A kind of method for preparing carbon-nitrogen airgel material based on alkali-thermal method

A gel material and nitrogen technology, applied in the field of nanomaterials, can solve the problems of complex preparation process of polymer crosslinking agent and increase the cost of use, and achieve the effect of promoting the surface chemical reaction rate, being easy to repeat, and having broad application prospects.

Active Publication Date: 2022-05-24
CHINA ACADEMY OF SPACE TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The cross-linking agent is generally a polymer material, which has a negative impact on the intrinsic properties of the airgel. In addition, the preparation process of the polymer cross-linking agent is relatively complicated, which increases the cost of use.

Method used

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  • A kind of method for preparing carbon-nitrogen airgel material based on alkali-thermal method
  • A kind of method for preparing carbon-nitrogen airgel material based on alkali-thermal method
  • A kind of method for preparing carbon-nitrogen airgel material based on alkali-thermal method

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preparation example Construction

[0033] The preparation method of the oxygen-doped carbon nitride aerogel photocatalyst proposed in the present invention, comprising the following steps:

[0034] (1) Bulk phase carbon nitride, hereinafter referred to as the preparation of BCN: dicyanamide and thiourea are mixed uniformly according to the mass ratio of (8 ~ 1): 1, and calcined in a muffle furnace. The heating procedure is 30 °C to 300 °C heating rate of 1 ~ 12 °C / min, 300 °C to 500 °C heating rate of 1 ~ 5 °C / min, 500 °C to 550 °C heating rate of 1 ~ 5 °C / min, and then 550 °C to maintain 1 ~ 6 hours, and finally natural cooling.

[0035] (2) Preparation of carbon and nitrogen aerogel based on sodium hydroxide alkali heat, hereinafter referred to as CNA-Na preparation: 0.1~1.5g BCN in 10~30mL of NaOH solution with a concentration of 1~4M maintain 40~80°C reflux stirring for 1~15h, take out ultrasound every 3~6 hours for one hour, wash and centrifuge, and let the sample stand for 15~30 hours to obtain a carbon...

Embodiment 1

[0039] Example 1, based on sodium hydroxide alkali heat preparation of carbon and nitrogen hydrogel

[0040] (1) Preparation of carbon nitride in the bulk phase, hereinafter referred to as BCN: dicyanamide and thiourea are mixed uniformly according to the mass ratio of 4:1 and calcined in a muffle furnace. The heating procedure is 30 °C to 300 °C heating rate of 8 °C / min, 300 °C to 500 °C heating rate of 2 °C / min, 500 °C to 550 °C heating rate of 1 °C / min, then 550 °C for 4 hours, and finally natural cooling.

[0041] (2) Preparation of carbon and nitrogen hydrogel based on sodium hydroxide alkali heat, hereinafter referred to as HNA-Na preparation: 0.5g BCN in 20mL concentration of 3M NaOH solution to maintain 60 °C reflux stirring for 10h, in the fifth hour at the time of ultrasonic one hour, wash centrifugation, the sample is left for 15 hours to obtain carbon nitrogen hydrogel HCN-Na.

[0042] as Figure 1 As shown, under alkaline thermal conditions, the hydroxyl groups of w...

Embodiment 2

[0043] Example 2, based on sodium hydroxide alkali heat preparation of carbon nitrogen aerogel

[0044] (1) Preparation of carbon nitride in the bulk phase, hereinafter referred to as BCN: dicyanamide and thiourea are mixed uniformly according to the mass ratio of 4:1 and calcined in a muffle furnace. The heating procedure is 30 °C to 300 °C heating rate of 8 °C / min, 300 °C to 500 °C heating rate of 2 °C / min, 500 °C to 550 °C heating rate of 1 °C / min, then 550 °C for 4 hours, and finally natural cooling.

[0045] (2) Preparation of carbon and nitrogen aerogel based on sodium hydroxide alkali heat, hereinafter referred to as CNA-Na preparation: 0.5g BCN in 20mL concentration of 3M NaOH solution to maintain 60 °C reflux stirring for 10h, in the fifth hour to take out the ultrasound for one hour, wash centrifugation, the sample is left for 15 to 30 hours after the yield of carbon and nitrogen hydrogel, referred to as HCN-Na. The above HCN-Na is freeze-dried, and the freeze-drying ...

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Abstract

The invention relates to a method for preparing a carbon-nitrogen airgel material based on an alkali-thermal method, and belongs to the technical field of nanometer materials. The method of the present invention prepares a carbon-nitrogen airgel material with a three-dimensional network structure through a simple alkali-thermal clipping and self-assembly process, and the preparation method is simple to operate, easy to repeat, and does not use additional support materials, providing a good solution for commercial applications. Technical basis and material guarantee. The carbon-nitrogen airgel material with a loose cotton-like structure prepared by the method of the present invention has a three-dimensional network structure and an open pore structure compared with the general bulk carbon nitride, and can expose more reaction sites, providing fast The mass transfer channel, and then the adsorption of pollutants or the promotion of the surface chemical reaction rate make the application prospect of the present invention in the fields of photocatalysis, electrocatalysis and pollutant adsorption very broad.

Description

Technical field [0001] The present invention relates to a method for preparing carbon nitrogen aerogel materials based on alkaline thermal method, belonging to the field of nanomaterial technology. Background [0002] The three-dimensional aerogel structure has the advantages of large specific surface area and exposed active sites, so it is widely used in photocatalysis, electrocatalysis and pollutant adsorption. However, most of the current carbon and nitrogen materials with a three-dimensional aerogel structure need to be constructed with the help of crosslinking agents. [0003] The crosslinker is generally a polymer material, which has a negative impact on the intrinsic properties of the aerogel, in addition, the preparation process of the polymer crosslinker is more complicated, which increases the cost of use. [0004] Therefore, it is important to develop a simpler and environmentally friendly method for constructing carbon and nitrogen three-dimensional aerogels. Content...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/00
CPCB01J13/0091
Inventor 姜文君姚伟
Owner CHINA ACADEMY OF SPACE TECHNOLOGY
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