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Sulfur-doped crystal carbon nitride for photocatalytic decomposition of water to produce hydrogen and preparation method and application thereof

A technology of sulfur doping and carbon nitride, which is applied in the field of photocatalytic materials, can solve the problems of small specific surface area of ​​crystalline carbon nitride, wide band gap, and limitation of photocatalytic hydrogen production activity, so as to achieve increased sulfur content and narrow band gap , The effect of reducing the duration of molten salt calcination

Pending Publication Date: 2021-03-12
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystalline carbon nitride obtained by the above method has shortcomings such as small specific surface area and wide band gap, which limit the improvement of photocatalytic hydrogen production activity.

Method used

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  • Sulfur-doped crystal carbon nitride for photocatalytic decomposition of water to produce hydrogen and preparation method and application thereof
  • Sulfur-doped crystal carbon nitride for photocatalytic decomposition of water to produce hydrogen and preparation method and application thereof
  • Sulfur-doped crystal carbon nitride for photocatalytic decomposition of water to produce hydrogen and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Weigh 2g of thiocyanic acid and disperse it into 80ml of deionized water, stir at room temperature for 30min, then transfer the dispersion to a 100ml hydrothermal kettle, seal and react at 120°C for 4h, and cool to room temperature after the reaction; Suction filter the product, and freeze-dry the resulting filter cake at -40°C to obtain a precursor;

[0041] (2) Place the precursor in a tube furnace, calcinate at 550°C for 4 hours in a flowing argon atmosphere, and then naturally cool to room temperature to obtain sulfur-doped carbon nitride; the volume space velocity of argon is 2 minutes –1 ;

[0042] (3) The obtained sulfur-doped carbon nitride and molten salt were mixed uniformly by grinding, the mixture was placed in a tube furnace, and calcined at 550°C for 40min under a flowing argon atmosphere; after that, the sample was quickly taken out of the furnace and Rapidly cool to room temperature under the protection of inert gas, wash away excess molten salt wit...

Embodiment 2

[0044] (1) Weigh 1g of thiocyanic acid and 1g of melamine and disperse it into 80ml of deionized water, stir at room temperature for 40min, then transfer the dispersion to a 100ml hydrothermal kettle, seal it and react at 140°C for 2h, cool down after the reaction to room temperature; then the product was filtered with suction, and the resulting filter cake was freeze-dried at -40°C to obtain a precursor;

[0045] (2) Place the precursor in a tube furnace, calcinate at 550°C for 4 hours in a flowing argon atmosphere, and then naturally cool to room temperature to obtain sulfur-doped carbon nitride; the volume space velocity of argon is 2 minutes –1 ;

[0046] (3) The obtained sulfur-doped carbon nitride and molten salt were mixed uniformly by grinding, the mixture was placed in a tube furnace, and calcined at 550°C for 40min under a flowing argon atmosphere; after that, the sample was quickly taken out of the furnace and Rapidly cool to room temperature under the protection o...

Embodiment 3

[0048] (1) Weigh 2g of thiocyanuric acid and disperse it into 80ml of deionized water, stir at room temperature for 30min, then transfer the dispersion to a 100ml hydrothermal kettle, seal and react at 100°C for 3h, and cool to room temperature after the reaction; Suction filter the product, and freeze-dry the resulting filter cake at -40°C to obtain a precursor;

[0049] (2) Place the precursor in a tube furnace, calcinate at 550°C for 4 hours in a flowing argon atmosphere, and then naturally cool to room temperature to obtain sulfur-doped carbon nitride; the volume space velocity of argon is 2 minutes –1 ;

[0050] (3) The obtained sulfur-doped carbon nitride and molten salt were mixed evenly by grinding, the mixture was placed in a tube furnace, and calcined at 550°C for 90min under a flowing argon atmosphere; after that, the sample was quickly taken out of the furnace and Rapidly cool to room temperature under the protection of inert gas, wash away excess molten salt with...

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Abstract

The invention discloses sulfur-doped crystal carbon nitride for photocatalytic decomposition of water into hydrogen as well as a preparation method and application of the sulfur-doped crystal carbon nitride, and belongs to the technical field of photocatalytic materials. The preparation method comprises the following steps: by taking trithiocyanuric acid or a mixture of trithiocyanuric acid and melamine as a raw material, carrying out hydrothermal freeze drying to pre-polymerize reactants, calcining to obtain sulfur-doped carbon nitride, and carrying out short-time molten salt treatment to obtain the sulfur-doped crystal carbon nitride. According to the method, heteroatom doping and crystallization modification means are combined, so that sulfur atoms are fixed in a carbon-nitrogen networkthrough hydrothermal freeze-drying prepolymerization, sulfur volatilization can be effectively reduced through short-time molten salt treatment, and sulfur doping is achieved on the basis that crystal carbon nitride is obtained. The sulfur-doped crystal carbon nitride is small in forbidden band width and large in specific surface area, wherein the photocatalytic hydrogen production activity is remarkably higher than that of crystal carbon nitride, sulfur-doped carbon nitride and bulk-phase carbon nitride. In addition, fused salt calcination time is remarkably shortened, and energy conservation is improved.

Description

technical field [0001] The invention belongs to the technical field of photocatalytic materials, and in particular relates to a sulfur-doped crystalline carbon nitride used for photocatalytic decomposition of water to produce hydrogen, a preparation method and application thereof. Background technique [0002] With the continuous advancement of industrialization, energy crisis and environmental pollution have become two major problems restricting the development of human society. Solar energy is an ideal renewable energy source, but solar energy itself has a low energy density and is difficult to use directly. Photocatalytic decomposition of water to produce hydrogen through photocatalytic materials can convert solar energy into clean hydrogen energy with high energy density. One of the ideal measures for puzzles. [0003] Since it was first applied to the field of photocatalysis in 2009, carbon nitride materials have attracted extensive attention from researchers due to th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10B01J37/10B01J37/08C01B21/082C01B3/04
CPCB01J27/24B01J37/10B01J37/082C01B21/0605C01B3/042C01P2002/72C01P2004/04C01P2002/84C01P2006/12B01J35/615B01J35/39Y02P20/10Y02E60/36
Inventor 李伟魏可欣关庆鑫邹芳
Owner NANKAI UNIV
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