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A kind of preparation method of carbon nitride fluffy microsphere with high catalytic activity

A high catalytic activity, carbon nitride technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problem of rapid acquisition and large-scale application of zero-dimensional carbon nitride The carbon nitride size is small, the preparation process is complicated, etc., and the effect of high practical value, inhibition of agglomeration, and simple synthesis process is achieved.

Active Publication Date: 2021-12-10
ZHANGJIAGANG DONGDA IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the size of zero-dimensional carbon nitride is very small, the agglomeration phenomenon is serious, and the preparation process is very complicated, and the yield is very low, which is not conducive to the rapid acquisition and large-scale application of zero-dimensional carbon nitride.

Method used

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  • A kind of preparation method of carbon nitride fluffy microsphere with high catalytic activity
  • A kind of preparation method of carbon nitride fluffy microsphere with high catalytic activity
  • A kind of preparation method of carbon nitride fluffy microsphere with high catalytic activity

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Effect test

Embodiment 1

[0027] Put 5 g of melamine into 70 mL of sulfuric acid solution with a concentration of 0.5 mol / L, ultrasonically disperse it for 30 min, then transfer it to a 100 mL hydrothermal kettle and heat it at 180°C for 8 h, and cool it down to room temperature naturally; collect the white precipitate by suction filtration and use deionized Wash with water three times, dry overnight at 80°C, and grind into powder, which is the precursor; put the precursor into a ceramic crucible, cover the crucible and place it in the center of the muffle furnace cavity, and slowly heat up at a rate of 2°C / min Raise the temperature to 550°C and keep it warm for 4 hours, then open the furnace door and cool down to room temperature naturally to obtain fluffy carbon nitride microspheres.

[0028] figure 1 SEM images of carbon nitride fluffy microspheres under different magnifications, figure 1 a It can be seen that the size of the microspheres is relatively uniform, showing a fluffy spherical or ellipso...

Embodiment 2

[0033] Put 5 g of melamine into 70 mL of sulfuric acid solution with a concentration of 1.0 mol / L, ultrasonically disperse it for 30 min, then transfer it to a 100 mL hydrothermal kettle and heat it at 180°C for 8 h, then cool it down to room temperature naturally; collect the white precipitate by suction filtration and use deionized Wash with water three times, dry overnight at 60°C, and grind into powder, which is the precursor; put the precursor into a ceramic crucible, cover the crucible and place it in the center of the muffle furnace cavity, and slowly heat up at a rate of 2°C / min Raise the temperature to 550°C and keep it warm for 4 hours, then open the furnace door and cool down to room temperature naturally to obtain fluffy carbon nitride microspheres. The diameter of the microsphere is about 8 μm, and the specific surface area is 203.6m 2 / g, the photocatalytic first-order kinetic constant is 0.614min -1 .

Embodiment 3

[0035] Put 5 g of melamine into 70 mL of sulfuric acid solution with a concentration of 2.0 mol / L, ultrasonically disperse it for 30 min, then transfer it to a 100 mL hydrothermal kettle and heat it at 120°C for 8 h, and cool it to room temperature naturally; collect the white precipitate by suction filtration and use deionized Wash with water three times, dry overnight at 40°C, and grind into powder, which is the precursor; put the precursor into a ceramic crucible, cover the crucible and place it in the center of the muffle furnace cavity, and slowly heat up at a rate of 2°C / min Raise the temperature to 550°C and keep it warm for 4 hours, then open the furnace door and cool down to room temperature naturally to obtain fluffy carbon nitride microspheres. The diameter of the microsphere is about 14μm, and the specific surface area is 152.3m 2 / g, the photocatalytic first-order kinetic constant is 0.457min -1 .

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Abstract

The invention discloses a method for preparing fluffy carbon nitride microspheres with high catalytic activity, which is characterized in that it comprises the following steps: (1) taking nitrogen-containing organic matter powder as raw material, acidifying with sulfuric acid, hydrothermally treating, washing and drying Obtaining the precursor; (2) Put the precursor into a ceramic crucible, cover the crucible and place it in the center of the muffle furnace cavity, and calcinate at high temperature to obtain carbon nitride fluffy microspheres. Carbon nitride fluffy microspheres are composed of carbon nitride nanosheets connected with a diameter of about 10 μm. Compared with traditional bulk carbon nitride, it can significantly improve the specific surface area and mass transfer, and has efficient photodegradation under visible light. Organic pollutant performance. The method uses wide sources of raw materials and simple operation process, and can prepare carbon nitride fluffy microspheres with high specific surface area and high catalytic activity in large quantities.

Description

technical field [0001] The invention relates to the technical field of carbon nitride nanometer material preparation, in particular to a preparation method of carbon nitride fluffy microspheres with high catalytic activity. Background technique [0002] Carbon nitride is a man-made compound composed of C element, N element and trace H element. As early as 1996, Teter and Hemley proposed through theoretical calculations that carbon nitride may have five crystal phases: α phase, β phase, cubic phase, quasi-cubic phase and graphite phase (Science, 1996.271:53). Graphite phase carbon nitride is named for its graphite-like layered structure. It is the only soft phase among the five crystal phases, and it is also the most stable crystal phase at room temperature. The C and N atoms in the graphitic carbon nitride sheet are sp 2 Hybridized and arranged alternately, connected by σ bonds to form a hexagonal structure, p z The lone pair of electrons on the orbital form a large π bon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/08B01J35/10C02F1/30C02F101/30
Inventor 王继刚徐奇楠乔坤吴珊
Owner ZHANGJIAGANG DONGDA IND TECH RES INST
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