A kind of preparation method of doped graphitic carbon nitride material

A technology of carbon nitride and graphite, applied in the field of preparation of graphitic carbon nitride, can solve the problems of limiting the performance of graphite carbon nitride materials, no photocatalytic activity, low photocatalytic activity, etc., and is convenient for large-scale industrialization. The effect of producing, improving photocatalytic activity, and high photocatalytic activity

A technology of carbon nitride and graphite, applied in the field of preparation of graphitic carbon nitride, can solve the problems of limiting the performance of graphite carbon nitride materials, no photocatalytic activity, low photocatalytic activity, etc., and is convenient for large-scale industrialization. The effect of producing, improving photocatalytic activity, and high photocatalytic activity

CN110813343BActive Publication Date: 2020-12-01SHANGHAI JIAOTONG UNIV
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  • A kind of preparation method of doped graphitic carbon nitride material
  • A kind of preparation method of doped graphitic carbon nitride material
  • A kind of preparation method of doped graphitic carbon nitride material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] After grinding 10g of urea evenly, put it into a ceramic crucible; after grinding 10mg of copper acetylacetonate evenly, put it into a quartz boat; place the quartz boat with copper acetylacetonate in a ceramic crucible; put the ceramic crucible into In the muffle furnace, the reaction pressure is 1MPa, the heating rate is 5°C / min to 550°C, and then the temperature is kept for 4 hours. After the reaction system is cooled to room temperature with the furnace, the light yellow sample is taken out.

[0033] The structure of the obtained light yellow sample was characterized by X-ray diffraction pattern.

[0034] figure 1 is the X-ray diffraction pattern of the resulting product, which can prove that the modified sample still has a graphite-like layered carbon nitride, that is, graphite-like carbon nitride.

[0035] figure 2 It is a transmission electron microscope picture of the obtained product. It can be seen from the figure that the modified carbon nitride has a lame...

Embodiment 2

[0063] This example is a modification example of Example 1, which only involves changing the calcination temperature and holding time: specifically, in the steps of Example 1, the ceramic crucible is placed in the muffle furnace, and the temperature is raised to 450 °C at a heating rate of 5 °C / min After ℃, start to keep warm, and keep warm for 6 hours. Other steps and test conditions remain unchanged, and the measured hydrogen production rate is 320umol / h.

Embodiment 3

[0065] This embodiment is a modification of embodiment 1, which only involves changing the calcination temperature and holding time: specifically, in the steps of embodiment 1, the ceramic crucible is placed in the muffle furnace, and the temperature is raised to 550 °C at a heating rate of 5 °C / min. After ℃, start to keep warm and keep warm for 2 hours. Other steps and test conditions remain unchanged, and the measured hydrogen production rate is 270umol / h.

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Abstract

The invention discloses a method for preparing doped graphite-like carbon nitride materials; using metal organic matter with sublimation or low boiling point characteristics (such as acetylacetone complex, bis(2,2,6,6-tetramethyl-3 , 5-heptanedione) copper, bis(hexafluoroacetylacetonate) copper, ferrocene, copper formate, metal carbonyl compound) in the polycondensation process of graphite carbon nitride nitrogen-rich precursor, metal ions and anions gas phase Co-doping control; during the heating and polycondensation process, the precursors of metal organic salts and graphite carbon nitride are partitioned, the control pressure is 0.1-20MPa, the heating rate is 1-30℃ / min, and the temperature is maintained at 450-600℃ for 2- 6h, the graphite carbon nitride is obtained. This method is based on a gas-phase co-doping method, which can efficiently and quickly obtain doped graphite-like carbon nitride with a hierarchical pore structure; the obtained material is highly active in the photocatalytic decomposition of water and the catalytic degradation of organic matter.

Description

technical field [0001] The present invention relates to the preparation of graphite-phase carbon nitride, in particular to a one-step preparation method for gas-phase doping of metal-organic salts based on sublimation characteristics and regulation and control of modified graphite-like carbon nitride materials, which is used for photocatalytic technology to decompose water to produce hydrogen, Photocatalytic decomposition of organic pollutants such as VOC, S-VOC in the field. Background technique [0002] In today's society, among the many ways to seek renewable energy, photocatalytic technology is considered to be one of the most promising technologies for converting sunlight energy into hydrogen energy, and it also provides a feasible idea for solving environmental problems. Graphite carbon nitride, as a non-metallic n-type semiconductor polymer, has many excellent electrical, optical and physicochemical properties. Photocatalysts based on graphitic carbon nitride have at...

Claims

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Application Information

Patent Timeline
01 Dec 2020
Publication
CN110813343B
IPC
B01J27/24; B01J35/00; B01D53/86; B01D53/72
CPC
B01J27/24; B01D53/8668; B01J35/39; Y02A50/20
Inventors
江治; 戚荣杰