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

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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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 peaks (X-ray diffraction pattern shows the results), and no matter how adjusted, they cannot be removed

In 2013, Professor Zuo Ruqiang from Peking University used ethanol as a solvent to directly use H 3 BTC can be used as a ligand to obtain MIL-100Al. It should be pointed out that the synthesized product is a colloidal substance, which needs to be processed by supercritical CO 2 After cleaning, high-purity samples can be obtained. Although this method has economical raw materials and no impurities in the product, the post-processing process is somewhat harsh.

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