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In-MOF material based on tricarboxylic acid ligand as well as preparation method and application of In-MOF material

A technology of tricarboxylic acids and ligands, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc. For problems such as easy closure, it can achieve the effects of good photocatalytic degradation efficiency, easy recyclability and simple preparation method.

Active Publication Date: 2020-12-15
XI'AN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, metal oxides such as TiO 2 , ZnO, etc. are easy to be lost during the application process, and the regeneration is poor. A single photocatalyst has a wide band gap, it is difficult to effectively use visible light, the photogenerated electron-hole pairs are easy to close, and the photoelectric flux yield and degradation rate are low.
Metal sulfides such as CdS, In 2 S 3 etc. are easily corroded by light to cause secondary pollution, and the surface energy of the particles is high and easy to agglomerate and fail

Method used

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  • In-MOF material based on tricarboxylic acid ligand as well as preparation method and application of In-MOF material
  • In-MOF material based on tricarboxylic acid ligand as well as preparation method and application of In-MOF material
  • In-MOF material based on tricarboxylic acid ligand as well as preparation method and application of In-MOF material

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0056] organic ligand H 3 The preparation method of L specifically follows the steps:

[0057] Step a, dissolving 4-amino-2-methylbenzoic acid in DMF, and continuously magnetic stirring in an ice-water bath until completely dissolved to obtain a mixed solution;

[0058] Every 1mol of 4-amino-2-methylbenzoic acid corresponds to 65mL of DMF;

[0059] Step b, dissolve trimesoyl chloride in DMF, stir until dissolved, and slowly add dropwise to the mixture in step a within 15 minutes, then add triethylamine dropwise within 10 minutes, react in an ice-water bath for 3 hours, and then React at room temperature for 24h to obtain a reaction solution;

[0060] Every 1mol of trimesoyl chloride corresponds to 100mL of DMF and 0.36mol of triethylamine

[0061] Step c, adding distilled water to the reaction solution under continuous magnetic stirring, and removing DMF and distilled water with a Buchner funnel after 30 min under reduced pressure suction filtration, that is, washing with d...

Embodiment 1

[0065] The organic ligand H 3 L (0.02mmol, 12.22mg), In(NO 3 ) 2 ·3H 2 O (0.04mmol, 12.75mg) and hexamethylenetetramine (0.004mmol, 0.56mg) were mixed in 6.5mL of N,N-dimethylformamide, and concentrated nitric acid with a mass fraction of 65% was added dropwise solution, adjust the pH value of the reaction system to 5.0, and seal it in a 25mL small glass bottle. The solvothermal reaction was carried out at 115°C for 72 hours, and then naturally cooled to room temperature to obtain a colorless and transparent long In-MOF material.

[0066] The method for testing the crystal structure of the In-MOF material obtained in the above examples is the same as the structure, see the following for details:

[0067] Determination of the crystal structure:

[0068] Select a single crystal of the transparent and crack-free In-MOF material, and use the Bruker Aper II CCD single crystal X-ray diffractometer of Bruker, Germany at room temperature (about 296K) to perform single crystal str...

Embodiment 2

[0085] A method for preparing an In-MOF material based on a tribasic carboxylic acid ligand, specifically:

[0086] Under closed conditions, indium nitrate trihydrate In(NO 3 ) 2 ·3H 2 O and organic ligand H 3 L. The template agent hexamethylenetetramine is dissolved in N,N-dimethylformamide, and concentrated nitric acid solution is added dropwise to adjust the pH of the reaction system to 4.0, and react under solvothermal conditions to obtain the above crystal structure In-MOF materials.

[0087] The temperature of the solvothermal reaction is 100°C, and the required reaction time is 72 hours;

[0088] Indium nitrate trihydrate, organic ligand H 3 L. The molar ratio of hexamethylenetetramine and N,N-dimethylformamide is 2:1:0.2:300; the mass fraction of concentrated nitric acid solution is 65%;

[0089] organic ligand H 3 The preparation method of L specifically follows the steps:

[0090] Step a, dissolving 4-amino-2-methylbenzoic acid in DMF, and continuously magnet...

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Abstract

The invention discloses an In-MOF material based on a tricarboxylic acid ligand, the chemical formula of the InMOF material is {[(CH3)2NH2]2(In3O4L1)}n.(solvent)x, wherein H3L is a triangular organicligand 4, 4',4"[benzoyl tri(carbonyl benzene)]-3,3',3" trimethyl tribenzoic acid; the invention also discloses a preparation method of the material, which comprises the following steps: dissolving indium nitrate trihydrate, the organic ligand H3L and hexamethylenetetramine in N,N-dimethylformamide, dropwisely adding a concentrated nitric acid solution to regulate the pH value, and reacting under solvothermal conditions to obtain. The In-MOF material disclosed by the invention has a visible light absorption wavelength range of 400-650nm, has excellent visible light response capability, and shows good photocatalytic degradation efficiency, water stability, easiness in recovery and recyclability when being used for the photocatalytic degradation of methyl orange in water.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and specifically relates to an In-MOF material based on a tribasic carboxylic acid ligand, a preparation method of the In-MOF material, and an application of the In-MOF material. Background technique [0002] About two-thirds of the world's people face water shortages, and the deterioration of water quality caused by water pollution has further exacerbated water shortages. According to statistics, the world consumes nearly hundreds of thousands of tons of dyes every year. In the process of production and use, about 15-20% of the dyes will be lost, and then hundreds of millions of tons of high-concentration dyeing residues will be produced. Even if the concentration is diluted after being discharged into the water body Very low (<1mg L -1 ) also produces high chroma, which shades sunlight and destroys aquatic ecosystems. From a molecular point of view, the structure of the dye is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/28B01J35/02C02F1/30C07C231/02C07C233/81C08G83/00C02F101/30C02F101/38B01J35/00
CPCB01J31/2239B01J31/28C08G83/008C02F1/30C07C231/02C02F2305/10C02F2101/308C02F2101/40B01J2531/33B01J35/39B01J35/40B01J35/33C07C233/81Y02W10/37
Inventor 李庆樊增禄张洛红武占省王理明朱炜
Owner XI'AN POLYTECHNIC UNIVERSITY
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