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Preparation method and application of Z-type carbon nitride-iron oxide catalyst containing nitrogen defect structure

A defect structure, catalyst technology, applied in physical/chemical process catalysts, ammonia preparation/separation, chemical instruments and methods, etc., to achieve the effect of good photocatalytic nitrogen fixation and ammonia production and simple operation.

Active Publication Date: 2021-02-19
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the N-N triple bond in the N2 molecule is very stubborn, the most challenging problem in the photocatalytic nitrogen fixation process is the adsorption and activation of the N2 molecule on the catalyst surface.

Method used

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  • Preparation method and application of Z-type carbon nitride-iron oxide catalyst containing nitrogen defect structure
  • Preparation method and application of Z-type carbon nitride-iron oxide catalyst containing nitrogen defect structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A nitrogen-containing defect structure Z-type g-C 3 N x / Fe 2 o 3 The preparation method of catalyst, comprises the steps:

[0032] (1) Disperse 5 g of urea in 50 mL of sodium hydroxide solution (0.5 mol / L), stir for 30 min, dry at 60°C for 12 h, then cool to room temperature, grind into powder and collect for later use.

[0033] (2) Mix and grind 5g of the above-mentioned urea / sodium hydroxide mixture with 0.5g ferric oxalate, add it into the crucible, put it into the muffle furnace, and heat it at 10 ℃·min -1 Raise the temperature to 150 °C, after heating for 1 h, at 10 °C min -1 Raise the temperature to 450 °C, heat for 1 hour, then cool down to room temperature, grind into powder, wash with water, centrifuge and dry to prepare the nitrogen-containing defect structure Z-type photocatalyst g-C 3 N x -0.1 / Fe 2 o 3 -0.1.

[0034] Under normal temperature and pressure conditions, add 50 mg of g-C to 500 mL methanol aqueous solution (0.001 mol / L) 3 N x -0.1 / Fe ...

Embodiment 2

[0036] A nitrogen-containing defect structure Z-type g-C 3 N x / Fe 2 o 3 The preparation method of catalyst, comprises the steps:

[0037] (1) Disperse 10 g of melamine in 50 mL of potassium hydroxide solution (0.5 mol / L), stir for 30 min, dry at 60°C for 12 h, then cool to room temperature, grind into powder and collect for later use.

[0038] (2) Mix and grind 5g of the above-mentioned melamine / potassium hydroxide mixture and 1g of ferrous oxalate, add it into the crucible, put it into the muffle furnace, and heat it at 10 ℃·min -1 Raise the temperature to 200 °C, after heating for 2 h, at 10 °C min -1 The temperature was raised to 500 °C, heated for 2 h, then cooled to room temperature by program cooling, ground into powder, washed with water, centrifuged and dried to prepare the nitrogen-containing defect structure Z-type photocatalyst g-C 3 N x -0.2 / Fe 2 o 3 -0.2.

[0039] Under normal temperature and pressure conditions, add 100 mg of g-C to 500 mL methanol aque...

Embodiment 3

[0041] A nitrogen-containing defect structure Z-type g-C 3 N x / Fe 2 o 3 The preparation method of catalyst, comprises the steps:

[0042] (1) Disperse 25g of melamine in 50mL of ammonia solution (0.5 mol / L), stir for 30min, dry at 60°C for 12h, then cool to room temperature, grind into powder and collect for later use.

[0043] (2) Mix and grind 5g of the above-mentioned melamine / ammonia water mixture and 1.5g of ferrous oxalate into the crucible, put it into the muffle furnace, and heat it at 10 ℃·min -1 Raise the temperature to 350 °C, after heating for 2 h, at 10 °C min -1 The temperature was raised to 530 °C, heated for 3 h, then cooled to room temperature by program cooling, ground into powder, washed with water, centrifuged and dried to prepare the nitrogen-containing defect structure Z-type photocatalyst g-C 3 N x -0.5 / Fe 2 o 3 -0.3.

[0044] Under normal temperature and pressure conditions, add 100 mg of g-C to 500 mL methanol aqueous solution (0.001 mol / L) ...

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Abstract

The invention discloses a preparation method and application of a Z-type carbon nitride-iron oxide catalyst containing a nitrogen defect structure, belongs to the technical field of photocatalytic material synthesis, and relates to modification of graphite-type carbon nitride (g-C3Nx) containing a nitrogen defect structure and preparation of the Z-type carbon nitride-iron oxide photocatalyst (g-C3Nx / Fe2O3) containing a nitrogen defect structure by compounding graphite-type carbon nitride with iron oxide (Fe2O3). The preparation method comprises the following steps of: taking urea, melamine orthiourea as a carbon nitride precursor; taking ammonia water, sodium hydroxide, potassium hydroxide or barium hydroxide and other alkalis as auxiliary materials; and taking iron oxalate, ferrous oxalate, ferrous sulfate and the like as iron sources, heating for 2-8 hours at 250-650 DEG C through a one-step roasting method, cooling to the room temperature through programmed cooling, grinding the reaction product into powder, washing the powder with water, and carrying out centrifuging and drying to obtain the catalyst. The preparation method is simple to operate, a nitrogen defect structure isintroduced into conventional g-C3N4 to prepare g-C3Nx, the g-C3Nx and ferric salt are synchronously roasted to compound Fe2O3, and the catalyst is applied to photocatalytic nitrogen fixation for ammonia production. Experimental results show that the prepared catalyst has good photocatalytic nitrogen fixation and ammonia production performance, has a popularization effect on photocatalytic green synthesis ammonia, and is energy-saving and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of synthesis of photocatalytic materials, and relates to photoresponsive catalysts, in particular to graphite-type carbon nitride (g-C 3 N x ) modification, and composite iron oxide (Fe 2 o 3 ) to prepare a Z-type carbon nitride-iron oxide photocatalyst (g-C 3 N x / Fe 2 o 3 ) and its application in visible light catalytic nitrogen fixation. Background technique [0002] Ammonia is the foundation of modern industry and agriculture, and also one of the important carriers of clean energy. With the increasing demand for ammonia, the research on the synthesis of ammonia by artificial nitrogen fixation has received extensive attention. At present, the Haber-Bosch method, which is mainly used for artificial nitrogen fixation, needs to react and synthesize ammonia under the conditions of high temperature 300-550 ℃ and high pressure 15-25 MPa. This method has the disadvantages of high energy consumption and l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/00C01C1/02
CPCB01J27/24C01C1/026B01J35/39Y02P20/52Y02P20/50Y02P20/10
Inventor 荣新山张仕贤荣坚周向同吴智仁
Owner JIANGSU UNIV
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