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Preparation method of nitrogen-manganese co-doped hierarchical porous carbon material

A co-doping and multi-level pore technology, which is applied in the preparation/purification of carbon, hybrid capacitor electrodes, etc., can solve the problems of cumbersome and time-consuming preparation steps, high toxicity of raw material reagents, expensive template agents, etc., and achieve reliable material structure and performance. control, the reaction process is easy to control, and the effect of simple steps

Active Publication Date: 2021-07-13
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a preparation method with high specific capacity and good speed for the problems of cumbersome and time-consuming preparation steps of nitrogen-doped carbon materials, expensive templating agent used, high toxicity of raw material reagents, and low nitrogen content. A method for nitrogen-manganese co-doped hierarchical porous carbon materials with high capacity, low electrolyte transport resistance and excellent cycle stability

Method used

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  • Preparation method of nitrogen-manganese co-doped hierarchical porous carbon material
  • Preparation method of nitrogen-manganese co-doped hierarchical porous carbon material
  • Preparation method of nitrogen-manganese co-doped hierarchical porous carbon material

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Example 1: Preparation of a nitrogen-manganese co-doped hierarchical porous carbon material

[0039] Follow the steps below:

[0040] (1) Preparation of oligomeric phenolic resin Resol

[0041] Add 1.0 g of phenol and 2.5 mL of 40% formaldehyde solution to 4 mL of 0.5 M NaOH solution, and stir at 65° C. for 0.7 h to obtain the oligomeric phenolic resin Resol.

[0042] (2) Preparation of hierarchically porous carbon bulk materials co-doped with nitrogen and manganese oxide

[0043] 0.6g P123 (EO 20 PO 70 EO 20 ), 1.1g F127 (EO 106 PO 70 EO 106 ), 0.05g melamine, added to the above-mentioned oligomeric phenolic resin Resol, stirred at 65°C for 4h, after cooling to room temperature, added 0.05g MnCl 2 4H 2 O, continue stirring at 65°C for 3h, transfer the obtained solution to a hydrothermal kettle, heat at 100°C for 18h, filter out the obtained block material, wash repeatedly with distilled water, dry in vacuum at 50°C for 24h, and then transfer to a tube furnace ...

Embodiment 2

[0052] Electrochemical impedance spectroscopy was used to study the transport resistance of the N-MnO-HPCM material, and the Nyquist curve was as follows Figure 8 As shown, the inset is the Nyquist curve of the N-MnO-HPCM material in the high frequency region. The intercept of the semicircle on the horizontal axis is the equivalent series resistance (Rs), which is 0.34Ω, which represents the sum of the resistance from the electrolyte and the active material, and the contact resistance between the active material and the current collector, which is relatively small , indicating that the supercapacitor has good rate capacity or power density. The diameter of the semicircle corresponds to the charge transfer resistance at the electrode-electrolyte interface, which is 0.14Ω, indicating that the N-MnO-HPCM material has a lower charge transfer resistance and higher conductivity. The Nyquist curve is close to a straight line in the low frequency region, showing ideal capacitive beh...

Embodiment 3

[0063] Example 3: Preparation of a nitrogen-manganese co-doped hierarchical porous carbon material

[0064] Follow the steps below:

[0065] (1) Preparation of oligomeric phenolic resin Resol

[0066] Add 1.0 g of phenol and 3.5 mL of 39% formaldehyde solution into 5 mL of 0.5 M NaOH solution, and stir at 65° C. for 0.7 h to obtain the oligomeric phenolic resin Resol.

[0067] (2) Preparation of hierarchically porous carbon bulk materials co-doped with nitrogen and manganese oxide

[0068] Add 0.85g P123, 1.15g F127, 0.5g urea to the above oligomeric phenolic resin Resol, stir at 70°C for 3h, cool to room temperature, add 0.4g MnCl 2 4H 2 O, continue stirring at 70°C for 2h, transfer the obtained solution to a hydrothermal kettle, heat at 120°C for 15h, filter out the obtained block material, wash repeatedly with distilled water, dry in vacuum at 60°C for 15h, and then transfer to a tube furnace Under the protection of nitrogen gas, it was calcined at 700°C for 4h, and aft...

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Abstract

The invention discloses a preparation method of a nitrogen-manganese co-doped hierarchical porous carbon material, which comprises the following steps: (1) preparation of an oligomeric phenolic resin: dissolving phenol and formaldehyde in an alkali solution, heating and stirring to obtain the product; (2) Preparation of hierarchically porous carbon block material co-doped with nitrogen and manganese: Add template agents P123 and F127 and nitrogen-containing compounds to the oligomeric phenolic resin prepared in step (1), stir at 65-75°C for 2- 4h, after cooling to room temperature, add manganese salt, continue to stir at 65-75°C for 0.5-3h, transfer the resulting solution to a hydrothermal kettle for hydrothermal reaction, filter out the bulk material, wash and dry it, and place it under the protection of an inert gas Calcining at 550-800°C for 1.5-5 hours, cooling to room temperature, and obtaining a hierarchical porous carbon block material co-doped with nitrogen and manganous oxide. The prepared carbon materials have high specific capacity, good rate capacity, low electrolyte transport resistance and excellent cycle stability.

Description

technical field [0001] The invention relates to a preparation technology of a novel carbon material, in particular to a preparation method of a nitrogen-manganese co-doped hierarchical porous carbon material. Background technique [0002] Supercapacitor is a new type of green energy storage device, which has the advantages of fast charging and discharging speed, high efficiency, long cycle life, wide temperature range, high safety, and no pollution to the environment. It is used in fuel cell vehicles, hybrid electric vehicles , buses, low-temperature starting of vehicles, solar system power storage devices, high-power fast charging power supplies, etc. have very broad application prospects. Electrode materials are the key factors determining the performance of supercapacitors. Porous carbon materials have the advantages of low price, good electrochemical stability, large specific surface area and pore volume, and are the preferred electrode materials for supercapacitors. H...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05H01G11/32H01G11/46
CPCC01P2004/03C01P2004/04C01P2006/12C01P2006/14C01P2006/16C01P2006/40H01G11/32H01G11/46Y02E60/13
Inventor 刘玉荣胡荣
Owner CHONGQING UNIV OF ARTS & SCI
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