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Preparation method of Cu-based two-dimensional sheet mofs material

A flake-like, amino-terephthalic acid technology, applied in the field of metal-organic framework material preparation, can solve the problems of high experimental equipment, low catalytic performance, difficulty in large-scale production, etc., to achieve increased contact area, simple preparation method, The effect of short experimental period

Active Publication Date: 2021-11-23
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Surfactants are used to prevent the longitudinal growth of MOFs during the self-assembly process, so that it grows laterally into a two-dimensional sheet, but the preparation process requires too high experimental equipment and is difficult to produce on a large scale, and the surfactant in the two-dimensional sheet The surface of the MOFs material blocks the nanopores of the MOFs material to a certain extent, so that the specific surface area of ​​the prepared MOFs material is greatly reduced, and its catalytic performance is greatly reduced.

Method used

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  • Preparation method of Cu-based two-dimensional sheet mofs material
  • Preparation method of Cu-based two-dimensional sheet mofs material
  • Preparation method of Cu-based two-dimensional sheet mofs material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In order to test the effect of the ratio of metal ions and ligands on the morphology of MOFs materials, the experiment was carried out by the control variable method. The specific steps are:

[0031] Add Cu(NO 3 ) 2 ·3H 2 O stirred until completely dissolved, then added ligand 2-aminoterephthalic acid, 2-aminoterephthalic acid and Cu(NO 3 ) 2 ·3H 2 The molar ratio of O is 0.5:1, Cu(NO 3 ) 2 ·3H 2 The molar concentration of O is 0.005 mol / L. Stir for 30 minutes to mix the two evenly, then move the solution to a polytetrafluoroethylene reactor, and after installation, let it stand at 120°C for 24 hours. After the reactor was taken out and cooled to room temperature naturally, it was centrifuged at 6000r / min for 3min, and the supernatant was discarded to obtain a blue-green precipitate.

[0032] Add DMF to wash the blue-green precipitate, add 1 mL of DMF to each 1 mg of precipitate, sonicate for 10 min, centrifuge at the same speed for 3 min, and discard the supe...

Embodiment 2-3

[0034] Other steps are the same as in Example 1, and the difference is that the amount of the ligand (2-aminoterephthalic acid) added is different, and the ligand and Cu(NO 3 ) 2 ·3H 2 The molar ratio of O is 1:1 and 1.5:1 in turn. The obtained MOFs materials are marked as No. 2 and No. 3 after drying.

[0035] figure 1 a, figure 1 b, figure 1 c is the corresponding Cu(BDC-NH 2 ) SEM image of MOFs material, it can be seen that figure 1 The flake structure in b is more regular, and the flake diameter is about 8 μm. Therefore, Cu(NO 3 ) 2 ·3H 2 The optimum molar ratio of O to ligand is about 1:1. When the ligand ratio decreases, the formed flakes are smaller, about 2 μm. When the proportion of ligands increases, the increase of ligands makes the lamellar structure tightly combined and affects the lamellar separation. Therefore, suitable ligands with Cu(NO 3 ) 2 ·3H 2 The ratio of O molar weight is the 2 ) important conditions for MOFs materials.

Embodiment 4-6

[0037] In order to explore the relationship between 2-aminoterephthalic acid and Cu(NO 3 ) 2 ·3H 2 The molar concentration of O for Cu(BDC-NH 2 ) of MOFs material morphology, our implementation steps are as follows:

[0038] Add Cu(NO 3 ) 2 ·3H 2 O was stirred until completely dissolved, and the added 2-aminoterephthalic acid and Cu(NO 3 ) 2 ·3H 2 The molar ratio of O is 1:1. Cu(NO 3 ) 2 ·3H 2 The molar concentration of O is 0.001mol / L, 0.005mol / L, and 0.010mol / L in turn. Other steps are with embodiment 1. After drying, measure SEM to observe the morphology. Mark them as samples 4, 5, and 6 in turn.

[0039] figure 2 a, figure 2 b, figure 2 c are the corresponding Cu(BDC-NH 2 ) of the MOFs material, it can be seen that the sheet structure in sample No. 5 is more regular and the edges are smoother, so the added Cu(NO 3 ) 2 ·3H 2 The optimum molar concentration of O and 2-aminoterephthalic acid is about 0.005mol / L. When the concentration decreases, the ...

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Abstract

The invention relates to a preparation method of a Cu-based two-dimensional flake MOFs material. The method comprises the steps of: adding Cu(NO 3 ) 2 ·3H 2 O, stir until dissolved, then add 2-aminoterephthalic acid, and stand at 110-130°C for 22-26 hours; after cooling, centrifuge, add DMF to the precipitate, and wash the obtained precipitate; then solvent Substitution, the obtained precipitate was soaked in ethanol, centrifuged, and then dried to obtain a Cu-based two-dimensional sheet-like MOFs material. The preparation method of the present invention is simple, the production period is short, there is no influence of surfactant, the specific surface area of ​​the flake MOFs material is not affected, the contact area with reactants is increased, and it has great potential in the field of catalysis.

Description

technical field [0001] The invention belongs to the field of preparation of metal-organic framework (MOFs) materials, in particular to the preparation of two-dimensional sheet-like Cu(BDC-NH 2 ) preparation method. Background technique [0002] MOFs are a type of porous material with a periodic network structure formed by self-assembly of inorganic metal centers (metal ions or metal clusters) and bridging organic ligands. According to the constituent units of MOFs materials and the different synthesis methods, MOFs materials can be divided into network metal-organic frameworks (isoreticular metal-organic frameworks, IRMOFs), zeoliticimidazolate frameworks (zeoliticimidazolateframeworks, ZIFs), Levasil Skeleton materials (material sofinstitute Lavoisierframeworks, MILs), hole-channel framework materials (pocket-channel frameworks, PCNs) and other categories. Due to the diversity of organic ligands, the structure of MOFs materials can be designed, the channel size can be adj...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
Inventor 杨永芳王园园马野卉叶金周雪键李振兴何佳辉郭亚慧傅聪聪葛凯
Owner HEBEI UNIV OF TECH
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