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A preparation method of thin-walled graphitized carbon-wrapped metal core-shell structure material

A technology of graphitized carbon and metal composite materials, applied in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc. The problem of high reaction temperature can achieve the effect of protecting the natural environment, improving production efficiency and simple synthesis method.

Active Publication Date: 2021-05-18
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these preparation methods for preparing carbon-encapsulated transition metal materials still have shortcomings. Among them, the arc discharge method has a high reaction temperature and the obtained phase purity is low; while the laser evaporation method is difficult to control the size of the metal core and the thickness of the wrapped carbon layer Inhomogeneous; the solid-phase pyrolysis method involves graphite-based carbon sources, and it is difficult to form graphitized carbon; the thickness of the carbon layer in the chemical vapor deposition method is difficult to control, usually around 20-30 layers, because the wrapped carbon layer is too thick and the surface The curvature is reduced, which affects the catalytic activity

Method used

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  • A preparation method of thin-walled graphitized carbon-wrapped metal core-shell structure material
  • A preparation method of thin-walled graphitized carbon-wrapped metal core-shell structure material
  • A preparation method of thin-walled graphitized carbon-wrapped metal core-shell structure material

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Experimental program
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Effect test

Embodiment 1

[0045] 1. Throw lignin, formaldehyde, and sodium hydroxide into a round-bottomed flask at a mass ratio of 1:1.3:0.1 for reaction. First, dissolve lignin in an aqueous solution, then put in sodium hydroxide, and raise the temperature to 60°C. Add formaldehyde slowly, and obtain lignin resin after reacting for 3 hours;

[0046] 2. Weigh 1g of lignin resin and 50mL of 0.1mol / L ferric nitrate solution, stir evenly, put it into a hydrothermal kettle, react at 180°C for 24h, centrifuge, wash and dry to obtain lignin-iron composite Material.

[0047] 3. Place the product prepared in step 2 in a tube furnace, first raise the temperature of the tube furnace to 600°C, then quickly place the lignin-iron composite material in the tube furnace, and after carbonization for 0.5h, use 1°C The temperature is lowered at a rate of / min, and finally centrifuged, washed, and dried to obtain a core-shell structure material with 2-7 layers of graphitized carbon-wrapped iron.

[0048] refer to im...

Embodiment 2

[0050] 1. Throw lignin, formaldehyde, and sodium hydroxide into a round-bottomed flask at a mass ratio of 1:1.3:0.1 for reaction. First, dissolve lignin in aqueous solution, then add sodium hydroxide, and raise the temperature to 70°C. Slowly add formaldehyde and react for 4 hours to obtain lignin resin.

[0051] 2. Weigh 1g of lignin resin and 50mL of 0.1mol / L cobalt nitrate solution and stir evenly, put it in a hydrothermal kettle, react at 160°C for 18h, centrifuge, wash and dry to obtain lignin-cobalt composite Material.

[0052] 3. Place the product prepared in step 2 in a tube furnace, first raise the temperature of the tube furnace to 650°C, then quickly place the lignin-iron composite material in the tube furnace, and after carbonization for 0.2h, use 1°C The temperature is lowered at a rate of / min, and finally centrifuged, washed, and dried to obtain a core-shell structure material with 3-8 layers of graphitized carbon-wrapped cobalt.

[0053] refer to Figure 4 ,...

Embodiment 3

[0055] 1. Throw lignin, formaldehyde, and sodium hydroxide into a round-bottomed flask at a mass ratio of 1:1.3:0.1 for reaction. First, dissolve lignin in aqueous solution, then add sodium hydroxide, and raise the temperature to 90°C. Slowly add formaldehyde and react for 3 hours to obtain lignin resin.

[0056] 2. Weigh 1g of lignin resin and 50mL of 0.1mol / L nickel nitrate solution and stir evenly, put it in a hydrothermal kettle, react at a temperature of 160°C for 20h, centrifuge, wash and dry to obtain lignin- cobalt composite.

[0057] 3. Place the product prepared in step 2 in a tube furnace, first raise the temperature of the tube furnace to 750°C, then quickly place the lignin-iron composite material in the tube furnace, and after carbonization for 0.2h, use 1°C The temperature is lowered at a rate of 1 / min, and finally centrifuged, washed, and dried to obtain a core-shell structure material with 1-4 layers of graphitized carbon-wrapped nickel.

[0058] refer to ...

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Abstract

The invention provides a method for preparing a thin-walled graphitized carbon-wrapped metal core-shell structure material, comprising: a lignin-metal composite material preparation step, including using lignin resin as a carbon source, metal salt as a metal source, and hydrothermal Carry out carbonization to carbon source and metal source by method to obtain lignin-metal composite material; And carbonization step, comprise adopting inverse programmed temperature method to carry out carbonization treatment to described lignin-metal composite material, obtain thin-walled graphitization wrapping metal core-shell material , in which metal is the core and graphitized carbon is the shell. The invention provides a method for preparing a thin-wall graphitized carbon-wrapped metal core-shell structure material with simple operation and low cost, and the performance of the thin-wall graphitized carbon-wrapped metal core-shell structure material prepared by the method is improved.

Description

technical field [0001] The invention relates to the technical field of preparation of core-shell structural materials, in particular to a preparation method of thin-walled graphitized carbon-wrapped metal core-shell structural materials. Background technique [0002] In recent years, carbon wrapped transition metal catalysts, especially graphitized carbon (graphitized carbon, GC) wrapped transition metal (transition metal, TM) type TM@GC catalysts have received extensive attention. During the reaction process, due to the introduction of carbon atoms, the The bond length of the metal bond increases, which leads to the contraction of the metal d-band and the increase of the density of states near the Fermi level, making it have electronic structures and catalytic properties similar to platinum, rhodium, iridium, palladium, ruthenium and other rare noble metal catalysts. The activity and stability of "quasi-platinum catalysts" have been demonstrated in classical catalytic react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J23/75B01J23/755B01J35/00B01J37/08B01J37/10
CPCB01J23/745B01J23/75B01J23/755B01J35/0086B01J37/082B01J37/084B01J37/10
Inventor 秦恒飞周月金思佳周冬琴张莹莹
Owner JIANGSU UNIV OF TECH
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