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Preparation method of porous carbon material with high thermal-oxidative stability and regular pore structure

A porous carbon material and pore structure technology, which can be used in the preparation/purification of carbon, chemical instruments and methods, carbon compounds, etc., can solve the problems of disordered pore structure, poor thermal and oxygen stability, etc. The effect of improved oxygen stability and adjustable specific surface area

Pending Publication Date: 2020-02-14
UNIV OF SCI & TECH OF CHINA
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Problems solved by technology

[0004] The present invention aims at the disadvantages of poor thermal oxygen stability and disordered pore structure of traditional porous carbon materials, and provides a preparation method of porous carbon materials with high thermal oxygen stability and regular pore structure, and prepares heteroelement-doped carbon materials by high-temperature calcination. Porous carbon material with excellent thermo-oxidative stability and regular pore structure

Method used

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  • Preparation method of porous carbon material with high thermal-oxidative stability and regular pore structure
  • Preparation method of porous carbon material with high thermal-oxidative stability and regular pore structure
  • Preparation method of porous carbon material with high thermal-oxidative stability and regular pore structure

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Embodiment 1

[0027] 1. Using 25mmol of acetic acid as a catalyst, dissolve 10mmol of pyroglucinol and 15mmol of p-phenylenediamine in 10mL of 1,4-dioxane, react in vacuum at 120°C for 3 days, filter with suction and wash with acetone, 150 ℃ vacuum drying to obtain COFs.

[0028] 2. COFs (1.0 g) were annealed at 450° C. for 30 minutes under argon protection to prepare nitrogen-doped porous carbon (Ncarbon). COFs (0.3g) and B 2 o 3 (3g) was annealed at 300°C for 30min (BNcarbon1), 450°C for 30min (BNcarbon 2), 450°C for 50min (BNcarbon 3), 450°C for 90min (BN carbon 4) and 600°C for 30min (BNcarbon 5) Porous carbon doped with boron and nitrogen is obtained.

[0029] figure 1 It is the thermogravimetric curve of the nitrogen-doped and boron-nitrogen-doped porous carbon materials in Example 1 under air conditions. Depend on figure 1 Known, N carbon in 10wt% mass loss (T 10wt％ ) under the temperature of 386.7 ° C, at 50wt% mass loss (T 50wt％ ) is 493.0°C, the temperature at the peak val...

Embodiment 2

[0033] 1. Using 12.5 mmol of acetic acid as a catalyst, dissolve 15 mmol of terephthalaldehyde and 10 mmol of melamine in 10 mL of dimethyl sulfoxide, react in vacuum at 180°C for 3 days, filter with suction, wash with acetone, and dry in vacuum at 150°C to obtain COFs.

[0034] 2. COFs (1.0 g) were annealed at 600° C. for 30 minutes under argon protection to prepare nitrogen-doped porous carbon. The mixture of COFs (0.3 g) and phosphoric acid (3 g) was annealed at 300 °C for 30 min, 450 °C for 30 min, 600 °C for 30 min and 750 °C for 30 min to obtain phosphorus and nitrogen doped porous carbon.

Embodiment 3

[0036] 1. With 25mmol of acetic acid as a catalyst, 20mmol of 1,3,5-benzenetriboronic acid and 10mmol of 2,3,6,7,10,11-hexahydroxybiphenyl were dissolved in 8mL of 1,4-dioxane, 120 ℃ vacuum reaction for 3 days, suction filtration and washing with acetone, vacuum drying at 100 ℃ to obtain COFs.

[0037] 2. COFs (1.0 g) were annealed at 600° C. for 30 minutes under argon protection to prepare boron-doped porous carbon. The mixture of COFs (0.3 g) and melamine (1.5 g) was annealed at 300 °C for 30 min, 450 °C for 30 min, 600 °C for 30 min and 750 °C for 30 min to obtain boron and nitrogen doped porous carbon.

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Abstract

The invention discloses a preparation method of a porous carbon material with high thermal-oxidative stability and a regular pore structure. Aiming at the defects of poor thermal-oxidative stability and disordered pore structures of traditional porous carbon materials, the hetero-element-doped porous carbon material with excellent thermal-oxidative stability and the regular pore structure is prepared by a high-temperature calcination method, so that the application range of the traditional carbon-based materials in a high-temperature environment can be further expanded.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and in particular relates to a preparation method of a porous carbon material with high thermal oxygen stability and regular pore structure. Background technique [0002] Carbon materials such as graphene, carbon fibers, and carbon / carbon composites have attracted much attention due to their applications in the fields of electrodes, catalysts, friction components, flame retardants, and mechanical reinforcements. However, the shortcoming of insufficient thermal-oxidative stability limits the application of carbon-based materials in high-temperature environments. So far, strategies to improve the thermal oxidation resistance of carbon materials mainly include: heat treatment, coating treatment and chemical doping. Among them, the chemical doping method is the most effective treatment method. In 2014, S. Sandoval et al. reported a nitrogen-doped graphene oxide in Chemistry-A European Jour...

Claims

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Application Information

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IPC IPC(8): C01B32/00C01B32/05
CPCC01B32/00C01B32/05
Inventor 牧小卫阚永春宋磊胡源
Owner UNIV OF SCI & TECH OF CHINA
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