which can solve the problems of poor moisture resistance and achieve the effects of weakening binding force, increasing adsorption capacity and high surface area

Active Publication Date: 2014-02-26
SOUTH CHINA UNIV OF TECH
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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 provide a method for preparing a hydrophobic MIL-101 chromium metal-organic framework material for the defects of poor moisture resistance of existing MIL series adsorption materials

Method used

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  • Preparation method of hydrophobic MIL-101 chromium organometallic skeleton material
  • Preparation method of hydrophobic MIL-101 chromium organometallic skeleton material
  • Preparation method of hydrophobic MIL-101 chromium organometallic skeleton material

Examples

Experimental program
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Effect test

Embodiment 1

[0041] 1.20gCr(NO 3 ) 3 9H 2 O and 0.65g of 1,4-naphthalene dicarboxylic acid were dissolved in 27mL of water, 0.026g of hydrofluoric acid and 0.090g of acetic acid were added, and placed on a magnetic stirrer and stirred for 30min to make the mixed solution uniform to obtain a precursor solution; Put it into a stainless steel high-pressure reaction kettle, seal it and put it into a temperature-programmed furnace for hydrothermal reaction. The temperature-raising program is set as follows: heat the solution from room temperature to 210°C at 5°C / min, react at a constant temperature at 210°C for 10 hours, and then heat it at 0.4°C The cooling rate of ℃ / min lowers the temperature of the reaction solution to 35°C; after the reaction, the precipitate is obtained, and the precipitate is washed with deionized water, dimethylformamide and ethanol for 2 to 3 times respectively, and the temperature of the reaction solution is 3000r / min Centrifuge for 25 minutes, filter, and dry the lo...

Embodiment 2

[0043] 1.50gCr(NO 3 ) 3 9H 2 O and 0.54g of 1,4-naphthalene dicarboxylic acid were dissolved in 22.5mL of water, 0.025g of hydrofluoric acid and 0.075g of acetic acid were added, and placed on a magnetic stirrer and stirred for 50min to make the mixed solution uniform to obtain a precursor solution; then the precursor solution Put it into a stainless steel high-pressure reactor, seal it, and put it into a temperature-programmed furnace for hydrothermal reaction. The temperature-rising program is set as follows: heat the solution from room temperature to 220°C at 5°C / min, react at a constant temperature at 220°C for 12 hours, and then The cooling rate of 0.4°C / min reduces the temperature of the reaction solution to 35°C; after the reaction, the precipitate is obtained, and the precipitate is washed with deionized water, dimethylformamide and ethanol for 2 to 3 times respectively, and the speed is 5000r / min Centrifuge for 30 minutes, filter, and dry the lower layer product at ...

Embodiment 3

[0045] 1.20gCr(NO 3 ) 3 9H 2 O and 0.52g of 1,4-naphthalene dicarboxylic acid were dissolved in 21.6mL of water, 0.024g of hydrofluoric acid and 0.072g of acetic acid were added, and placed on a magnetic stirrer and stirred for 40min to make the mixed solution uniform to obtain a precursor solution; then the precursor solution Put it into a stainless steel high-pressure reactor, seal it, and put it into a temperature-programmed furnace for hydrothermal reaction. The temperature-rising program is set as follows: heat the solution from room temperature to 220°C at 5°C / min, react at a constant temperature at 220°C for 10 hours, and then The cooling rate of 0.4°C / min lowers the temperature of the reaction solution to 35°C; after the reaction, the precipitate is obtained, and the precipitate is washed with deionized water, dimethylformamide and ethanol for 2 to 3 times respectively, and the speed is 4000r / min Centrifuge for 35 minutes, filter, and dry the lower layer product at 1...

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Abstract

The invention discloses a preparation method of a hydrophobic MIL-101 chromium organometallic skeleton material. The method comprises the following steps: dissolving chromium nitrate and 1,4-naphthalenedicarboxylic acid in water, adding hydrofluoric acid and acetic acid to stir evenly, performing a hydrothermal reaction at 210-220 DEG C, washing the obtained product with deionized water, dimethylformamide and ethanol in turn, centrifuging, filtering, and drying to prepare the hydrophobic MIL-101 chromium organometallic skeleton material. The hydrophobic MIL-101 chromium organometallic skeleton material has high Langmuir surface area and also has the high specific surface area and micro-mesoporous skeleton of a traditional MIL-101 material; and as a benzene ring is grafted on the organic connector in the skeleton, the material has higher hydrophobicity and the adsorption capacity of the material to nonpolar organic volatile substances can be increased.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a preparation method of a chromium-containing metal organic framework material, in particular to a preparation method of a hydrophobic MIL-101 chromium metal organic framework material. Background technique [0002] Metal-organic frameworks (abbreviation: MOFs) are a new type of multifunctional porous material formed by self-assembly of transition metal ions or metal clusters and organic ligands. The advantages of good stability, diverse and adjustable structural composition and functional groups, as well as chemical modification according to the target requirements, have been used in energy storage, gas adsorption separation, photoelectromagnetic catalysis, molecular recognition, microreactor and ion exchange. And other fields have shown advantages in application prospects, especially the prospect of capturing various gases and organic vapors is even more interesting. The huge sp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F11/00B01D53/02B01J20/22B01J20/30
Inventor 赵祯霞李忠夏启斌奚红霞
Owner SOUTH CHINA UNIV OF TECH
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