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Nitrogen-sulfur co-doped porous graphitized carbon nanomaterial and preparation method thereof

A technology of carbon nanomaterials and nitrogen-sulfur co-doping, applied in chemical instruments and methods, nanotechnology, inorganic chemistry, etc., can solve the problems of harsh treatment process, low reuse rate, complex process, etc., and achieve low raw material cost, Improved removal ability and easy operation

Active Publication Date: 2022-07-29
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is little research on carbon nanomaterials doped with multiple non-metallic heteroatoms, and the low reuse rate of traditional non-metallic heteroatom-doped carbon nanomaterials is not conducive to the application
[0005] At present, due to the problems of complex process, high cost and even harsh treatment process, the actual synthesis of nitrogen and sulfur co-doped carbon nanomaterials still faces certain challenges. Therefore, the present invention has developed a nitrogen-sulfur co-doped medium with great potential and simplicity Porous carbon nanomaterials preparation method, and the removal of organic pollutants in the environment through the synergistic effect of adsorption and catalytic degradation

Method used

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  • Nitrogen-sulfur co-doped porous graphitized carbon nanomaterial and preparation method thereof
  • Nitrogen-sulfur co-doped porous graphitized carbon nanomaterial and preparation method thereof
  • Nitrogen-sulfur co-doped porous graphitized carbon nanomaterial and preparation method thereof

Examples

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Embodiment 1

[0034] This embodiment prepares a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial (NS-C-800), including the following steps:

[0035] Step 1. Take 20 g of thiourea as a raw material doped with nitrogen and sulfur in a ceramic crucible; then raise the temperature to 600°C at a heating rate of 5°C / min in a muffle furnace and calcinate for 4 hours to obtain powder A;

[0036] Step 2. Add 1.0 g of powder A and glucose obtained in step 1 into a mixed solution of acetic acid and dehydrated alcohol with a volume ratio of 1:5 according to a mass ratio of 2:1, wherein the acetic acid and dehydrated ethanol in the mixed solution The volumes are 1mL and 5mL respectively, fully ground, and dried naturally to obtain powder B;

[0037] Step 3. Put powder B obtained in step 2 in a tube furnace, and under the protection of nitrogen with a flow rate of 100 mL / min, firstly heat up to 550 °C at a rate of 2 °C / min, pyrolyze for 2 hours, and then heat at 2 °C / min. The rate of heat...

Embodiment 2

[0047] In this example, a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial (NS-C-700) was prepared. Compared with Example 1, the preparation method differed only in that the temperature of the second pyrolysis in step 3 was changed from 800°C was adjusted to 700°C, that is, firstly heated to 550°C at a rate of 2°C / min, pyrolyzed for 2h, then heated to 700°C at a rate of 2°C / min, further pyrolyzed for 2h; other steps remained unchanged.

[0048] According to as image 3 As shown in the BET test results, it can be seen that the average pore size of the obtained NS-C-700 is 2.0-50 nm, and the pore volume is 0.38 m 3 / g, the specific surface area is 217.20m 2 / g.

[0049] According to as Figure 5 The XRD pattern shown shows that the obtained NS-C-700 also has the structure of graphitized carbon at 2θ=26.3.

[0050] The NS-C-700 obtained in this example was tested for the removal performance of antibiotics in water by the same method as in Example 1. Image 6 I...

Embodiment 3

[0052] In this example, a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial (NS-C-600) is prepared. Compared with Example 1, the preparation method differs only in that the temperature of the second pyrolysis in step 3 is changed from 800°C was adjusted to 600°C, that is, the temperature was first heated to 550°C at a rate of 2°C / min, pyrolyzed for 2 hours, then heated to 600°C at a rate of 2°C / min, and further pyrolyzed for 2 hours; other steps remained unchanged.

[0053] According to as image 3 As shown in the BET test results, it can be seen that the average pore diameter of the obtained NS-C-600 is 2.0-50 nm, and the pore volume is 0.14 m 3 / g, the specific surface area is 31.96m 2 / g of NS-C-600.

[0054] According to as Figure 5 As shown in the XRD pattern, it can be seen that the obtained NS-C-600 has a clear diffraction peak at 2θ=27.7, indicating that C 3 N 4 , which may be due to its lower calcination temperature.

[0055] The NS-C-600 obtained...

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Abstract

The invention provides a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial and a preparation method thereof, belonging to the technical field of preparation of environmentally functional and friendly carbon materials. Porous graphitized carbon nanomaterials are graphitized carbon nanosheets with a porous structure with nitrogen groups and sulfur groups. The pores include mesopores of 2 to 50 nm and micropores with a pore size of less than 2 nm. The mass fraction of sulfur is 0.15% to 0.62. %, the atomic ratio of nitrogen to sulfur is (15-37):1. The preparation method is as follows: calcining thiourea at 400-600 DEG C for 2-6 hours, adding the obtained powder and glucose into a mixed solution of acetic acid and absolute ethanol, grinding and drying the obtained powder under protective gas, first at 500- Pyrolysis at 600℃ for 1~4h, and then pyrolysis at 600~800℃ for 2~5h. The present invention increases more active sites by incorporating nitrogen and sulfur heteroatoms into the carbon atom skeleton, thereby greatly improving the ability to remove organic pollutants in water.

Description

technical field [0001] The invention belongs to the technical field of preparation of environment-friendly functional carbon materials, in particular to a nitrogen-sulfur co-doped porous graphitized carbon nanomaterial and a preparation method thereof. Background technique [0002] In recent years, antibiotics and organic dyes have widely existed in various water bodies, which are difficult to biodegrade in the natural environment and can accumulate in the aquatic environment for a long time, causing great harm to the environment and human health. Therefore, how to quickly and effectively remove antibiotics and organic dyes from water has become a top priority. [0003] At present, adsorption, photocatalysis, advanced oxidation process (AOP), membrane separation, ion exchange and other technologies have been used to remove organic pollutants in wastewater. Among these technologies, adsorption technology is a promising technology for removing organic pollutants in wastewater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/205B82Y40/00C02F1/28C02F1/30C02F1/46C02F101/30
CPCC01B32/205B82Y40/00C02F1/283C02F1/30C02F1/46C02F2101/30
Inventor 陈文瑾朱科何红梅宾琼黄金何东东
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA