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CN-121990620-A - Preparation method and application of nitrogen-sulfur co-doped modified layered double oxide material

CN121990620ACN 121990620 ACN121990620 ACN 121990620ACN-121990620-A

Abstract

The invention discloses a preparation method of a nitrogen-sulfur co-doped modified layered double oxide material, which belongs to the technical field of water treatment and comprises the following steps of (1) pretreating and drying a carbon felt substrate, putting the treated substrate into a uniform solution containing Fe (NO 3 ) 3 ·9H 2 O and Ni (NO 3 ) 2 ·6H 2 O), carrying out hydrothermal reaction, taking out the substrate after completion, carrying out ultrasonic treatment and washing with deionized water to obtain a NiFe-LDH precursor, (2) drying the obtained precursor, immersing the dried precursor into an ethanol solution of ammonium persulfate, and then carrying out high-temperature carbonization treatment under an inert gas atmosphere to obtain the nitrogen-sulfur co-doped modified nickel-iron layered double oxide material.

Inventors

  • CHEN ZHEN
  • Xie Zuoju
  • LI HUIXI
  • ZHU WEI
  • LI SHUTING
  • DU BINGQIAN
  • YU QIANG

Assignees

  • 昆明理工大学

Dates

Publication Date
20260508
Application Date
20260116

Claims (8)

  1. 1. A preparation method of a nitrogen-sulfur co-doped modified layered double oxide material is characterized by comprising the following steps: (1) Pretreating and drying a carbon felt substrate, placing the treated substrate into a uniform solution containing Fe (NO 3 ) 3 ·9H 2 O and Ni (NO 3 ) 2 ·6H 2 O) for hydrothermal reaction, taking out after the reaction is finished, and drying after ultrasonic treatment and deionized water washing to obtain a NiFe-LDH precursor; (2) And drying the obtained precursor, immersing the dried precursor in an ethanol solution of ammonium persulfate, and then carrying out high-temperature carbonization treatment under the protection of inert gas atmosphere to finally prepare the nitrogen-sulfur co-doped modified ferronickel layered double oxide material.
  2. 2. The preparation method of the nitrogen-sulfur co-doped modified layered double oxide material is characterized in that in the step (1), the carbon felt substrate is immersed in sulfuric acid solution, absolute ethanol solution and deionized water in sequence and subjected to ultrasonic treatment for 15 minutes respectively, wherein the concentration of the sulfuric acid solution is 0.5-1.5mol/L.
  3. 3. The method of claim 1, wherein in the step (1), 1mmol Fe (NO 3 ) 3 ·9H 2 O and 1-3mmol Ni (NO 3 ) 2 ·6H 2 O) are added to 10mL deionized water to form a uniform solution.
  4. 4. The method for preparing the nitrogen-sulfur co-doped modified layered double oxide material according to claim 3, wherein in the step (1), the hydrothermal reaction temperature is 120-180 ℃ and the time is 6-12 hours.
  5. 5. The method for preparing the nitrogen-sulfur co-doped modified layered double oxide material according to claim 1, wherein in the step (2), the concentration of the ethanol solution of ammonium persulfate is 2.5-10mmol/L, and the time for immersing the precursor in the ethanol solution of ammonium persulfate is 6-12h.
  6. 6. The method for preparing a nitrogen-sulfur co-doped modified layered double oxide material according to claim 1, wherein in the step (2), the high-temperature carbonization treatment is carried out at a temperature of 500-700 ℃ for a holding time of 1-3h.
  7. 7. The method for preparing a nitrogen-sulfur co-doped modified layered double oxide material according to claim 1, wherein in the step (2), the inert gas is nitrogen or argon.
  8. 8. The application of the nitrogen-sulfur co-doped modified nickel-iron layered double oxide material prepared by the preparation method according to any one of claims 1-7 in water treatment is characterized in that the nitrogen-sulfur co-doped modified nickel-iron layered double oxide material is used as a cathode, a graphite plate is used as an anode, and the nitrogen-sulfur co-doped modified nickel-iron layered double oxide material is used for removing heavy metals Cr (VI) and p-nitrophenol in water.

