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Hollow nitrogen-doped carbon sphere supported metal catalyst as well as preparation method and application thereof

A metal-loaded, nitrogen-doped carbon technology, applied in the direction of catalyst activation/preparation, catalyst carrier, chemical instruments and methods, can solve the problems of high catalyst consumption, long reaction time, low stability, etc.

Pending Publication Date: 2022-08-05
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the above-mentioned shortcoming of the prior art, provide a kind of hollow nitrogen-doped carbon sphere supported metal catalyst and its preparation method and application, to solve the problem of catalyst system in the process of furfural reductive amination to prepare furfurylamine The reaction conditions are harsh, requiring high temperature and high pressure reaction conditions, long reaction time, high catalyst dosage and low stability

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  • Hollow nitrogen-doped carbon sphere supported metal catalyst as well as preparation method and application thereof
  • Hollow nitrogen-doped carbon sphere supported metal catalyst as well as preparation method and application thereof

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preparation example Construction

[0039] The embodiment of the present invention provides a preparation method of a catalyst applied to furfural reductive amination to prepare furfuryl amine. The preparation method includes the following processes: (1) preparation of a hard template; (2) carbon source and nitrogen source precursors in the hard The surface of the template is polymerized to form a composite; (3) metal precursor is added; (4) high temperature calcination. The steps of (3) and (4) can be reversed according to the sequence of loading the metal precursors.

[0040] The embodiment of the present invention provides a nitrogen-doped hollow carbon sphere-loaded noble metal-based nanocatalyst applied to furfural reductive amination to prepare furfurylamine, the specific steps of which include:

[0041] 1. Preparation of hard template:

[0042] Preparation of polystyrene hard template: 21 mL of styrene, 1.1 mL of methyl methacrylate, 0.92 mL of acrylic acid, and 0.49 g of ammonium bicarbonate were added ...

Embodiment 1

[0064] Direct synthesis, preparation of Ru@NHCS-1-500-3 catalyst

[0065] Add 0.1g of hard template (polystyrene nanospheres) to 50mL of deionized water, after sonicating for 30min, put it into an oil bath and stir, after stirring for 30min, add 0.1g of dopamine (add multiple times), add 17.6mg RuCl 3 , after stirring for 30 min, 0.30285 g of trisaminomethane and 61.5 microliters of concentrated hydrochloric acid were added, and the pH value of the entire mixed system was 8.5. After stirring for 22 h, it was centrifuged and washed, and then placed in a refrigerator for freezing, followed by freeze-drying. The frozen samples were ground into powder and then roasted in a mixture of nitrogen and hydrogen. The firing temperature was 500 °C, the heating rate was 10 °C / min, and the holding time was 2 h. After the roasting, nitrogen-doped hollow carbon was obtained. Ball-supported Ru nanocatalysts.

Embodiment 2

[0067] Direct synthesis, preparation of Ru@NHCS-1-600-3 catalyst

[0068] Add 0.1 g of hard template (polystyrene beads) into 50 mL of deionized water, and after sonicating for 30 min, put it into an oil bath and stir, after stirring for 30 min, add 0.1 g of dopamine (multiple additions), add 17.6 g of dopamine mg RuCl 3 , after stirring for 30 min, 0.30285 g of trisaminomethane and 61.5 microliters of concentrated hydrochloric acid were added, and the pH value of the entire mixed system was 8.5. After stirring for 22 h, it was centrifuged and washed, and then placed in a refrigerator for freezing, followed by freeze-drying. The frozen samples were ground into powder and then roasted in a mixture of nitrogen and hydrogen. The firing temperature was 600 °C, the heating rate was 10 °C / min, and the holding time was 2 h. After the roasting, nitrogen-doped hollow carbon was obtained. Ball-supported Ru nanocatalysts.

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Abstract

The invention provides a hollow nitrogen-doped carbon sphere supported metal catalyst and a preparation method and application thereof.The preparation method is divided into two methods, one method is a direct synthesis method, firstly, a hard template is prepared, dopamine hydrochloride serves as a nitrogen source and a carbon source to be polymerized on the surface of the hard template, after a metal source is added, the metal source is attached to the template, and the hollow nitrogen-doped carbon sphere supported metal catalyst is obtained; and roasting to finally form the nitrogen-doped hollow carbon sphere loaded metal nano-catalyst. According to the post-synthesis method, dopamine hydrochloride is added into a prepared hard template to serve as a nitrogen source and a carbon source, the nitrogen source and the carbon source are polymerized and roasted on the hard template to form nitrogen-doped hollow carbon spheres, and a metal source is added on the basis of the nitrogen-doped hollow carbon spheres, so that the metal source is loaded on the nitrogen-doped hollow carbon spheres. According to the two methods, nitrogen-doped hollow carbon spheres are prepared on the basis of taking polystyrene as a hard template, and the nitrogen-doped hollow carbon spheres are taken as a frame structure.

Description

technical field [0001] The invention belongs to the technical field of carbon material preparation, and in particular relates to a hollow nitrogen-doped carbon ball-supported metal catalyst and a preparation method and application thereof. Background technique [0002] Carbon material refers to a porous material with carbon as the basic framework and a highly developed pore structure. Due to its well-developed pore structure, carbon materials also have the advantages of high specific surface area and adjustable pore size. In addition, carbon materials have a series of characteristics such as good chemical stability, fast thermal conductivity, high temperature resistance and corrosion resistance, which can be widely used. In the fields of catalyst carriers, biological reactions, sensors, electrode materials, adsorbents, water purification and gas separation, etc., it is the focus of research in the fields of materials, chemical industry, and physics. Nitrogen-doped hollow ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J32/00B01J37/08B01J35/10B82Y30/00B82Y40/00C07D307/52
CPCB01J27/24B01J37/082B01J37/0018C07D307/52B01J35/23B01J35/61Y02E60/50
Inventor 吴君靳明李永赵峻锋谢宇航李宜晟王成兵
Owner SHAANXI UNIV OF SCI & TECH
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