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Keggin type phosphotungstic acid composited zirconium-based MOF (metal-organic framework) photocatalyst and preparation method thereof

A technology of organic framework and photocatalyst, which is applied in the field of Keggin-type phosphotungstic acid composite zirconium-based metal-organic framework photocatalyst and its preparation, can solve the problems of high raw material cost and complicated preparation process, and achieve simple preparation process and improved separation Efficiency, the effect of improving light absorption performance

Active Publication Date: 2018-07-20
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there have been reports on the introduction of heteropolyacids into porous MOFs to construct heteropolyacid composite metal-organic frameworks ([Ni 4 (H 2 O) 2 (PW 9 o 34 ) 2 ] 10- / UiO (Journal of the American Chemical Society, 2015, 137(9): 3197-3200.), but this technology mainly combines Dawson-type POMs with noble metal-sensitized Zr-MOFs, and the cost of raw materials is high and the preparation process is complicated.

Method used

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  • Keggin type phosphotungstic acid composited zirconium-based MOF (metal-organic framework) photocatalyst and preparation method thereof
  • Keggin type phosphotungstic acid composited zirconium-based MOF (metal-organic framework) photocatalyst and preparation method thereof
  • Keggin type phosphotungstic acid composited zirconium-based MOF (metal-organic framework) photocatalyst and preparation method thereof

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Embodiment 1

[0031] A Keggin type phosphotungstic acid composite zirconium-based metal-organic framework photocatalyst and a preparation method thereof. The steps of the preparation method described in this embodiment are:

[0032] Step 1. According to the molar ratio of zirconium tetrachloride:N,N-dimethylformamide:hydrochloric acid of 1:10:(60~65), first combine the N,N-dimethylformamide with the The hydrochloric acid is mixed to obtain a mixed solution, and then the zirconium tetrachloride is added to the mixed solution and ultrasonically dissolved to obtain a zirconium tetrachloride mixed solution.

[0033] Step 2. According to the molar ratio of 2-aminoterephthalic acid:N,N-dimethylformamide of 1:(30~39), dissolve 2-aminoterephthalic acid in N,N-dimethylformamide In formamide, an organic ligand solution is obtained.

[0034] Step 3. According to the volume ratio of the zirconium tetrachloride solution: the organic ligand solution is (1.8~2.0):1, mix the zirconium tetrachloride solution and...

Embodiment 2

[0042] A Keggin type phosphotungstic acid composite zirconium-based metal-organic framework photocatalyst and a preparation method thereof. The steps of the preparation method described in this embodiment are:

[0043] Step 1. According to the molar ratio of zirconium tetrachloride:N,N-dimethylformamide:hydrochloric acid of 1:10:(65~70), first combine the N,N-dimethylformamide with the The hydrochloric acid is mixed to obtain a mixed solution, and then the zirconium tetrachloride is added to the mixed solution and ultrasonically dissolved to obtain a zirconium tetrachloride mixed solution.

[0044] Step 2: According to the molar ratio of 2-aminoterephthalic acid:N,N-dimethylformamide of 1:(37~46), dissolve 2-aminoterephthalic acid in N,N-dimethylformamide In formamide, an organic ligand solution is obtained.

[0045] Step 3. According to the volume ratio of the zirconium tetrachloride solution: the organic ligand solution is (2.0~2.1):1, mix the zirconium tetrachloride solution and...

Embodiment 3

[0050] A Keggin type phosphotungstic acid composite zirconium-based metal-organic framework photocatalyst and a preparation method thereof. The steps of the preparation method described in this embodiment are:

[0051] Step 1. According to the molar ratio of zirconium tetrachloride:N,N-dimethylformamide:hydrochloric acid of 1:10:(70~75), first combine the N,N-dimethylformamide with the The hydrochloric acid is mixed to obtain a mixed solution, and then the zirconium tetrachloride is added to the mixed solution and ultrasonically dissolved to obtain a zirconium tetrachloride mixed solution.

[0052] Step 2. According to the molar ratio of 2-aminoterephthalic acid:N,N-dimethylformamide of 1:(45~54), dissolve 2-aminoterephthalic acid in N,N-dimethylformamide In formamide, an organic ligand solution is obtained.

[0053] Step 3. According to the volume ratio of the zirconium tetrachloride solution: the organic ligand solution is (2.1~2.3):1, mix the zirconium tetrachloride solution and...

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Abstract

The invention relates to a Keggin type phosphotungstic acid composited zirconium-based MOF (metal-organic framework) photocatalyst and a preparation method thereof. The technical scheme is that the preparation method comprises the following steps: zirconium tetrachloride, N,N-dimethylformamide and hydrochloric acid are mixed and ultrasonically dissolved, and a zirconium tetrachloride mixed solution is obtained; 2-aminoterephthalic acid is dissolved in N,N-dimethylformamide, and an organic ligand solution is obtained; the zirconium tetrachloride mixed solution and the organic ligand solution are mixed and stirred, a precursor solution of a zirconium-based MOF compound is obtained, then Keggin type phosphotungstic acid is added and stirred, and a precursor solution of the Keggin type phosphotungstic acid composited zirconium-based MOF photocatalyst is obtained; the precursor solution is transferred into a reactor and subjected to a hydrothermal reaction, then centrifugation, washing anddrying are performed, and the Keggin type phosphotungstic acid composited zirconium-based MOF photocatalyst is obtained. The process is simple, operability is high, and the product can improve separation of photo-generated electron-hole pairs in a photocatalysis process and has excellent visible-light-based water splitting for hydrogen production.

Description

Technical field [0001] The invention belongs to the technical field of metal-organic framework photocatalysis. Specifically, it relates to a Keggin type phosphotungstic acid composite zirconium-based metal-organic framework photocatalyst and a preparation method thereof. technical background [0002] Metal-organic framework materials (MOFs) are three-dimensional porous materials with a periodic network structure formed by metal ions and organic ligands through self-assembly. Compared with traditional porous materials, MOFs materials have the characteristics of porosity, large specific surface area, rich in unsaturated metal sites, and adjustable composition and structure. They are widely used in gas adsorption and separation, sensing and heterogeneous catalysis. And other fields. In recent years, with the continuous in-depth research on the characteristics of MOFs narrow-band semiconductors, they have also shown great application prospects in the fields of photocatalytic reduct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/188B01J31/22B01J31/34B01J37/10C01B3/04
CPCC01B3/042B01J27/188B01J31/1691B01J31/34B01J37/10C01B2203/1088B01J2531/48B01J35/39Y02E60/36
Inventor 赵雷田盼何漩方伟李薇馨陈辉张富青张晚秋汪花丽
Owner WUHAN UNIV OF SCI & TECH
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