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Preparation method of g-C3N4/C composite material containing nitrogen vacancy

A composite material, g-c3n4 technology, applied in the field of photocatalytic materials and nitrogen reduction synthesis of ammonia, can solve the problem of less nitrogen vacancies on the surface, and achieve the effects of high production efficiency, low price and short cycle

Pending Publication Date: 2020-05-15
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the problem with this preparation method is that the experiment requires two-step pyrolysis and a nitrogen atmosphere, and the obtained surface nitrogen vacancies are less

Method used

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  • Preparation method of g-C3N4/C composite material containing nitrogen vacancy
  • Preparation method of g-C3N4/C composite material containing nitrogen vacancy
  • Preparation method of g-C3N4/C composite material containing nitrogen vacancy

Examples

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Embodiment 1

[0030] This embodiment is g-C containing nitrogen vacancies 3 N 4 / C composite preparation process. Such as Figure 6 As shown, the following steps are included: Weigh 4.85g of melamine, add 0.15g of citric acid monohydrate into 40ml of absolute ethanol, place in a planetary ball mill to fully disperse at a speed of 300r / min, and ball mill for 12h. The emulsion was transferred to a beaker, and dried in an oven at 80° C. for 12 hours to obtain a uniformly dispersed melamine precursor. Grind the bulk precursor into powder in a mortar, take 3g and transfer it to an alumina crucible, place it in an atmosphere furnace, raise it to 550°C at a rate of 2°C / min, keep it warm for 2h, and then cool down naturally. Sonicate in deionized water for 1 h, and then dry in an oven at 80 °C for 24 h.

[0031] g-C of nitrogen vacancies prepared according to Example 1 3 N 4 / C composite material can be seen after scanning by X-ray diffractometer figure 1 , g-C 3 N 4 g-C can be clearly see...

Embodiment 2

[0033] This example is used to illustrate the g-C of nitrogen vacancies 3 N 4 / C composite preparation process. Such as Figure 6 As shown, the following steps are included: Weigh 4.65g of melamine, add 0.35g of citric acid monohydrate into 40ml of absolute ethanol, place in a planetary ball mill to fully disperse at a speed of 300r / min, and ball mill for 12h. The emulsion was transferred to a beaker, and dried in an oven at 80° C. for 12 hours to obtain a uniformly dispersed melamine precursor. Grind the bulk precursor into powder in a mortar, take 3g and transfer it to an alumina crucible, place it in an atmosphere furnace, raise it to 550°C at a rate of 2°C / min, keep it warm for 2h, and then cool down naturally. Sonicate in deionized water for 1 h, and then dry in an oven at 80 °C for 24 h.

[0034] g-C of nitrogen vacancies prepared according to Example 2 3 N 4 / C composite material by N 2 -The temperature rise desorption curve of nitrogen obtained after the TPD tes...

Embodiment 3

[0036] This example is used to illustrate the use of oxyacids in g-C 3 N 4 Versatility of methods for constructing nitrogen defects on surfaces. Such as Figure 6As shown, the following steps are included: Weigh 4.65g of melamine, add 0.35g of adipic acid into 40ml of absolute ethanol, place in a planetary ball mill to fully disperse at a speed of 300r / min, and ball mill for 12h. The emulsion was transferred to a beaker, and dried in an oven at 80° C. for 12 hours to obtain a uniformly dispersed melamine precursor. Grind the bulk precursor into powder in a mortar, take 3g and transfer it to an alumina crucible, place it in an atmosphere furnace, raise it to 550°C at a rate of 2°C / min, keep it warm for 2h, and then cool down naturally. Sonicate in deionized water for 1 h, and then dry in an oven at 80 °C for 24 h.

[0037] g-C of nitrogen vacancies prepared according to Example 3 3 N 4 / C composite material observed by transmission electron microscope, see image 3 , it ...

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Abstract

The invention discloses a preparation method of a g-C3N4 / C composite material containing nitrogen vacancy, wherein the preparation method comprises the following steps: mixing oxyacid and a melamine precursor with absolute ethyl alcohol, dispersing by planetary ball milling, drying an obtained sample, and grinding to obtain a catalyst precursor; calcining the precursor in a tubular furnace, and grinding an obtained sample to obtain the g-C3N4 / C composite material containing the nitrogen vacancy. The prepared g-C3N4 / C composite material containing the nitrogen vacancy has excellent catalytic performance on a photocatalytic nitrogen fixation reaction. Compared with the prior art, the preparation method provided by the invention is wide in raw material source, simple in preparation process and high in catalyst nitrogen vacancy content, and the photocatalytic nitrogen fixation efficiency can be effectively improved.

Description

technical field [0001] The invention relates to the field of photocatalytic materials and nitrogen reduction synthesis ammonia, in particular to a g-C containing nitrogen vacancies 3 N 4 / C composite material preparation method. Background technique [0002] The traditional industrial method of nitrogen fixation, the Haber-Bosch process, consumes 1% of the world's energy supply and produces 2.3 tons of greenhouse gases each year. So far, the hydrogen used in the synthesis of ammonia is mainly through methane steam reforming. It can be seen that this process is complex in operation, harsh in conditions, and consumes a lot of energy. Therefore, the heterogeneous photocatalytic nitrogen fixation strategy imitating biological nitrogenase is a promising method for nitrogen fixation. [0003] Photocatalytic nitrogen fixation requires sufficient energy to break the N≡N bond, while the introduction of surface defects can effectively reduce the activation energy required to open t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C01C1/04
CPCB01J27/24C01C1/0411B01J35/39Y02P20/52
Inventor 曲虹霞崔健魏新宇
Owner NANJING UNIV OF SCI & TECH
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