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Nitrogen and sulfur codoped porous carbon prepared from direct coal liquefaction heavy organic matter and preparing method and application thereof

A technology of direct coal liquefaction and nitrogen-sulfur co-doping, applied in the manufacture of hybrid/electric double layer capacitors, hybrid capacitor electrodes, etc., can solve the problems of limited selection range and high cost of nitrogen source and sulfur source, and achieve excellent electrocatalytic performance , the effect of excellent electrochemical performance

Active Publication Date: 2016-07-20
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the preparation process of nitrogen-sulfur co-doped porous carbon, most of the polymers containing nitrogen and sulfur are used as precursors, the cost is high, and the selection range of nitrogen source and sulfur source is limited.

Method used

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  • Nitrogen and sulfur codoped porous carbon prepared from direct coal liquefaction heavy organic matter and preparing method and application thereof
  • Nitrogen and sulfur codoped porous carbon prepared from direct coal liquefaction heavy organic matter and preparing method and application thereof
  • Nitrogen and sulfur codoped porous carbon prepared from direct coal liquefaction heavy organic matter and preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 10 g of ground coal direct liquefaction heavy organic matter was sulfonated in 200 g of 90% concentrated sulfuric acid at 100° C. for 15 h to obtain the first hydrophilic product. Take 0.5g of the first product and add it to a saturated solution of thiourea with a thiourea content of 1g, then add 5.5g of formaldehyde solution (37wt%), react at 100°C for 10min, and dry at 100°C to remove moisture to obtain the second product. Get the second product 1g and mechanically mix 5g magnesium citrate, it is placed in the carbonization furnace, at 200mLmin -1 Ar atmosphere, at 2°C min -1 The temperature was raised from room temperature to 490°C at a rate of 1h, and then at 5°C min -1 The rate is raised from 490°C to 700°C, kept for 1h, and then at 200mLmin -1 Cooled to room temperature under an Ar atmosphere, the resulting mixture was washed with 1M HCl to remove magnesium oxide, filtered, the filter cake was washed with water until the filtrate was close to neutral, and the fi...

Embodiment 2

[0036] 10 g of ground coal direct liquefaction heavy organic matter was sulfonated in 200 g of 98% concentrated sulfuric acid at 180° C. for 1 h to obtain the first hydrophilic product. Take 1.5g of the first product and add it to a saturated solution of thiourea with a thiourea content of 1g, then add 1.5g of formaldehyde solution (37wt%), react at 150°C for 1min, and dry at 100°C to remove moisture to obtain the second product. Get the second product 1g and 6g magnesium oxalate (or magnesium citrate) mechanically mixed, it is placed in the carbonization furnace, in 200mLmin -1 Ar atmosphere, at 2°C min -1 The rate is raised from room temperature to 490°C, kept for 30min, and then at 5°Cmin -1 The rate is raised from 490°C to 800°C, kept for 7h, and then at 200mLmin -1 Cooled to room temperature under an Ar atmosphere, the resulting mixture was washed with 1M HCl to remove magnesium oxide, filtered, the filter cake was washed with water until the filtrate was close to neutr...

Embodiment 3

[0038] 10 g of ground coal directly liquefied heavy organic matter in 180 g of fuming sulfuric acid (15 wt% SO 3 ) at 40°C for 24h to obtain the first hydrophilic product. Take 1g of the first product and add it to a saturated solution of thiourea with a thiourea content of 1g, then add 4g of formaldehyde solution (37wt%), react at 50°C for 1h, and dry at 100°C to remove moisture to obtain the second product. Get the second product 1g and mechanically mix 5g magnesium citrate, it is placed in the carbonization furnace, at 200mLmin -1 Under nitrogen atmosphere, at 1°C min -1 The temperature was raised from room temperature to 490°C at a rate of 1h, and then at 5°C min -1 The rate is raised from 490°C to 900°C, kept for 3h, and then at 200mLmin -1 Cooled to room temperature under a nitrogen atmosphere, the resulting mixture was washed with 1M HCl to remove magnesium oxide, filtered, the filter cake was washed with water until the filtrate was close to neutral, and the filter ...

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Abstract

The invention discloses a method for preparing nitrogen and sulfur codoped porous carbon prepared from direct coal liquefaction heavy organic matter. The method includes the following steps that 1, the direct coal liquefaction heavy organic matter is ground into powder, and a first hydrophilic product is obtained through hydroxylation, or carboxylation or sulfonation; 2, the first product react with a mixture of formaldehyde and thiourea to obtain a second product containing nitrogen and sulfur; 3, the second product is mechanically mixed with a magnesium source by a certain ratio, the mixture is placed in a carbonization furnace to be carbonized, and a magnesium oxide and nitrogen and sulfur codoped porous carbon mixture is obtained; magnesium oxide is removed through pickling to obtain the nitrogen and sulfur codoped porous carbon. The purpose is to broaden the selection range of nitrogen-containing species, sulfur-containing species and carbon-containing precursors in the preparing process of the nitrogen and sulfur codoped porous carbon, and a new path is found for using coal liquefaction residues. The prepared nitrogen and sulfur codoped porous carbon has excellent electrochemical performance and is high-performance electrode material of a supercapacitor and an oxygen reduction reaction catalyst.

Description

technical field [0001] The invention relates to a nitrogen-sulfur co-doped porous carbon prepared by directly liquefying heavy organic matter from coal, a preparation method and application thereof. Background technique [0002] my country's energy characteristics are rich in coal, poor in oil and little in gas, which determines that the characteristics of my country's energy structure must be dominated by coal. Coal liquefaction is an important way to use abundant coal resources to alleviate oil shortages. Abundant and cheap coal resources are an important prerequisite for China to take the lead in utilizing this technology. However, no matter what kind of coal direct liquefaction and separation technology is used at present, it is inevitable to produce liquefaction residues accounting for more than 20-30% of the total amount of raw coal. A large amount of residues can not be underestimated for the resource utilization and economic efficiency of the liquefaction process. i...

Claims

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Application Information

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IPC IPC(8): C01B31/02H01G11/24H01G11/32H01G11/86
CPCY02E60/13H01G11/24C01P2004/03C01P2006/17C01P2006/40H01G11/32H01G11/86
Inventor 周颖曹伟然邱介山王春雷肖南李玉龙刘瑞峰马冬菊万鹏
Owner DALIAN UNIV OF TECH
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