Preparation method of graphite phase carbonitride

A graphite-phase carbon nitride and graphite technology, which is applied in the direction of nitrogen and non-metallic compounds, can solve the problems of rapid heating of bulk phases that are difficult to exert microwave irradiation, low power, and influence on preparation efficiency, etc., and achieves controllable structure and properties, The effect of simple preparation process and simple raw materials

Active Publication Date: 2016-07-13
ZHANGJIAGANG DONGDA IND TECH RES INST +1
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Problems solved by technology

[0006] At present, some people have used microwave method to prepare carbon nitride materials, but due to the limitation of microwave equipment, knowledge system and application field, the application of high energy microwave technology is not widespread enough.
The common microwave heating equipment is a household microwave oven, the power is generally low (300-1000W), and the preparation efficiency and effect are not ideal.
Yuan Yupeng and others from Anhui University (Yuan Yupeng, Qiu Lingguang, Xu Gengsheng, Peng Fumin, Xu Wentao, Ma Lin, rapid preparation of graphite-like structure

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  • Preparation method of graphite phase carbonitride
  • Preparation method of graphite phase carbonitride
  • Preparation method of graphite phase carbonitride

Examples

Experimental program
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Effect test

Embodiment 1

[0055] 10g melamine (C 3 h 6 N 6 ) and 2g of graphite powder were ground and mixed evenly. The mixture is then placed in a ceramic crucible and placed in a resonant cavity of an industrial high-energy microwave oven. Vacuumize the resonant cavity of the microwave oven to 5kPa, then turn on the microwave, and start to keep warm after the temperature reaches 450°C. At this time, the microwave power is about 2kW. After 5 minutes, turn off the microwave oven, let the reaction system cool down to room temperature with the furnace, and then take out the sample. A large amount of bright yellow powder can be seen in the crucible.

[0056] The structure of the bright yellow powder obtained after microwave irradiation was characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy, and it was confirmed that the product was pure graphite phase carbon nitride, and the product was pure, with a yield of about 46wt%.

[0057] figure 1 It is the...

Embodiment 2

[0060] Weigh the same two-component raw materials in Example 1 and move them into a ceramic crucible after thorough mixing. After placing the crucible in an industrial high-energy microwave resonator, start vacuuming to 5kPa. Turn on the microwave again, set the microwave irradiation power to 3kW, start to keep warm after the temperature reaches 550°C, turn off the microwave after 10min, let the reaction system cool down to room temperature with the furnace, and take out the yellow sample. Through the analysis of X-ray diffraction and scanning electron microscope characterization adopted in Example 1, it can be proved that the obtained yellow product is graphite phase carbon nitride. Because the microwave power is increased, the heating temperature is higher, the color of the obtained graphite phase carbon nitride is deepened, and the yield is about 41wt%.

[0061] The X-ray diffraction pattern of the product shows that a (100) diffraction peak appears at the position of 13.3...

Embodiment 3

[0064] The two-component raw materials in Example 1 were weighed and thoroughly mixed, then transferred into a ceramic crucible and placed in a resonant cavity of an industrial high-energy microwave oven. Evacuate the resonant cavity of the microwave oven to a vacuum of 10kPa. Turn on the microwave, set the microwave irradiation power to 3kW, start to keep warm after the temperature reaches 550°C, turn off the microwave after 20min, let the reaction system cool down to room temperature with the furnace, and take out the dark yellow sample. Through the characterization analysis such as X-ray diffraction and scanning electron microscopy adopted in Example 1, it can be proved that the dark yellow product obtained is graphite phase carbon nitride. Due to the further extension of the holding time, the color of the graphitic carbon nitride changed to dark yellow, and the yield was 39wt%.

[0065] The X-ray diffraction pattern of the product shows that a (100) diffraction peak appears...

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Abstract

The invention discloses a preparation method of graphite phase carbonitride. A preparation process comprises the following steps of using nitrogen-rich organic matters are raw materials; graphite or silicon carbide is used as a microwave absorption agent; the nitrogen-rich organic matters and the microwave absorption agent are uniformly mixed; in a microwave radiation electromagnetic field, the pressure is controlled to be 5 to 35 kPa, the microwave radiation power is 2 to 10 kW, the temperature rise speed is controlled to be 50 to 500 DEG C/min, and the heat insulation reaction is performed for 5 to 30 min at 450 to 700 DEG C; the graphite phase carbonitride is obtained. The method is based on a high-energy microwave radiation treatment method; the graphite phase carbonitride in a layered structure can be fast and efficiently obtained; the method is simple and efficient; the cost is low; varies kinds of expansive or environment-harmful reagents such as catalysts, organic solvents and protection gas are not used. The method has the advantages that the environment-friendly effect is achieved; the raw material pretreatment is not needed, and the like. The method belongs to a green preparation method favorable for large-scale business production.

Description

technical field [0001] The invention relates to the technical field of preparation of graphite-phase carbon nitride, in particular to a preparation method for rapidly obtaining graphite-phase carbon nitride based on high-energy microwave irradiation heating technology. Background technique [0002] Finding alternative new clean energy to solve the energy crisis and environmental pollution in the world today has always been one of the most important tasks and missions in the scientific community. Among them, semiconductor photocatalysts can convert non-polluting, non-toxic and inexhaustible solar energy into chemical energy, or directly degrade organic pollutants, showing great potential in solving energy crisis and environmental pollution. Graphite phase carbon nitride is a new type of semiconductor optical functional material, due to its low density, thermal stability, suitable band gap, excellent acid and alkali resistance, unique electronic energy band structure, optical ...

Claims

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Application Information

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IPC IPC(8): C01B21/082
CPCC01B21/082C01P2002/72C01P2004/03C01P2004/04
Inventor 王继刚余永志张浩周清张安蕾顾永攀
Owner ZHANGJIAGANG DONGDA IND TECH RES INST
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