Method for directly compounding metal-organic framework material MIL-100A1 by using trimesic acid

A MIL-100A1, metal-organic framework technology, applied in the field of preparation of metal-organic framework material MIL-100A1, can solve the problems of harsh post-treatment process, high price, and cannot be removed by adjustment, so as to achieve no environmental pollution and accurate data. Effect

Active Publication Date: 2015-11-18
TAIYUAN UNIV OF TECH
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Problems solved by technology

In the report of the first synthesis, the author chose methyl-tribenzoate (Me 3 BTC) is used as a ligand precursor, which is decomposed during the synthesis process to obtain trimesic acid (H 3 BTC) coordinates with metallic aluminum to obtain MIL-100Al, however with H 3 BTC vs. Me 3 BTC is eight times more expensive
In 2012, the Ferey group reported the synthesis of nanoparticle MIL-100Al by microwave method, which can be directly used in the synthesis 3 BTC instead of Me 3 BTC, but the synthesized samples are always accompanied by MIL-96 miscellaneous p

Method used

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  • Method for directly compounding metal-organic framework material MIL-100A1 by using trimesic acid
  • Method for directly compounding metal-organic framework material MIL-100A1 by using trimesic acid
  • Method for directly compounding metal-organic framework material MIL-100A1 by using trimesic acid

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Embodiment Construction

[0021] In order to describe the present invention in detail, the synthesis method of the present invention will be described below in conjunction with specific experimental procedures.

[0022] Chemical substances and materials: aluminum nitrate nonahydrate, tribenzoic acid, N, N dimethylformamide, nitric acid, and deionized water. The combined dosage is as follows: in grams and milliliters

[0023]

[0024] A method utilizing trimesic acid to directly synthesize metal-organic framework material MIL-100A1, the steps of which are:

[0025] (1) prepare 1mol / L dilute nitric acid standard aqueous solution

[0026] Measure 69.2mL±0.2mL of 65% concentrated nitric acid, add it to a 1000mL volumetric flask, measure deionized water and add it into the volumetric flask, and when the liquid level reaches the 1000mL mark, it becomes a 1.0mol / L dilute nitric acid aqueous solution.

[0027] (2) Hydrothermal synthesis of MIL-100Al crystal material

[0028] The synthesis of MIL-100Al cry...

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Abstract

The invention relates to the field of preparation of a metal-organic framework material MIL-100A1, particularly to a method for directly compounding the metal-organic framework material MIL-100A1 by using trimesic acid. The method comprises the following steps: mixing aluminium nitrate, trimesic acid and N,N-dimethylformamide with the molar ratio of 1:0.87:0.69; adding deionized water; uniformly stirring; dropwise adding a dilute nitric acid solution to regulate the pH of the mixed reaction solution to 1.6-1.7; sealing a polytetrafluoroethylene container in which the mixed reaction solution is accommodated in a stainless steel reaction kettle; carrying out constant-temperature crystallization reaction for 6 h at the temperature of 200 DEG C; naturally cooling to room temperature; carrying out suction filtration; adding deionized water for washing; repeatedly carrying out suction filtration for three times; drying for 15 min at the temperature of 85 DEG C and the vacuum degree of 50 Pa, so as to obtain the metal-organic framework material MIL-100A1. According to the method, aluminium nitrate is adopted as a metal source, ordinary trimesic acid is adopted as an organic ligand, and a trace amount of N,N-dimethylformamide is adopted as an additive, so that the preparation method is economic in raw material selection and free of environmental pollution.

Description

technical field [0001] The invention relates to the field of preparation of metal organic framework material MIL-100A1, in particular to a method for directly synthesizing metal organic framework material MIL-100A1 by using trimesic acid. Background technique [0002] Among the many researched MOFs materials, materials with high specific surface area and large pore size have attracted the attention of experts in many fields. The MIL-100 structure was originally composed of metallic chromium and trimesic acid (H 3 BTC) constructed MOFs materials, which have >2000m 2 / g of high specific surface area and 2.9nm macropores, which have high water stability and stability in acidic solvents, and have application potential in specific catalytic fields. [0003] In 2009, the MIL-100Al material with aluminum as the metal center was synthesized for the first time, with a specific surface area of ​​2150m 2 / g(BET), has the same topology and pore structure as MIL-100Cr. In the repo...

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Application Information

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IPC IPC(8): C07F5/06
CPCC07B2200/13C07F5/069
Inventor 杨江峰王珺邓曙光李晋平
Owner TAIYUAN UNIV OF TECH
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