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CN-121990557-A - Nitrogen-sulfur co-doped porous carbon, electrode material, preparation method and application thereof

CN121990557ACN 121990557 ACN121990557 ACN 121990557ACN-121990557-A

Abstract

The invention belongs to the technical field of functional materials, and particularly relates to nitrogen-sulfur co-doped porous carbon, an electrode material and a preparation method and application thereof, wherein macadamia nut shell powder, sodium sulfide nonahydrate and melamine are added into water and uniformly mixed, hydrothermal reaction is carried out for 8-10 hours at 180-190 ℃, hydrothermal products are collected, the hydrothermal products are calcined for 1-2 hours at 600-800 ℃ in a nitrogen protective atmosphere, the nitrogen-sulfur co-doped porous carbon is obtained, the ratio of macadamia nut shell powder to sodium sulfide nonahydrate to melamine to water is 1-3 g to 1.5-2 g to 50-70 mL, and through independent regulation and control of a nitrogen source and a sulfur source, the number of active sites of the electrode material is increased, the adsorption capacity and electrochemical response performance of the material to Cd 2+ and Pb 2+ are improved, and high-sensitivity detection of low concentration Cd 2+ and Pb 2+ is realized.

Inventors

  • LI HUIYU
  • YANG YIKAI
  • ZHANG DANDAN

Assignees

  • 山西科技学院
  • 聊城大学

Dates

Publication Date
20260508
Application Date
20260306

Claims (8)

  1. 1. The preparation method of the nitrogen-sulfur co-doped porous carbon is characterized by adding macadamia nut shell powder, sodium sulfide nonahydrate and melamine into water, uniformly mixing, performing hydrothermal reaction at 180-190 ℃ for 8-10 hours, collecting a hydrothermal product, and calcining the hydrothermal product at 600-800 ℃ for 1-2 hours under the protection of nitrogen to obtain the nitrogen-sulfur co-doped porous carbon; The macadamia nut shell powder, sodium sulfide nonahydrate melamine to water ratio 1-3 g, 1-2 g, 1.5-1.5 g and 50-70 mL.
  2. 2. A nitrogen-sulfur co-doped porous carbon prepared by the method of claim 1.
  3. 3. Use of the nitrogen-sulfur co-doped porous carbon of claim 2 in the preparation of an electrode material.
  4. 4. An electrode material is characterized in that the electrode material is obtained by uniformly mixing the nitrogen-sulfur co-doped porous carbon, the perfluorinated sulfonic acid resin and the ethanol, dripping the mixture on the surface of an electrode substrate, and drying and curing the mixture; the ratio of the nitrogen-sulfur co-doped porous carbon, the perfluorinated sulfonic acid resin and the ethanol is 3 mg-5 mg, 4 mu L-6 mu L and 994 mu L-996 mu L.
  5. 5. The use of the electrode material of claim 4 in the detection of Cd 2+ and Pb 2+ in a body of water.
  6. 6. The application of claim 5, wherein during detection, the electrode material is used as a working electrode in a three-electrode system, a supporting electrolyte and a water body sample to be detected are added into an electrolytic cell, detection is carried out through square wave anodic stripping voltammetry, enrichment potential is firstly applied to complete adsorption enrichment of heavy metal ions, then a stripping voltammetry curve is recorded through potential scanning, a calibration curve is established by utilizing a linear relation between characteristic oxidation peak current and heavy metal ion concentration, and quantitative detection of Cd 2+ and Pb 2+ in the water body sample to be detected is realized.
  7. 7. The use according to claim 6, wherein the reference electrode in the three-electrode system is a silver/silver chloride electrode and the counter electrode is a platinum electrode.
  8. 8. The use according to claim 6, wherein the supporting electrolyte is acetic acid-sodium acetate buffer solution.

