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Method for preparing nitrogen-doped porous carbon from heavy organic component in coal liquefaction residue

A technology of coal liquefaction residue and nitrogen doping, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., to achieve the effect of easy large-scale production, low equipment requirements, and simple preparation process

Active Publication Date: 2013-09-11
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the process of coal liquefaction, coal liquefaction residue is an unavoidable by-product, which accounts for about 20-30% of the total amount of raw coal. A large amount of residue has an impact on resource utilization and economics in the liquefaction process that cannot be underestimated.

Method used

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  • Method for preparing nitrogen-doped porous carbon from heavy organic component in coal liquefaction residue
  • Method for preparing nitrogen-doped porous carbon from heavy organic component in coal liquefaction residue
  • Method for preparing nitrogen-doped porous carbon from heavy organic component in coal liquefaction residue

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Effect test

Embodiment 1

[0028] Mix the coal liquefaction residue with THF, extract and evaporate the solvent to obtain carbon-rich heavy organic components; mix the heavy organic components with dicyandiamide at a mass ratio of 1:0.5, and pre-oxidize in air at 300 °C for 1 h , to obtain a nitrogen-rich carbon source; the resulting nitrogen-rich carbon source is placed in a tube furnace, and the nitrogen-rich carbon source is 2 Under the atmosphere, the temperature was raised to 1000 °C at a rate of 10 °C / min, and the CO flow rate was switched to 50 mL / min. 2 , activated for 1 h, after completion, switch to 50mL / min N 2 , and cooled to room temperature to obtain nitrogen-doped porous carbon. The main properties of the porous carbon are shown in Table 1.

Embodiment 2

[0030] The coal liquefaction residue was mixed with tetrahydrofuran, and after extraction, the solvent was evaporated to obtain carbon-rich heavy organic components; the heavy organic components were mixed with ammonium chloride at a mass ratio of 1:5, and pre-oxidized in air at 150 °C for 10 h. The nitrogen-rich carbon source was obtained; the obtained nitrogen-rich carbon source was placed in a tube furnace, under an Ar atmosphere of 300 mL / min, the temperature was raised to 800 °C at a rate of 5 °C / min, and the flow rate was switched to 50 mL / min of H 2 O, activated for 10 h, after completion, switch to Ar at 300 mL / min, and cool to room temperature to obtain nitrogen-doped porous carbon. The main properties of the porous carbon are shown in Table 1.

Embodiment 3

[0032] Mix coal liquefaction residue with tetrahydrofuran, extract and evaporate the solvent to obtain carbon-rich heavy organic components; mix heavy organic components with urea at a mass ratio of 1:2, pre-oxidize in air at 200 °C for 3 h, and obtain rich Nitrogen-carbon source; the obtained nitrogen-rich carbon source was placed in a tube furnace, and in a He atmosphere of 250 mL / min, the temperature was raised to 500 °C at a rate of 1 °C / min, and the flow rate was switched to O at 100 mL / min. 2 , activated for 2 h, after the completion, switch to 250 mL / min helium, and cool to room temperature to obtain nitrogen-doped porous carbon. The main properties of the porous carbon are shown in Table 1.

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Abstract

The invention provides a method for preparing nitrogen-doped porous carbon from a heavy organic component in a coal liquefaction residue, which belongs to the field of preparation technology for carbon materials. The method comprises the following steps: subjecting the coal liquefaction residue to solvent extraction so as to obtain a heavy organic component; mixing the obtained component with a nitrogen source and carrying out preoxidation treatment so as to obtain a nitrogen-rich carbon source; and with the nitrogen-rich carbon source as a raw material, preparing the nitrogen-containing porous carbon with a high specific area by respectively using physical activation, chemical activation or a template method. The method provided by the invention has the characteristics of simple process, a wide selection range of the nitrogen source and the like and provides a novel approach for high-added value utilization of the coal liquefaction residue. The prepared nitrogen-doped porous carbon can be extensively used in fields like electrode materials, adsorption materials and catalyst carriers.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-doped porous carbon by using heavy organic components of coal liquefaction residue as a raw material, and belongs to the technical field of carbon material preparation. Background technique [0002] Coal liquefaction to oil is an important way and measure to alleviate the shortage of oil resources by using abundant coal resources. The energy structure characteristic of rich coal and little oil is an important prerequisite for my country to use this technology. Coal liquefaction is the process of converting coal from a solid state to a liquid state. Usually, under the action of high-pressure hydrogen and a catalyst, the coal is heated to 400~460 °C to cause a chemical reaction in the solvent to convert the organic macromolecules in the coal Clean coal technology for liquid oils and chemicals. However, coal liquefaction residue, a by-product, is unavoidable in the coal liquefaction process, accoun...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/33C01B32/336C01B32/342C01B32/348
Inventor 周颖邱介山刘哲孙利王春雷赵强王道龙侯雨辰金新新
Owner DALIAN UNIV OF TECH
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