A functional metal-organic framework composite material and its preparation method

A technology of metal-organic framework and composite materials, applied in the field of pyrrolidone functionalized metal-organic framework/gold nanoparticle composite materials and its preparation

Active Publication Date: 2021-06-04
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to improve the catalytic performance of gold nanoparticles in the composite material, so that the conditions required in the catalytic alcohol oxidation reaction are milder and more environmentally friendly, so as to solve the problem that organic solvents and inorganic salt oxidants are needed in the current catalytic reaction

Method used

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  • A functional metal-organic framework composite material and its preparation method
  • A functional metal-organic framework composite material and its preparation method
  • A functional metal-organic framework composite material and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Step 1: Add 0.001mol chromium nitrate nonahydrate, 0.0015mol terephthalic acid, 0.00075mol hydrofluoric acid and 0.2mol deionized water 1 into the hydrothermal reactor, react at 220°C for 9 hours; cool to room temperature and filter , washed three times with deionized water and absolute ethanol respectively; respectively used 0.5mol deionized water 2 and DMF as solvents, heated and stirred at 50°C for 24 hours; °C for 12 hours in vacuum to obtain MIL-101-Cr containing a chromium open metal center.

[0033] Step 2: At room temperature, disperse 0.001 mol of the MIL-101-Cr in 0.05 mol of anhydrous benzene; add 0.003 mol of ethylenediamine under nitrogen protection and stirring conditions, and react at 60°C for 24 hours; after cooling to room temperature Filter, wash 3 times with benzene, and vacuum dry at 150°C for 12 hours under the condition of vacuum degree of 133Pa to obtain MIL-101-NH with open metal center modified ethylenediamine 2 .

[0034] Step 3: At room temp...

Embodiment 2

[0050] Step 1: Add 0.001mol chromium nitrate nonahydrate, 0.002mol terephthalic acid, 0.0001mol hydrofluoric acid and 0.2mol deionized water 1 into the hydrothermal reactor, react at 200°C for 12 hours; cool to room temperature and filter , washed three times with deionized water and absolute ethanol respectively; respectively used 0.5mol deionized water 2 and DMF as solvents, heated and stirred at 50°C for 24 hours; °C for 12 hours in vacuum to obtain MIL-101-Cr containing a chromium open metal center.

[0051] Step 2: At room temperature, disperse 0.001 mol of the MIL-101-Cr in 0.05 mol of anhydrous benzene; add 0.004 mol of ethylenediamine under nitrogen protection and stirring conditions, and react at 80°C for 20 hours; after cooling to room temperature Filter, wash 3 times with benzene, and vacuum dry at 150°C for 12 hours under the condition of vacuum degree of 133Pa to obtain MIL-101-NH with open metal center modified ethylenediamine 2 .

[0052] Step 3: At room tempe...

Embodiment 3

[0060] Step 1: Add 0.001mol chromium nitrate nonahydrate, 0.002mol terephthalic acid, 0.0001mol hydrofluoric acid and 0.2mol deionized water 1 into the hydrothermal reactor, react at 200°C for 12 hours; cool to room temperature and filter , washed 4 times with deionized water and absolute ethanol respectively; respectively used 0.6mol deionized water 2 and DMF as solvents, heated and stirred at 60°C for 24 hours; °C for 12 hours in vacuum to obtain MIL-101-Cr containing a chromium open metal center.

[0061] Step 2: At room temperature, disperse 0.001 mol of the MIL-101-Cr in 0.05 mol of anhydrous benzene; add 0.004 mol of ethylenediamine under nitrogen protection and stirring conditions, and react at 80°C for 20 hours; after cooling to room temperature Filter, wash 4 times with benzene, and vacuum dry at 120°C for 12 hours under the condition of vacuum degree of 133Pa to obtain MIL-101-NH with open metal center modified ethylenediamine 2 .

[0062] Step 3: At room temperatu...

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Abstract

The invention provides a pyrrolidone functionalized metal organic framework / gold nanoparticle composite material and a preparation method thereof, belonging to the technical field of material chemistry and catalytic chemistry. The pyrrolidone-functionalized metal-organic framework material is coordinated by terephthalic acid and metal chromium salt in the form of six coordination, and then the open metal center is modified with pyrrolidone functional sites. The preparation method of the pyrrolidone-functionalized metal-organic framework / gold nanoparticle composite material is as follows: the pyrrolidone-functionalized metal-organic framework material is used as a substrate, and gold nanoparticles are loaded on it. The composite material provided by the present invention, due to the electron-donating effect of the modified pyrrolidone group on the metal-organic framework material to the gold nanoparticles, makes it possible to achieve high-efficiency alcohol oxidation under the conditions of using water as a solvent and molecular oxygen in the air as an oxidant reaction. The pyrrolidone functionalized metal organic framework / gold nano particle composite material has the advantages of good selectivity, simple separation, mild reaction conditions required, environmental protection and the like.

Description

technical field [0001] The invention relates to the technical fields of material chemistry and catalytic chemistry, in particular to a pyrrolidone functionalized metal-organic framework / gold nanoparticle composite material and a preparation method thereof. Background technique [0002] As an efficient catalyst, noble metal materials have always been the focus of scientific research. With the rise of nanotechnology, the synthesis and application of noble metal nanomaterials have been extensively studied. Among them, gold nanoparticles exhibit excellent performance in the field of selective catalytic alcohol oxidation, which plays an important role in promoting industrial fields such as fine chemicals and pharmaceutical production. However, as a homogeneous catalytic material, gold nanoparticles need to be reused through a complex separation process, which not only complicates the production process but also increases the economic cost. At present, loading gold nanoparticles...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10C07C45/38C07C47/54C07C47/565C07C47/575
CPCB01J31/1691B01J31/2239B01J35/006B01J35/0093B01J35/1028B01J35/1042B01J2231/70B01J2531/62C07C45/38C07C47/54C07C47/565C07C47/575
Inventor 马鼎璇李柏延施展
Owner QINGDAO UNIV OF SCI & TECH
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