Preparation method and application of polyacid-based metal organic framework nanocrystalline catalyst

An organic framework and catalyst technology, which is applied in the field of preparation of polyacid-based metal-organic framework nanocrystalline catalysts, to achieve good catalytic activity, uniform size, and mild catalytic reaction conditions

Active Publication Date: 2017-10-13
NORTHEAST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the main synthesis methods of polyacid-based metal-organic frameworks include conventional aqueous solution synthesis and hydrothermal synthesis, and there is no report on the preparation of polyacid-based metal-organic frameworks by liquid-assisted grinding.

Method used

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  • Preparation method and application of polyacid-based metal organic framework nanocrystalline catalyst
  • Preparation method and application of polyacid-based metal organic framework nanocrystalline catalyst
  • Preparation method and application of polyacid-based metal organic framework nanocrystalline catalyst

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specific Embodiment 1

[0022] Specific embodiment 1: Cu 12 (TMA) 8 h 3 PW 12 o 40 liquid assisted milling synthesis

[0023] Take 0.24g Cu(NO 3 ) 2 ·3H 2 O and 0.28g H 3 PW 12 o 40 Dissolve in 10 mL of deionized water, adjust the pH value of the solution to 4 with NaOH, and dry the solution to obtain the mixture powder. The obtained powder and 0.14 g of trimesic acid were mixed in an agate mortar, and 1 mL of methanol was added for grinding. The mixed powder gradually turned blue. The blue powder was washed twice with water and twice with ethanol, and then dried in an oven at 60° C. for 24 hours after centrifugation to obtain a polyacid-based metal-organic framework nanocrystal catalyst. Specific embodiment 2: Cu 12 (TMA) 8 h 3 PW 12 o 40 Application of Catalytic Phenol Degradation

specific Embodiment 2

[0024] Dissolve 10 mg of phenol in 50 mL of deionized water to prepare a phenol aqueous solution with a concentration of 200 mg / L. Then, 0.05 mmol of catalyst and 15 mL of hydrogen peroxide (30 wt %) were added to the aqueous phenol solution, and the reaction temperature was 40° C. After reacting for 1 hour, monitored by gas chromatography, the conversion rate of phenol had reached 97%, and TOC detection showed that the mineralization rate had reached 87%. The conversion rate of the above reaction is monitored by gas chromatography, and the mineralization rate is monitored by TOC analyzer. The relationship of phenol conversion rate with time is shown in the appendix image 3 .

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Abstract

The invention provides a preparation method and application of a polyacid-based metal organic framework nanocrystalline catalyst. The nanocrystalline catalyst can be synthesized by a liquid-assisted grinding method, the obtained nanocrystalline catalyst has small particle dimension, and the grain size of the nanocrystalline catalyst is 50 to 200 nanometers; furthermore, the nanocrystalline catalyst has uniform morphology and size; meanwhile, the catalyst has determined component and structure. Under moderate condition, hydrogen peroxide is utilized as an oxidizing agent, the nanocrystalline can catalyze phenol to be degraded in high efficiency, and high phenol conversion rate and high mineralization rate are achieved. The catalyst can be completely separated and recycled through simple centrifugal operation, can be used repeatedly after being dried and can still keep good catalytic activity after being repeatedly utilized for multiple times. The preparation method of the polyacid-based metal organic framework nanocrystalline catalyst disclosed by the invention is simple and can effectively reduce the particle size of the catalyst; thus, phenomena of diffusional limitation and carbon deposit in catalytic reaction are reduced, and a material catalyzing efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of catalytic materials, and relates to a preparation method and application of a polyacid-based metal-organic framework nanocrystal catalyst. Background technique [0002] Polyoxometalates (POMs for short), also known as polyacid compounds, are a class of metal-oxygen cluster compounds composed of pre-transition metals (Mo, W, V, Nb, Ta, etc.) in the highest oxidation state. . Due to their strong acidity and rich redox chemistry, polyacids are an excellent class of acid, redox, and bifunctional catalysts (acid catalysis and oxidation catalysis). Polyacid-based metal-organic frameworks (POM-MOFs) introduce polyacids into the pores of metal-organic frameworks. On the one hand, it can realize the immobilization of homogeneous polyacid catalysts. Combining the catalytic functions of the latter is an important way to design new and efficient multi-acid catalysts. Although some progress has been made in the c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/34B01J35/02C02F1/72C02F101/34
CPCB01J31/2213B01J31/34B01J35/023B01J2531/16B01J2540/50C02F1/722C02F1/725C02F2101/345
Inventor 鹿颖刘术侠钟夏华
Owner NORTHEAST NORMAL UNIVERSITY
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