Method for synthesizing MIL-101 chrome metal organic framework by nitrogen heterocyclic

A nitrogen heterocyclic compound, organic framework technology, applied in chemical instruments and methods, compounds containing periodic table Group 6/16 elements, organic chemistry, etc. High, high-purity effect

Inactive Publication Date: 2012-12-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such synthetic features limit the application prospects of MIL-101

Method used

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  • Method for synthesizing MIL-101 chrome metal organic framework by nitrogen heterocyclic
  • Method for synthesizing MIL-101 chrome metal organic framework by nitrogen heterocyclic
  • Method for synthesizing MIL-101 chrome metal organic framework by nitrogen heterocyclic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Add 0.1809g of 4-nitroimidazole into 80ml of deionized water, place it on a magnetic stirrer and stir for 15min, then add 2.6581g of terephthalic acid, stir for 15min, finally add 6.4024gCr(NO3)3·9H2O, and continue stirring until the nitric acid Chromium dissolves. The mixed solution was transferred into a 110ml stainless steel autoclave lined with polytetrafluoroethylene. The reaction kettle was placed in a blast drying oven, the temperature was raised to 150°C and kept for 24 hours, and after cooling down to room temperature, the product was taken out from the kettle, washed with deionized water, filtered with suction, and dried at 100°C to obtain 0.8 g of the product with a yield of 15%.

Embodiment 2

[0054] Add 0.9046g of 4-nitroimidazole into 80ml of deionized water, place it on a magnetic stirrer and stir for 15min, then add 2.6581g of terephthalic acid, stir for 15min, finally add 6.4024gCr(NO3)3·9H2O, and continue stirring until the nitric acid Chromium dissolves. The mixed solution was transferred into a 110ml stainless steel autoclave lined with polytetrafluoroethylene. The reaction kettle was placed in a blast drying oven, heated to 150°C and kept for 24 hours. After cooling down to room temperature, the product was taken out from the kettle, washed with deionized water, filtered with suction, and dried at 100°C to obtain 2.9 g of the product. The yield was 59%. There are no characteristic peaks of terephthalic acid crystals in the XRD spectrum.

Embodiment 3

[0056] Add 1.2665g of 4-nitroimidazole to 80ml of deionized water, place it on a magnetic stirrer and stir for 15min, then add 2.6581g of terephthalic acid, stir for 15min, finally add 6.4024g of Cr(NO3)3 9H2O, and continue stirring until the nitric acid Chromium dissolves. The mixed solution was transferred into a 110ml stainless steel autoclave lined with polytetrafluoroethylene. The reaction kettle was placed in a blast drying oven, the temperature was raised to 150°C and kept for 24 hours, and after cooling down to room temperature, the product was taken out from the kettle, washed with deionized water, filtered with suction, and dried at 100°C to obtain 3.8 g of the product with a yield of 74%. There are no characteristic peaks of terephthalic acid crystals in the XRD spectrum

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Abstract

The invention discloses a method for synthesizing an MIL-101 chrome metal organic framework by nitrogen heterocyclic. The method comprises the following steps of: using the nitrogen heterocyclic as an additive; adding the additive to water; stirring the additive and the water; and then adding an organic ligand terephthalic acid to the water; stirring the organic ligand terephthalic acid and the water; and finally adding a water soluble metal chromic salt to the water; and stirring the water until the metal chromic salt is dissolved; transferring an obtained mixture into a stainless steel high pressure reaction kettle with a polytetrafluoroethylene lining or a high pressure stirring reaction kettle with a polytetrafluoroethylene lining; crystallizing the mixture at a constant temperature 150 DEG C for 34 hours so as to obtain a product, wherein the yield of the MIL-101 chrome metal organic framework material is 60-90%. The method for synthesizing the MIL-101 chrome metal organic framework by the nitrogen heterocyclic, disclosed by the invention, has the advantages of low synthesis temperature, high purity and high yield.

Description

technical field [0001] The invention belongs to a method for synthesizing a metal-organic framework, and relates to a method for synthesizing a MIL-101 chromium metal-organic framework by utilizing a nitrogen heterocyclic compound. Background technique [0002] Metal-organic framework (Metal-organic framework), also known as metal-organic complexes or organic-inorganic hybrid materials, is a type of porous material formed by the self-assembly of metal salts and organic ligands. In recent decades, due to some The emergence of metal-organic framework materials with excellent performance has become one of the hot spots in the research of porous materials. Metal-organic framework materials have high porosity, high specific surface area, and functional tunability, which make them have applied research value and considerable application prospects in catalysis, gas storage, gas separation, drug delivery, and luminescent materials. favored by more and more researchers. [0003] Ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F11/00
Inventor 张永春陈恒陈绍云
Owner DALIAN UNIV OF TECH
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