Description

Nitrogen-sulfur co-doped porous carbon, electrode material, preparation method and application thereof Technical Field The invention belongs to the technical field of functional materials, and particularly relates to a nitrogen-sulfur co-doped porous carbon, an electrode material, a preparation method and application thereof. Background Currently, methods for detecting Cd 2+ and Pb 2+ in water mainly comprise Atomic Absorption Spectrometry (AAS), inductively coupled plasma mass spectrometry (ICP-MS), high Performance Liquid Chromatography (HPLC) and the like. Although the method has the advantages of high detection precision, strong anti-interference capability and the like, the method has the defects of expensive equipment, complex operation flow, long detection period, need of operation of professional technicians and the like, and is difficult to meet the requirements of on-site rapid detection and large-scale water environment screening. The electrochemical detection technology has the unique advantages of high sensitivity, high response speed, portability of instruments, low cost, simple and convenient operation and the like, and becomes a research hot spot for on-site detection of heavy metal ions in water. The core of the electrochemical detection technology is electrode materials, and the performance of the electrode materials directly determines the sensitivity, selectivity and stability of detection. In recent years, carbon-based electrode materials (such as graphene, carbon nanotubes, biomass carbon and the like) are widely applied to the field of heavy metal ion electrochemical detection due to the characteristics of high specific surface area, good conductivity, strong chemical stability and the like. The biomass charcoal takes agricultural wastes as raw materials, has the advantages of wide sources, extremely low cost, environmental friendliness and the like, accords with the environment-friendly concept of treating waste with waste, and becomes one of the preferred directions of the carbon-based electrode material. However, the single biomass charcoal has the problems of few electrochemical active sites, limited heavy metal ion adsorption capacity and the like, so that the detection sensitivity is insufficient, and the detection requirements of low-concentration Cd 2+ and Pb 2+ are difficult to meet. In order to improve the performance, researchers often adopt a method of doping hetero atoms (nitrogen, sulfur, phosphorus and the like), and the electronic structure of the carbon material is regulated and controlled by introducing the hetero atoms, so that active sites are increased, and the adsorption capacity and electrochemical response performance to heavy metal ions are improved. The co-doping synergistic effect of the nitrogen atom and the sulfur atom is particularly remarkable, wherein the lone pair electrons of the nitrogen atom can form coordination action with heavy metal ions, and the electronegativity of the sulfur atom can enhance the adsorption affinity of the material to the heavy metal ions. However, the existing nitrogen-sulfur co-doped biomass charcoal has the defects that the single precursor simultaneously provides N, S and the doping amount of N, S cannot be regulated and controlled independently, so that the regulation and control flexibility of the type and the number of active sites is insufficient, the material performance is unstable, and the high-sensitivity detection of Cd 2+ and Pb 2+ in water is difficult to realize. Disclosure of Invention In order to solve the technical problems, the invention provides a nitrogen-sulfur co-doped porous carbon, an electrode material, a preparation method and application thereof. Adding macadamia nut shell powder, sodium sulfide nonahydrate and melamine into water, uniformly mixing, performing hydrothermal reaction at 180-190 ℃ for 8-10 h, collecting a hydrothermal product, and calcining the hydrothermal product at 600-800 ℃ for 1-2h under the protection of nitrogen to obtain the nitrogen-sulfur co-doped porous carbon; The macadamia nut shell powder, sodium sulfide nonahydrate melamine to water ratio 1-3 g, 1-2 g, 1.5-1.5 g and 50-70 mL. In the preparation method, through independent regulation and control of a nitrogen source and a sulfur source and combination of a porous structure, the number of active sites of an electrode material is increased, the adsorption capacity and electrochemical response performance of the material to Cd 2+ and Pb 2+ are improved, and high-sensitivity detection of low-concentration Cd 2+ and Pb 2+ is realized. The nitrogen-sulfur co-doped porous carbon prepared by the preparation method. The nitrogen-sulfur co-doped porous carbon is applied to the preparation of electrode materials. The electrode material is prepared by uniformly mixing the nitrogen-sulfur co-doped porous carbon, perfluorinated sulfonic acid resin and ethanol, dripping the mixture on the surface of an electrode substrate, and drying a