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Method for preparing nitrogen-doped carbon material by utilizing fluorine-containing macromolecules

A nitrogen-doped carbon and polymer technology, applied in chemical instruments and methods, carbon preparation/purification, catalyst activation/preparation, etc., can solve problems such as difficult to control the type of nitrogen doping, to achieve environmental protection and waste Utilization, low cost, and mild reaction conditions

Active Publication Date: 2021-04-30
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally, this method can achieve graphitization of carbon materials at higher temperatures (>900°C), thereby achieving high conductivity of materials, but because nitrogen-doped carbon materials tend to lose nitrogen when they are higher than 750°C, Therefore, the nitrogen content of general nitrogen-doped carbon materials obtained by this method is difficult to exceed 7%, and it is difficult to control to obtain the desired nitrogen doping type

Method used

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  • Method for preparing nitrogen-doped carbon material by utilizing fluorine-containing macromolecules
  • Method for preparing nitrogen-doped carbon material by utilizing fluorine-containing macromolecules
  • Method for preparing nitrogen-doped carbon material by utilizing fluorine-containing macromolecules

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preparation example Construction

[0058] Preparation of mixed slurry. The fluorine-containing polymer precursor material and the solvent are mixed to obtain a mixed solution. The above-mentioned fluorine-containing polymer precursor material is a polymer whose relative molecular weight is between 10 million and 10 million, and part of hydrogen is replaced by fluorine. Wherein, the solvent is at least one selected from at least one of N-methylpyrrolidone, chloroform, water and ethanol. The concentration of the mixed solution may be 5-100 mg / mL. Preferably, a templating agent is also added to the mixed solution. The template agent is selected from at least one of mesoporous silica, molecular sieve, and magnesium oxide. The mass ratio of the template agent to the fluorine-containing polymer precursor material can be (0.1-5):1. After calcination, an etchant (an acid solution corresponding to the template agent) is used to remove the template agent.

[0059] Soak the conductive carbon felt in the obtained mixe...

Embodiment 1

[0065] Weigh 0.5g of polyvinylidene fluoride (PVDF) powder sample, spread evenly in the corundum porcelain boat, and then place it in the tube atmosphere furnace, then connect the two ends of the tube atmosphere furnace with special flanges and introduce ammonia The flow rate of ammonia gas is 300mL / min, and ammonia gas is fed continuously at this flow rate during the subsequent calcination process. The tail gas is absorbed by sulfuric acid solution to prevent air pollution. After ventilation at room temperature for at least 60 minutes, turn on the program heating, and then turn on the program heating at 20 The heating rate of ℃ / min is raised to 700 ℃, and then the heating is stopped after 4 hours of heat preservation, and the temperature is naturally lowered. After the temperature drops to room temperature, the ammonia gas is stopped and the argon gas with a flow rate of 300mL / min is passed in for at least 60 minutes. Stop, take out the corundum porcelain boat containing the p...

Embodiment 2

[0067] Weigh 0.5g of polyvinylidene fluoride-hexafluoropropylene (PVDF-HFP) powder sample, spread it evenly in a corundum porcelain boat, and then place it in a tube-type atmosphere furnace. The ammonia gas flow rate is 300mL / min, and the ammonia gas is continuously fed at this flow rate during the subsequent calcination process. The tail gas is absorbed by the sulfuric acid solution to prevent air pollution. After aeration at room temperature for at least 60 minutes Turn on the heating program, raise the temperature to 700°C at a heating rate of 20°C / min, then stop heating after holding the temperature for 4 hours, and let the temperature drop naturally. After the temperature drops to room temperature, stop feeding ammonia and feed argon with a flow rate of 300mL / min , stop after at least 60 minutes, take out the corundum porcelain boat containing the product to get black amorphous porous nitrogen-doped carbon material powder, the product has a nitrogen content of 10% and a sp...

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Abstract

The invention relates to a method for preparing a nitrogen-doped carbon material from fluorine-containing macromolecules, which comprises the following steps: putting a fluorine-containing macromolecule precursor material in an ammonia atmosphere, and calcining at 360-1200 DEG C to obtain the nitrogen-doped carbon material, wherein the fluorine-containing polymer precursor material is a polymer of which the relative molecular mass is 1,000 to 10,000,000 and part of hydrogen is substituted by fluorine. In this way, the nitrogen-doped carbon material can be obtained at a low temperature, and due to the fact that electron exchange of fluorine and nitrogen species can greatly promote doping of the nitrogen element, the nitrogen content of the nitrogen-doped carbon material obtained through the method can reach 10% or above. Besides, controllable doping of the nitrogen content and type on the conductive carbon felt can be realized by regulating and controlling the reaction temperature.

Description

technical field [0001] The present invention relates to a method for preparing nitrogen-doped carbon materials by utilizing fluorine-containing polymers, in particular to a new mechanism for utilizing fluorine-containing polymers to decompose by carbonization at high temperatures in an ammonia atmosphere to promote nitrogen doping And forming a porous structure so as to obtain a carbon material with a high nitrogen doping amount and a rich pore structure belongs to the field of material preparation. Background technique [0002] Nitrogen-doped carbon materials and their composites are functional materials with a wide range of uses and much attention, and are hot research materials in academia and industry. However, there are still many bottlenecks in its research that cannot be broken through: for example, the type of nitrogen in nitrogen-doped carbon materials has a great influence on its functionalization, but how to control the synthesis is still a problem; The limitatio...

Claims

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Application Information

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IPC IPC(8): C01B32/05D06M11/74H01G11/24H01G11/32H01M4/583H01M4/96B01J27/24B01J35/10D06M101/40
CPCC01B32/05D06M11/74B01J27/24B01J37/0018H01G11/24H01G11/32H01M4/583H01M4/96D06M2101/40B01J35/33B01J35/617B01J35/618B01J35/64Y02E60/10Y02E60/50
Inventor 黄富强董武杰
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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