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Preparation method and application of oxygen-deficient rod-like core-shell structure catalyst

A core-shell structure and catalyst technology, which is applied in the field of new heterogeneous catalyst preparation, can solve the problems of differences in the number of oxygen vacancies and acid strength, the number of exposed active sites is reduced, and the size of metal nanoparticles is large. ability, improve catalytic activity, and the effect of simple preparation process

Pending Publication Date: 2022-07-29
JIANGSU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, different crystal forms of ZrO 2 The number of oxygen vacancies and acidity strength are different
However, the commonly used co-precipitation method and hydrothermal method in the preparation of ZrO 2 It is not easy to control the crystal form in the process, and the obtained ZrO 2 The particle size is large, and agglomeration is prone to occur, which makes the supported metal nanoparticles larger in size, and the number of exposed active sites is reduced, resulting in a decrease in catalytic activity.

Method used

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  • Preparation method and application of oxygen-deficient rod-like core-shell structure catalyst
  • Preparation method and application of oxygen-deficient rod-like core-shell structure catalyst
  • Preparation method and application of oxygen-deficient rod-like core-shell structure catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0038] 1. Oxygen-deficient rod-like core-shell structure 650℃-Au / 2L-ZrO 2 Preparation of @HNTs catalysts.

[0039] (1) Weigh 40g of HNTs into a three-necked flask, measure 250mL of HNO with a graduated cylinder 3 The solution was placed in a three-necked flask. Then it was placed in an oil bath and a reflux condensing device was installed, and stirred at 75° C. for 12 h. After the reaction was completed, the obtained reaction mixture was washed with deionized water until neutral, and then collected by centrifugation. The obtained samples were dried in a vacuum drying oven at 60 °C for 12 h. The obtained solid was then ground into powder, placed in a tube furnace under an air atmosphere, and calcined at 200° C. for 2 h.

[0040] (2) Weigh 0.23 g of pretreated HNTs and 0.01 g of HPC, disperse them in 20 mL of ethanol, dropwise add 0.1 mL of deionized water, and disperse by ultrasonic to make the samples evenly mixed. The flask was then placed in a 25°C water bath and stirre...

Embodiment 2

[0055] 1. Oxygen-deficient rod-like core-shell structure 450℃-Au / 2L-ZrO 2 Preparation of @HNTs catalysts.

[0056] (1) Weigh 10g of HNTs and place it in a three-necked flask, measure 63mL of HNTs with a graduated cylinder 2 SO 4 The solution was placed in a three-necked flask. Then it was placed in an oil bath and a reflux condensing device was installed, and the mixture was stirred at 75° C. for 8 h. After the reaction was completed, the obtained reaction mixture was washed with deionized water until neutral, and then collected by centrifugation. The obtained samples were dried in a vacuum drying oven at 60 °C for 24 h. The obtained solid was then ground into powder, placed in a tube furnace under air atmosphere, and calcined at 300° C. for 1 h.

[0057] (2) Weigh 0.92 g of pretreated HNTs and 0.04 g of HEC, disperse them in 80 mL of ethanol, dropwise add 0.4 mL of deionized water, and disperse by ultrasonic to make the samples evenly mixed. The flask was then placed in...

Embodiment 3

[0065] 1. Oxygen-deficient rod-like core-shell structure 350℃-Au / 2L-ZrO 2 Preparation of @HNTs catalysts.

[0066] (1) Weigh 20g of HNTs into a three-necked flask, measure 126mL of HNO with a graduated cylinder 3 The solution was placed in a three-necked flask. Then it was placed in an oil bath and a reflux condensing device was installed, and stirred at 80° C. for 8 h. After the reaction was completed, the obtained reaction mixture was washed with deionized water until neutral, and then collected by centrifugation. The obtained samples were dried in a vacuum drying oven at 50 °C for 24 h. The obtained solid was then ground into powder, placed in a tube furnace under air atmosphere, and calcined at 200° C. for 2 h.

[0067](2) Weigh 0.69 g of pretreated HNTs and 0.03 g of HPC, disperse them in 60 mL of ethanol, add 0.3 mL of deionized water dropwise, and disperse by ultrasonic to make the samples evenly mixed. The flask was then placed in a 25°C water bath and stirred for...

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Abstract

The invention belongs to the field of preparation of novel heterogeneous catalysts, and discloses a preparation method of a catalyst with an oxygen-deficient rod-like core-shell structure and a method for preparing 2, 5-furandicarboxylic acid (FDCA) by applying the catalyst to efficient catalysis of selective oxidation of biomass platform molecule 5-hydroxymethylfurfural (HMF). The obtained Au / ZrO2-coated HNTs catalyst has both oxygen vacancies and Lewis acid sites, the chemical adsorption energy of an oxidizing agent O2 in the reaction process can be reduced due to the existence of the oxygen vacancies, O2 adsorbed on the surface of the catalyst can receive delocalized electrons from the oxygen vacancies to be converted into active oxygen, and therefore the catalytic reaction activity is improved. In addition, lone pair electrons of oxygen atoms of hydroxyl groups in an intermediate in the reaction process can be captured due to existence of Lewis acid sites, the adsorption capacity of the catalyst to the reaction intermediate is improved, and the catalytic reaction efficiency is improved.

Description

technical field [0001] The invention belongs to the field of novel heterogeneous catalyst preparation, in particular to the construction of an oxygen-deficient rod-shaped core-shell structure catalyst and its application to high-efficiency catalytic biomass platform molecule 5-hydroxymenthylfurfural (HMF). A method for the preparation of 2,5-furandicarboxylic acid (2,5-Furandicarboxylic acid, FDCA) by selective oxidation. Background technique [0002] The increasing depletion of fossil energy and the environmental problems caused by its overuse have promoted the use of renewable biomass energy. HMF is a biomass platform compound derived from lignocellulosic biomass, which can be converted into a series of high value-added chemicals. For example, HMF can be oxidized to generate 2,5-diformylfuran (Furan-2 , 5-dicarbaldehyde, DFF), 5-Hydroxymethyl-2-furancarboxylic acid (HMFCA), 5-Formylfuran-2-carboxylic acid (5-Formylfuran-2-carboxylicacid, FFCA) ) and FDCA. Among these ox...

Claims

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Application Information

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IPC IPC(8): B01J23/52B01J37/16B01J37/03B82Y30/00B82Y40/00C07D307/68
CPCB01J23/52B01J37/16B01J37/036B82Y30/00B82Y40/00C07D307/68B01J35/397B01J35/393B01J35/40
Inventor 曹雨顾美凌宋忠贤应钰翟洪金张云雷
Owner JIANGSU UNIV
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