Description

Preparation method and application of nitrogen-sulfur co-doped modified layered double oxide material Technical Field The invention relates to the technical field of water treatment materials, in particular to a preparation method and application of a nitrogen-sulfur co-doped modified layered double oxide material. Background Along with the rapid development of industrialization, the problem of the combined pollution of heavy metals and organic pollutants in water bodies is increasingly severe, and serious threat is formed to ecological environment and human health. Among them, hexavalent chromium (Cr (VI)) is the key point for heavy metal pollution control due to its high toxicity and carcinogenicity, while paranitrophenol (PNP) is a typical organic pollutant which is difficult to degrade, has stable chemical properties and has bioaccumulation. In industrial wastewater, the two pollutants often exist at the same time, and development of the method capable of synchronously and efficiently removing the two pollutants is of great significance. At present, although each of the methods for treating a single type of contaminant has advantages, there are limitations. The Capacitive Deionization (CDI) and the electro-Fenton technology are coupled, so that functional complementation of ion adsorption and pollutant degradation can be realized, and synchronous removal of the ion adsorption and the pollutant degradation is facilitated. The key to achieving this coupling system is the development of high performance electrode materials. At present, noble metals and oxides (such as Pt and IrO 2、RuO2) have excellent catalytic performance but high cost, carbon materials have lower cost but limited catalytic activity, and non-noble metal catalysts such as transition metal-based phosphides, sulfides and Layered Double Hydroxides (LDH) are attracting attention because of low cost and adjustable structure. However, the existing LDH materials still generally have the problems of poor conductivity, insufficient exposure of active sites, low structural stability and the like, which limit the application of the LDH materials in water treatment. Disclosure of Invention In order to solve the problems in the related art, the invention provides a preparation method and application of a nitrogen-sulfur co-doped modified layered double oxide material, wherein the preparation method can improve the conductivity of the obtained composite material, promote the exposure and stability of active sites, and further realize the efficient and synchronous removal of Cr (VI) and PNP. In order to achieve the aim, the technical scheme of the invention is to provide a preparation method of a nitrogen-sulfur co-doped modified layered double oxide material, which is characterized by comprising the following steps: (1) Pretreating and drying a carbon felt substrate, placing the treated substrate into a uniform solution containing Fe (NO 3)3·9H2 O and Ni (NO 3)2·6H2 O) for hydrothermal reaction, taking out after the reaction is finished, and drying after ultrasonic treatment and deionized water washing to obtain a NiFe-LDH precursor; (2) And drying the obtained precursor, immersing the dried precursor in an ethanol solution of ammonium persulfate, and then carrying out high-temperature carbonization treatment under the protection of inert gas atmosphere to finally prepare the nitrogen-sulfur co-doped modified ferronickel layered double oxide material. Preferably, in the step (1), the pretreatment process comprises the steps of immersing the carbon felt substrate in sulfuric acid solution, absolute ethanol solution and deionized water in sequence and respectively carrying out ultrasonic treatment for 15 minutes, wherein the concentration of the sulfuric acid solution is 0.5-1.5mol/L. Preferably, in step (1), 1mmol of Fe (NO 3)3·9H2 O and 1-3mmol of Ni (NO 3)2·6H2 O) are added to every 10mL of deionized water to form a homogeneous solution. Preferably, in the step (1), the hydrothermal reaction temperature is 120-180 ℃ and the time is 6-12h. Preferably, in the step (2), the concentration of the ethanol solution of the ammonium persulfate is 2.5-10mmol/L, and the time for immersing the precursor in the ethanol solution of the ammonium persulfate is 6-12h. Preferably, in the step (2), the high-temperature carbonization treatment is carried out at a temperature of 500-700 ℃ for 1-3 hours. Preferably, in step (2), the inert gas is nitrogen or argon. The nitrogen-sulfur co-doped modified nickel-iron layered double oxide material prepared by the preparation method is used in water treatment, the nitrogen-sulfur co-doped modified nickel-iron layered double oxide material is used as a cathode, and a graphite plate is used as an anode for removing heavy metals Cr (VI) and p-nitrophenol in water. The invention provides a preparation method and application of a nitrogen-sulfur co-doped modified layered double oxide material, which have the following beneficial effec