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Nitrogen-doped mesoporous carbon catalyst for sewage degradation and its preparation method and application

A nitrogen-doped mesoporous carbon and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, water/sewage treatment, etc., can solve the problems of small surface area, uncontrollable structure of nitrogen-doped carbon materials, etc., to achieve The preparation method is simple and the steps are economical

Inactive Publication Date: 2017-02-15
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, under template-free conditions, the pyrolysis of irregular structure precursors cannot control the structure of nitrogen-doped carbon materials, and the resulting nitrogen-doped carbon materials usually have microporous structures with small surface areas.

Method used

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  • Nitrogen-doped mesoporous carbon catalyst for sewage degradation and its preparation method and application
  • Nitrogen-doped mesoporous carbon catalyst for sewage degradation and its preparation method and application
  • Nitrogen-doped mesoporous carbon catalyst for sewage degradation and its preparation method and application

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Embodiment 1

[0038] This embodiment provides a method for preparing a nitrogen-doped mesoporous carbon catalyst for sewage degradation, which includes the following steps:

[0039] Preparation of nitrogen-containing ligand 2,3-dimethyl-1,4-bis(4'-nitrobenzoic acid)butadiene:

[0040] Dissolve 57.6 g of 4-aminophenyl acid (420 mmol) in 100 mL of methanol (MeOH), add 80 drops of anhydrous formic acid, then add dropwise 17.6 mL (200 mmol) of 2,3-butanedione (dissolved in 100 mL of MeOH) , followed by stirring at room temperature for 24h; the precipitated precipitate was washed with cold MeOH at 5°C and dried in the air to obtain a light yellow powder nitrogen-containing ligand 2,3-dimethyl-1,4-bis(4'-nitrobenzoic acid ) butadiene (labeled L') with a yield of 21.8%.

[0041] Preparation of nitrogen-doped mesoporous carbon catalysts for sewage degradation:

[0042] 30mmol Zn(NO 3 ) 2 ·6H 2 O (9.0g) and 10mmol (3.25g) of ligand L' were dissolved in 50mL DMF under stirring conditions. When a...

Embodiment 2

[0051] This embodiment provides a method for preparing a nitrogen-doped mesoporous carbon catalyst for sewage degradation, which includes the following steps:

[0052] Preparation of nitrogen-doped mesoporous carbon catalysts for sewage degradation:

[0053] Dissolve 30mmol of zinc nitrate tetrahydrate and 10mmol of ligand L' in 600mL of DEF to form a uniform solution, add 15mL of triethylamine dropwise, then stir at room temperature for 1h, obtain a solid product by filtration, and then use the above solid product Wash slowly with 50-75mL DEF followed by 55mL CHCl 3 Exchange for 24 hours, repeat three times, and vacuum dry at 80°C for 5 hours to obtain nitrogen-containing zinc metal-organic framework powder (NZnMOF);

[0054] Put the NZnMOF powder obtained above in a quartz boat, raise the temperature to 910°C at a rate of 2°C / min in a nitrogen atmosphere, and then carbonize at 910°C for 4 hours in a nitrogen atmosphere to obtain a nitrogen-doped mesoporous carbon catalyst f...

Embodiment 3

[0056] This embodiment provides a method for preparing a nitrogen-doped mesoporous carbon catalyst for sewage degradation, comprising the following steps:

[0057] Dissolve 20mmol of zinc chloride and 10mmol of ligand L' in 100mL of DMAC, stir at room temperature for 0.5h, and filter to obtain a solid product, then slowly wash the above solid product with 50-75mL of DMAC, and then wash it with 60mL of CHCl 3 Exchange for 24 hours, repeat three times, and vacuum dry at 80°C for 8 hours to obtain nitrogen-containing zinc metal-organic framework powder (NZnMOF);

[0058] Put the NZnMOF powder obtained above in a quartz boat, raise the temperature to 980°C at a rate of 15°C / min in a nitrogen atmosphere, and then carbonize at 980°C for 2 hours in a nitrogen atmosphere to obtain a nitrogen-doped mesoporous carbon catalyst for sewage degradation , denoted as MNC-3.

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Abstract

The invention provides a preparation method of a nitrogen-doped mesoporous carbon catalyst for wastewater degradation. The preparation method comprises the following steps: zinc salt and nitrogen-containing ligand at the mole ratio of (1:1) to (5:1) are dissolved in an organic solvent to form a homogeneous solution, 5-20 mL of triethylamine is added into the solution dropwise, the solution is stirred for 0.5-3 h and filtered to obtain a solid product, and the solid product is subjected to washing, solvent exchange and vacuum drying to obtain powder of metal-organic frameworks containing nitrogen and zinc; the powder of metal-organic frameworks containing nitrogen and zinc is heated in a nitrogen atmosphere to be greater than or equal to 910 DEG C at the speed of 2-20 DEG C / min, and the temperature is kept for 1-12 h, and then is reduced to the room temperature, so that the catalyst is obtained. The invention further provides the nitrogen-doped mesoporous carbon catalyst for wastewater degradation, which is prepared by the preparation method, and application of the catalyst to wastewater degradation. The catalyst does not contain metals, has a low nitrogen content and a larger specific surface area, is easy in preparation method and economic in step, and can efficiently degrade 4-nitrophenol in wastewater.

Description

technical field [0001] The invention provides a nitrogen-doped mesoporous carbon catalyst for sewage degradation and a preparation method and application thereof, which relate to the technical field of chemical engineering, in particular to the technical field of functionalized carbon nanomaterials. Background technique [0002] Sewage treatment has great and far-reaching significance for environmental protection and sustainable development. The reduction of 4-nitrophenol, an organic pollutant in agricultural or industrial wastewater, to 4-aminophenol can not only reduce environmental pollution, but also turn waste into treasure, and provide raw materials for the production of fine chemicals such as aniline and paracetamol. [0003] However, the catalysts currently used for the reduction of 4-nitrophenol are mainly noble metal or doped noble metal catalysts such as Au, Pd, Ag, PtNi, AuCu, and PdCu. Although these noble metal catalysts have high activity, their high cost and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/10C02F1/58
Inventor 杨英李新松张雯张鑫
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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