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Preparation and application of hierarchical pore metal-organic framework loaded heteropolyacid catalyst

A technology of supporting heteropolyacids and organic frameworks, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, refining with oxygenated compounds, etc. It can achieve the effect of high oxidative desulfurization activity and photocatalytic degradation of dyes, high crystalline skeleton structure, and simple synthesis method.

Inactive Publication Date: 2018-02-16
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can make the metal-organic framework immobilize the heteropolyacid better, it still does not solve the problem that the heteropolyacid and the macromolecular reactant cannot be well contacted due to the micropores of the metal-organic framework.

Method used

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  • Preparation and application of hierarchical pore metal-organic framework loaded heteropolyacid catalyst
  • Preparation and application of hierarchical pore metal-organic framework loaded heteropolyacid catalyst
  • Preparation and application of hierarchical pore metal-organic framework loaded heteropolyacid catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Preparation of hierarchical pore structure POMs@HKUST-1 catalyst: Weigh 0.7g of trimesic acid and 0.12g of cetyltrimethylammonium bromide, dissolve them in 16mL of ethanol solution for later use. Weigh 1.45g copper nitrate trihydrate and 1.02g phosphotungstic acid, dissolve in 12mL deionized water, mix the two solutions, and stir vigorously for 30min. The mixture was poured into a reaction kettle and placed at 120°C for 12 hours of crystallization. Cool to room temperature, filter with suction, and rinse with deionized water. Rinse the product with 50ml of ethanol solution, put it into a 100ml Erlenmeyer flask, reflux at 85°C for 4h, then suction filter, and wash with ethanol solution. Repeat the previous step three times, put it in an oven at 120°C and dry it for 10 hours, and obtain the dark blue composite material POMs@HKUST-1.

[0046] The resulting product was characterized by XRD, figure 1 (a) is the wide-angle XRD pattern of the sample between 5-60°. It can be...

Embodiment 2

[0050] Preparation of hierarchical pore structure POMs@HKUST-1 catalyst: Weigh 0.84g of trimesic acid and 0.18g of cetyltrimethylammonium bromide, dissolve them in 16mL of ethanol solution for later use. Weigh 1.21g copper nitrate trihydrate and 1.44g phosphotungstic acid, dissolve in 12mL deionized water, mix the two solutions, and stir vigorously for 30min. The mixture was poured into a reaction kettle and placed at 120°C for 12 hours of crystallization. Cool to room temperature, filter with suction, and rinse with deionized water. Rinse the product with 50ml of ethanol solution, put it into a 100ml Erlenmeyer flask, reflux at 85°C for 4h, then suction filter, and wash with ethanol solution. Repeat the previous step three times, put it in an oven at 120°C and dry it for 10 hours, and obtain the dark blue composite material POMs@HKUST-1.

Embodiment 3

[0052] Preparation of hierarchical pore structure POMs@HKUST-1 catalyst: Weigh 1.37g of trimesic acid and 1.27g of cetyltrimethylammonium bromide, dissolve them in 16mL of ethanol solution for later use. Weigh 2.17g of copper nitrate trihydrate and 1.44g of phosphotungstic acid, dissolve them in 12mL of deionized water, mix the two solutions, and stir vigorously for 30min. The mixture was poured into a reaction kettle and placed at 120°C for 12 hours of crystallization. Cool to room temperature, filter with suction, and rinse with deionized water. Rinse the product with 50ml of ethanol solution, put it into a 100ml Erlenmeyer flask, reflux at 85°C for 4h, then suction filter, and wash with ethanol solution. Repeat the previous step three times, put it in an oven at 120°C and dry it for 10 hours, and obtain the dark blue composite material POMs@HKUST-1.

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Abstract

The invention discloses a preparation method and application of a hierarchical pore metal-organic framework loaded heteropolyacid catalyst. The catalyst adopts hydrothermal-extraction method for preparation. The method includes: dissolving an organic ligand, a template agent, a metal salt and Keggin type heteropolyacid in a solvent, conducting hydrothermal synthesis of a crystal product, and thenperforming Soxhlet extraction to obtain a catalyst. The obtained catalyst has a meso-micro hierarchical porous structure, realizes high dispersion of the active component heteropolyacid and ultra-highloading capacity, and at the same time solves the problems of large mass transfer resistance, long diffusion path and small reaction place in microporous materials. The catalyst provided by the invention shows excellent catalytic performance in both photocatalytic degradation of dye wastewater and catalysis of oxidation-extraction desulfurization reaction, the catalysis reaction uses visible light and hydrogen peroxide respectively, the process is clean, environment-friendly and green, and after repeated use, the catalyst still maintains high activity, and has high industrial application value.

Description

technical field [0001] The invention relates to the field of preparation of environmental protection catalysts, in particular to the preparation of a hierarchical pore structure metal-organic framework loaded heteropolyacid heterogeneous catalyst. Background technique [0002] Heteropolyacids (also known as polyoxometalates, Polyoxometalates, abbreviated as POMs) refer to a class of polyoxygen clusters with special properties and structures formed by condensation polymerization of pre-transition elements Mo, W, V, etc. The [XM of the Keggin structure 12 o 40 ] n- It has good stability and is widely used as a catalyst. X is mainly P, Si, Ge, As, etc., and M is mainly Mo, W, etc. It has a strong Acidic, exhibits a fast reversible multi-electron oxidation-reduction transition under mild conditions, and the acidity and redox properties can be adjusted in a wide range by changing its chemical composition; therefore, whether in homogeneous or heterogeneous systems, both It is...

Claims

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Application Information

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IPC IPC(8): B01J31/34B01J31/22C02F1/30C10G27/12
CPCC10G27/12C02F1/30B01J27/188B01J31/1691B01J31/34C02F2101/308C02F2305/10B01J2531/16B01J2531/62C10G2300/70B01J35/64B01J35/39
Inventor 卢玉坤柳云骐孙道峰刘晨光王雪
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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