Metal-loaded covalent organic framework composite material, and preparation method and application thereof

A technology of covalent organic frameworks and composite materials, which is applied in the field of metal-supported covalent organic framework composite materials and its preparation, can solve the problems of reduced catalytic activity, reduced catalytic applications, and hazards, and achieve improved catalytic performance and excellent stability , good dispersion effect

Active Publication Date: 2021-10-08
GUANGDONG INST OF ECO ENVIRONMENT & SOIL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

4-Nitrophenol is harmful to plants and animals, and short-term exposure can cause headaches, nausea, and drowsiness in humans
[0006] However, when the noble metal is supported on the surface of the covalent organic framework material, the catalytic application is reduced due to the large particle size of the noble metal nanoparticles. At the same time, the noble metal nanoparticles are easily aggregated due to the large surface energy, resulting in a decrease in catalytic activity. Effectively balancing the particle size and content of noble metal nanoparticles is a difficult point in current research; in addition, when preparing noble metal nanoparticles, a strong reducing agent is required, which puts higher requirements on the stability and corrosion resistance of the carrier. How to choose a stable and strong covalent organic framework material as the carrier of noble metal nanoparticles, and how to ensure that when the noble metal nanoparticles are embedded in the covalent organic framework material, it will not damage its own structural framework is another difficulty that needs to be broken through

Method used

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  • Metal-loaded covalent organic framework composite material, and preparation method and application thereof
  • Metal-loaded covalent organic framework composite material, and preparation method and application thereof
  • Metal-loaded covalent organic framework composite material, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0040] 1) Preparation method of covalent organic framework material TpMA

[0041] A planetary ball mill (AM400, Ant Source Scientific Instruments (Beijing) Co., Ltd., Beijing, China) was used. Specific steps are as follows:

[0042] (1) Add 5 pieces of 5mm diameter grinding balls and 15 pieces of 7mm diameter grinding balls in a 50mL zirconia grinding jar. 1 mL of p-toluenesulfonic acid catalyst and 340 mg of melamine (MA) were added to the grinding jar, then the mixture was ground at 300 rpm for 15 min.

[0043] (2) Add 378 mg of 1,3,5-triformylphloroglucinol (TP) to the mixture, and continue grinding for 2.75 h by utilizing the kinetic energy between the grinding ball and the grinding jar. Subsequently, 0.5 mL of water was added to the mixture and triturated for 5 h.

[0044] (3) Wash twice with DMF, then vacuum-dry at 60° C. to collect TpMA.

[0045] 2) Preparation method of covalent organic framework materials supported by gold nanoparticles (Au NPs)

[0046] (1) Weig...

Embodiment 2

[0050] 1) Preparation method of covalent organic framework material TpMA

[0051] A planetary ball mill (AM400, Ant Source Scientific Instruments (Beijing) Co., Ltd., Beijing, China) was used. Specific steps are as follows:

[0052] (1) Add 5 pieces of 5mm diameter grinding balls and 15 pieces of 7mm diameter grinding balls in a 50mL zirconia grinding jar. 1.5 mL of p-toluenesulfonic acid catalyst and 360 mg of melamine (MA) were added to the grinding jar, then the mixture was ground at 300 rpm for 30 min.

[0053] (2) 390 mg of 1,3,5-triformylphloroglucinol (TP) was added to the mixture, and grinding was continued for 2.75 h by utilizing the kinetic energy between the grinding ball and the grinding jar. Subsequently, 0.2 mL of water was added to the mixture and triturated for 6 h.

[0054] (3) Wash 3 times with DMF, then vacuum dry at 65°C to collect TpMA.

[0055] 2) Preparation method of covalent organic framework materials supported by gold nanoparticles (Au NPs)

[0...

Embodiment 3

[0061] 1) Preparation method of covalent organic framework material TpMA

[0062] A planetary ball mill (AM400, Ant Source Scientific Instruments (Beijing) Co., Ltd., Beijing, China) was used. Specific steps are as follows:

[0063] (1) Add 5 pieces of 5mm diameter grinding balls and 15 pieces of 7mm diameter grinding balls in a 50mL zirconia grinding jar. 0.5 mL of p-toluenesulfonic acid catalyst and 320 mg of melamine (MA) were added to the grinding jar, and then the mixture was ground at 300 rpm for 12 min.

[0064] (2) Add 370 mg of 1,3,5-triformylphloroglucinol (TP) to the mixture, and continue grinding for 2 h by utilizing the kinetic energy between the grinding ball and the grinding jar. Subsequently, 0.5 mL of water was added to the mixture and triturated for 4 h.

[0065] (3) Wash twice with DMF, then vacuum-dry at 55° C. to collect TpMA.

[0066] 2) Preparation method of covalent organic framework materials supported by gold nanoparticles (Au NPs)

[0067] (1) W...

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Abstract

The invention belongs to the field of material preparation and environment, and particularly relates to a metal-loaded covalent organic framework composite material, and a preparation method and application thereof. The composite material is prepared from the following components: metal nanoparticles and TpMA. The preparation method comprises the following steps: mixing TpMA, chloroauric acid and methanol; and then adding sodium borohydride, and reacting to obtain the product. The metal nanoparticle loaded covalent organic framework material prepared by the invention is a novel heterogeneous catalyst which is simple to prepare, green and efficient, has high catalytic activity, high degradation rate and short time, and can catalytically reduce high-concentration pollutants.

Description

technical field [0001] The invention belongs to the field of material preparation and environment, and in particular relates to a metal-loaded covalent organic framework composite material and a preparation method and application thereof. Background technique [0002] Nitro compounds are common organic pollutants in industrial wastewater, and 4-nitrophenol, as a typical nitro pollutant, is widely used in dyestuff, papermaking, pharmaceutical, pesticide, petroleum and other industries, and it is also the chemical precursor of 4-aminophenol body. 4-Nitrophenol is harmful to plants and animals, and short-term exposure can cause headaches, nausea, and drowsiness in humans. It is listed as one of 114 organic pollutants by the U.S. Environmental Protection Agency, and the maximum allowable content in drinking water is 0.43 μmol / L. Among many methods such as adsorption, membrane separation, solvent extraction, and catalytic reduction, the catalytic reduction method based on noble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J35/00C02F1/70C02F101/38
CPCB01J31/06B01J35/006C02F1/70C02F2101/308C02F2101/38Y02W10/37B01J31/2239C02F2305/08C02F2101/345C02F1/705B01J37/0063B01J37/04
Inventor 赵晓丽牛琳吴丰昌
Owner GUANGDONG INST OF ECO ENVIRONMENT & SOIL SCI
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