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Preparation method of doped graphite-like carbon nitride material

A technology of graphite-like carbon nitride and graphite, which is applied in the field of preparation of graphite-phase carbon nitride, can solve the problems of limiting the performance of graphite-like carbon nitride materials, cumbersome preparation process, and small specific surface area, so as to facilitate large-scale industrial production, High photon quantum efficiency and wide range of raw material sources

Active Publication Date: 2020-02-21
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the graphitic carbon nitride material prepared by traditional pyrolysis of nitrogen-rich organic matter has a small specific surface area, low photocatalytic activity, and almost no photocatalytic activity in the near-infrared region.
[0005] However, the existing methods for preparing doped and modified graphitic carbon nitride materials often have complicated steps, and it is difficult to realize the co-doping control of metal cations and anions, which limits the doping and modification of graphitic carbon nitride materials. Material properties
For example, the bimetallic ion-doped graphitic carbon nitride material mentioned in the patent CN105214709B requires a series of complex steps such as dissolving, stirring, drying, grinding and mixing, and fails to realize the co-doping regulation of metal cations and anions
Another example is the preparation method of inorganic ion-doped carbon nitride photocatalyst mentioned in the patent CN103301867A. The preparation process is also relatively cumbersome, and only the doping of specific ions is considered, and the co-doping regulation of metal cations and anions cannot be realized.

Method used

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  • Preparation method of doped graphite-like carbon nitride material
  • Preparation method of doped graphite-like carbon nitride material
  • Preparation method of doped graphite-like carbon nitride material

Examples

Experimental program
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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 preparation method of a doped graphite-like carbon nitride material. Metallorganics such as acetylacetone complexes, bis(2,2,6,6-tetramethyl-3,5-heptanedionato)copper(II), bis(hexafluoroacetoacetonato)copper, ferrocene, copper formate and metal carbonyls with sublimation or low-boiling-point characteristics are adopted to be subjected to metal ion and anion gas-phase co-doping control in a condensation polymerization process of nitrogen-rich precursors of graphite-like carbon nitride; and in a heating condensation polymerization process, organometallic salts and the precursors of the graphite-like carbon nitride are partitioned, pressure is controlled to be 0.1-20 MPa, the heating rate is 1-30 DEG C / min, thermal insulation is performed for 2-6 h at 450-600 DEG C,and graphite-like carbon nitride is obtained. According to the method, the doped graphite-like carbon nitride with a hierarchical porous structure can be efficiently and rapidly obtained on the basisof a gas-phase co-doping method; and the obtained material has quite high activity on photocatalytic decomposition of water and 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

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IPC IPC(8): B01J27/24B01J35/00B01D53/86B01D53/72
CPCB01J27/24B01D53/8668B01J35/39Y02A50/20
Inventor 江治戚荣杰
Owner SHANGHAI JIAO TONG UNIV