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Nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material as well as preparation method and application of nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material

A technology of composite materials and oxidized rocks, which is applied in the new fields of environmental functional materials and water treatment, to achieve the effects of improving catalytic performance, facilitating the formation of single atoms, and easy separation and recycling

Pending Publication Date: 2022-07-01
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is: aiming at the technical problems existing in the prior art, develop a nitrogen-doped magnetic graphene oxide confining iron-cobalt bimetallic single atom that is highly efficient and easy to separate from solid and liquid and can be used to treat antibiotic pollutants composite material

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  • Nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material as well as preparation method and application of nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material
  • Nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material as well as preparation method and application of nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material
  • Nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material as well as preparation method and application of nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetallic monatomic composite material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) adopt Hummers method to prepare graphene oxide aqueous suspension, specifically comprises the following steps:

[0040] 6g graphite powder, 5gK 2 S 2 O 8 , 5gP 2 O 5 Add to 24 mL of 98% H 2 SO 4 , put it in a water bath with a triangular conical flask and stir, oxidize at 80°C for 4.5h, cool to room temperature, add 1L of ultrapure water to dilute and leave overnight for 12h to obtain mixture A;

[0041] The mixture A was filtered and rinsed with deionized water to neutralize the residual acid, and oven-dried at 60°C to obtain pre-graphite oxide;

[0042] Add pre-oxidized graphite to 240 mL 98% H 2 SO 4 In the solution, add 5g NaNO while stirring 3 , 30gKMnO 4 React at below 0°C for 4 hours, then raise the temperature to 35°C for 2 hours, add 500mL ultrapure water and react at 98°C for 1 hour, then continue to add 1L ultrapure water and 40mL 30% H at room temperature 2 O 2 , continue to react for two hours to obtain mixture B;

[0043] The obtained mixt...

Embodiment 2

[0054] The nitrogen-doped graphene oxide confined iron-cobalt bimetal single-atom composite material of the present invention treats tetracycline in wastewater, comprising the following steps:

[0055] 5 mg of the catalytic material D prepared in Example 1 was charged into a 250 mL glass bottle reactor containing 100 mL of tetracycline solution, and the reactor containing the mixture was shaken in a constant temperature shaker with a rotational speed of 150 rpm and 25°C. The adsorption-desorption equilibrium was reached within 30 minutes, then, 0.1 mol / L, 1-3 mL of persulfate (PDS) was added to initiate the degradation reaction, after 60 min, a 1 mL aliquot was taken and 1 mL of 0.1 mol / L Sodium thiosulfate was quenched and quickly collected into the sample bottle. The concentration of tetracycline was confirmed by high performance liquid chromatography. The calculated degradation efficiency results are shown in Table 1:

[0056] Table 1: Degradation efficiency data under diff...

Embodiment 3

[0061] The nitrogen-doped graphene oxide confined iron-cobalt bimetal single-atom composite material of the present invention treats tetracycline in wastewater, comprising the following steps:

[0062] 5 mg of MGO prepared in Example 1, catalytic materials I, E, F, H, G, D were charged into a 250 mL glass bottle reactor containing 100 mL of tetracycline solution, in a constant temperature shaker at 150 rpm and 25 °C. Shake the reactor containing the mixture. The adsorption-desorption equilibrium was reached within 30 min, then, 0.1 mol / L, 1 mL PDS was added to initiate the degradation reaction, after 60 min, a 1 mL aliquot was taken, immediately quenched with 1 mL 0.1 mol / L sodium thiosulfate, and Quickly collected into the sample bottle, the concentration of tetracycline was confirmed by high performance liquid chromatography, and the calculated degradation efficiency results are shown in Table 2; in the system without adding PDS, 5 mg of the catalytic material D prepared in ...

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Abstract

The invention relates to a nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetal monatomic composite material, a preparation method and application of the nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetal monatomic composite material. Graphene oxide serves as a base material of the composite material, firstly, the graphene oxide is magnetized through a coprecipitation method, and then the nitrogen-doped magnetic graphene oxide confinement iron-cobalt bimetal monatomic composite material is obtained; and then forming nitrogen vacancy defect anchored iron-cobalt bimetallic monoatoms on the magnetic graphene oxide in one step through a fused salt assisted high-temperature pyrolysis method. In the preparation process of the composite material, anchoring sites of monatomic iron and cobalt on graphene oxide are greatly increased by introducing nitrogen-containing groups, metal atom agglomeration can be reduced by applying molten salt to assist high-temperature pyrolysis, and a salt phase is easy to wash and recycle, environment-friendly and non-toxic. According to the prepared catalyst, loading of monatomic iron and cobalt on graphene oxide is greatly increased, and the obtained material is high in stability, can be easily separated from a solution, can be recycled, reduces the preparation cost and is economical and efficient. The product has a good degradation effect on tetracycline in wastewater.

Description

technical field [0001] The invention belongs to the field of environmental functional materials and new technologies for water treatment, in particular to a nitrogen-doped magnetic graphene oxide confined iron-cobalt bimetallic single-atom composite material, a preparation method and its application in antibiotic-contaminated water bodies. Background technique [0002] All along, antibiotics have been used in large quantities for the treatment of human and animal diseases and are added to animal feeds to prevent diseases and promote their growth. After the antibiotics are absorbed by the body, a small part of them undergoes metabolic reactions such as hydroxylation, cleavage and glucuronidation to form inactive products, while most of them enter the environment in the form of prototypes or metabolites, causing pollution to soil and water bodies. At present, antibiotic pollution has been listed as an important environmental problem by many countries. Therefore, it is necessa...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/03B01J37/08C02F1/72C02F101/34C02F101/38
CPCB01J27/24B01J37/035B01J37/082C02F1/722C02F1/725C02F2101/34C02F2101/345C02F2101/38C02F2305/023B01J35/40B01J35/33
Inventor 李美芳黄辰栖柴贝遐张美娟宋诗瑀胡琳严丽琴王平
Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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