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Electrolytic and nitrogen-doping one-step method for preparing petroleum coke-based carbon quantum dots

A technology of coke-based carbon quantum dots and petroleum coke, which is applied in the field of electrolytic preparation of petroleum coke-based carbon quantum dots and nitrogen doping, and can solve problems such as difficult large-scale preparation and cumbersome preparation process

Active Publication Date: 2016-07-06
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation and chemical modification of CQDs generally need to be carried out step by step, which makes the preparation process cumbersome and difficult to prepare on a large scale.

Method used

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  • Electrolytic and nitrogen-doping one-step method for preparing petroleum coke-based carbon quantum dots
  • Electrolytic and nitrogen-doping one-step method for preparing petroleum coke-based carbon quantum dots
  • Electrolytic and nitrogen-doping one-step method for preparing petroleum coke-based carbon quantum dots

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At 60°C, preheat the petroleum asphalt for 20 minutes. Weigh preheated petroleum asphalt 0.96 (16wt%), 1.5 (23wt%), 2.5g (33wt%) respectively, add appropriate amount of dichloromethane, stir until the asphalt is completely dissolved, then weigh 5.0g of petroleum coke respectively, and Mix the asphalt evenly, put it into a constant temperature water bath, evaporate most of the solvent, and obtain the electrode sheet raw material in black paste. The paste was extruded to obtain disc-shaped electrode sheets. The prepared electrode sheets were calcined in a tube electric furnace at 800° C. for 2 h under a nitrogen atmosphere. The prepared electrode sheet was used as the working electrode, the Pt electrode was used as the counter electrode, and 100mL of 0.5M NaOH solution was used as the electrolyte, at 220mA·cm -2 Electrolysis was carried out in the electrolytic cup for 12 hours under the current density to obtain an electrolyte solution containing carbon nanoparticles. ...

Embodiment 2

[0031] At 60°C, preheat the petroleum asphalt for 20 minutes. Weigh 1.5g of preheated petroleum asphalt, add appropriate amount of dichloromethane, stir until the asphalt is completely dissolved, then weigh 5.0g of petroleum coke, mix it with petroleum asphalt, put it in a constant temperature water bath, evaporate most of the solvent, and obtain Electrode sheet raw material in black paste. The paste was extruded to obtain disc-shaped electrode sheets. The prepared electrode sheets were calcined in a tube electric furnace at 500, 800, and 1000° C. for 2 h under a nitrogen atmosphere, respectively. The prepared electrode sheet was used as the working electrode, the Pt electrode was used as the counter electrode, and 100mL of 0.5M NaOH solution was used as the electrolyte, at 220mA·cm -2Under the current density, it was electrolyzed in the electrolytic cup for 24 hours to obtain an electrolyte solution containing carbon nanoparticles. After filtering through a 0.22 μm micropo...

Embodiment 3

[0033] At 60°C, preheat the petroleum asphalt for 20 minutes. Weigh 1.5g of preheated petroleum asphalt, add appropriate amount of dichloromethane, stir until the asphalt is completely dissolved, then weigh 5.0g of petroleum coke, mix with petroleum asphalt, put it in a constant temperature water bath, evaporate most of the solvent, and obtain Electrode sheet raw material in black paste. The paste was extruded to obtain disc-shaped electrode sheets. The prepared electrode sheet was calcined in a tube electric furnace at 800 °C for 2 h under a nitrogen atmosphere. The prepared electrode sheet was used as the working electrode, the Pt electrode was used as the counter electrode, and 100mL of 0.1M NaOH solution was used as the electrolyte, at 220mA·cm -2 Under the current density, electrolyze in the electrolytic cup for 8, 12, 24, 48, 72, 96, 120, and 144 hours, respectively, to obtain an electrolyte containing carbon nanoparticles. After filtering through a 0.22 μm microporou...

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Abstract

The invention belongs to the scientific field of carbon nano-materials and relates to an electrochemical method for preparing petroleum coke-based carbon quantum dots and doping nitrogen in a one-step manner. In the invention, petroleum coke, which has high carbon content, low ash and a developed graphite lamellar structure, is creatively selected as a carbon source, and through an electrochemical oxidizing method, a novel technical method of preparing the carbon quantum dots is developed. Through change on calcination temperature, types of electrolytes and current density, fluorescent performance of the carbon quantum dots can be regulated. By means of addition of a nitrogen-doping agent to the electrolyte, preparation of nitrogen-doped carbon quantum dots through the electrochemical method in one step is achieved, and for the first time, ethylenediamine is employed as the electrolytic nitrogen-doping agent. Meanwhile, for the first time, foam nickel is creatively employed instead of a conventional Pt electrode, so that the method greatly increases electrolytic efficiency and reduces preparation cost. The petroleum coke is easy to obtain and low in cost. The whole process is simple in operation process, is convenient to product the carbon quantum dots industrially in large scale. The carbon quantum dots have wide application prospects in the fields of photo-catalysis, bio-imaging, and detection of ions and macromolecules.

Description

technical field [0001] The invention belongs to the fields of high value-added utilization of heavy oil and carbon nanometer material science, and relates to electrolytic preparation of petroleum coke-based carbon quantum dots and a nitrogen doping method. Using petroleum coke, a by-product of petroleum refining, as a raw material, petroleum pitch as a binder, and ethylenediamine or ammonia as a nitrogen doping agent, one-step preparation of nitrogen-doped carbon quantum dots with unique structure and good fluorescence properties by electrochemical oxidation , to realize the new high value-added utilization of petroleum coke, and this method provides a new way for the large-scale preparation of fluorescent nitrogen-doped carbon quantum dots. Background technique [0002] Carbon Quantum Dots (CarbonQuantumDots, CQDs) is a new fluorescent carbon nanomaterial with carbon as the skeleton structure discovered in 2004. It is a kind of dispersed quasi-spherical quasi-zero-dimension...

Claims

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Application Information

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IPC IPC(8): C09K11/65C25B3/00B82Y20/00B82Y40/00
Inventor 吴明铂饶袁王月谢辉马骁郑经堂吴文婷李忠涛
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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