A preparation method of P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon for water treatment

Abstract

The application relates to a preparation method of a P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material for water treatment, in particular to the following steps: dispersing chitosan into ethanol, adding salicylaldehyde, drying after reaction to obtain a solid; mixing the solid with ethanol and Ni(NO3)2.6H2O, grinding after drying and reaction to obtain a powder; mixing the powder with WO3 powder, dispersing in ethanol, dropping onto foamed nickel iron, placing into a magnetic boat, placing NaH2PO2.H2O into another magnetic boat, placing the two magnetic boats in a tube furnace, placing NaH2PO2.H2O at the rear end, roasting under an Ar atmosphere to obtain a P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon; and the application of the prepared P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material in a water treatment reaction.

Description

TECHNICAL FIELD

[0001] The application relates to a preparation method of a P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon for water treatment, and belongs to the fields of material preparation and application. BACKGROUND

[0002] With the increasing demand for energy and the overconsumption of traditional fossil fuels, finding alternative renewable energy sources has attracted a lot of attention. Among potential alternative energy sources, hydrogen energy is considered one of the cleanest and greenest energy sources due to its high energy density and atomic efficiency. Water electrolysis is considered an ideal method to provide hydrogen energy. Water electrolysis includes an oxygen evolution reaction at the anode and a hydrogen evolution reaction at the cathode. So far, Pt is considered to be the most active hydrogen evolution reaction catalyst; the oxygen evolution reaction activation energy barrier can be effectively reduced by catalysts IrO2 and RuO2. The existing disadvantage is that the price of noble metals limits their industrial application. Therefore, developing non-noble metal catalysts to drive water splitting is an urgent task at present.

[0003] Recent studies have shown that transition metal-based materials, especially W-based materials, are considered a potential water electrolysis material. Transition metal oxides have high content, adjustable composition, and diverse synthesis strategies. Various material design strategies, including chemical doping, defect engineering, and interface engineering, have become effective paths to adjust catalyst performance. For example: Chen's team used MoO3, cobalt acetate, nickel acetate, etc. to obtain MoNiCoO x complex by hydrothermal treatment at 90 DEG C for 5 h; the MoS2 / NiS2 / CoS2 nanotube was obtained by high-temperature treatment of the MoS2 / NiS2 / CoS2 nanotube with S powder at 400 DEG C for 2 h; the MoS2 / NiS2 / CoS2 nanotube was applied to catalyze water splitting to prepare hydrogen and oxygen, and when the voltage was 1.58 V, the current density was 10 mA / cm 2 (Materials Today Nano 17 (2022) 100156). Wen's team used Ni(NO3)2·6H2O, Fe(NO3)3·9H2O, (NH4)6Mo7O 24 ·4H2O, red P, etc. to synthesize NiFeP-MoO2 nanorods; the NiFeP-MoO2 nanorod was applied to catalyze water splitting to prepare hydrogen and oxygen, and when the voltage was 1.41 V and 1.65 V, the current density was 10 mA / cm 2 and 100 mA / cm 2(Chemical Engineering Journal 409 (2021) 128161). Tang team dissolved Mo powder in hydrogen peroxide, then added SDS, put into foamed Ni, hydrothermal treatment at 180 ℃ for 5 h, the obtained product was treated by 5% H2 / N2 at 450 ℃ for 1 h to obtain NiMoO 4-x / MoO2 complex; the NiMoO 4-x / MoO2 complex is applied to catalytic water decomposition to prepare hydrogen and oxygen, and when the voltage is 1.56 V, the current density is 10 mA / cm 2 (Journal of Materials Chemistry A 6 (2018) 12361). We use chitosan to construct P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon, which effectively catalyzes water decomposition, which has important practical significance. SUMMARY

[0004] The present application aims to provide a preparation method of P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon for water treatment.

[0005] Based on the above purpose, the technical scheme of the present application is as follows:

[0006] (1) Preparation of P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon: 0.5-1.5 g of chitosan is dispersed in 40-60 mL of ethanol, then 0.5-1.5 g of salicylaldehyde is added, and the reaction is carried out at 60 ℃ for 10 h, and then the solid is obtained after drying; 0.1-0.2 g of the solid is mixed with 15 mL of ethanol and 0.5 g of Ni(NO3)2·6H2O, and the reaction is carried out at 70-100 ℃ for 8 h, and then the powder is obtained after drying and grinding; 0.1-0.6 g of the powder is mixed with 0.1-0.5 g of WO3 powder, dispersed in ethanol, and then added dropwise to foamed nickel iron, placed in a porcelain boat, and another porcelain boat is placed in a porcelain boat. 0.5 g of NaH2PO2·H2O, two porcelain boats are placed in a tube furnace, NaH2PO2·H2O is placed at the rear end, and the two porcelain boats are placed in a tube furnace under Ar atmosphere, and calcined at 400-500 ℃ for 1 h to obtain P-WO3-Ni5P4 heterostructure material loaded on nitrogen-doped carbon. The above preparation method, the Ni5P4 belongs to standard card JCPDS #18-0883, and the WO3 belongs to standard card JCPDS #43-1035.

[0007] (2) Application of the P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material prepared by the above preparation method in water treatment reaction; in the electrocatalytic decomposition of water, the reaction current density is 10 mA / cm 2 , and the voltage is 1.58-1.65 V.

[0008] The present application has the following advantages:

[0009] (1) A new synthesis route of P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material is provided.

[0010] (2) The P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon exhibits high catalytic ability in water treatment reaction. BRIEF DESCRIPTION OF DRAWINGS

[0011] Figure 1 are XRD, SEM and Ni, P, C, N Mapping characterization results of the P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material. DETAILED DESCRIPTION

[0012] The following examples are used to further illustrate the present application, but do not limit the present application.

[0013] Example 1

[0014] 0.5 g of chitosan was dispersed in 40 mL of ethanol, and then 0.5 g of salicylaldehyde was added, and the mixture was reacted at 60°C for 10 h, and then dried to obtain a solid; 0.1 g of the solid was mixed with 15 mL of ethanol and 0.5 g of Ni(NO3)2·6H2O, and the mixture was reacted at 70°C for 8 h, and then dried and ground to obtain a powder; 0.1 g of the powder was mixed with 0.1 g of WO3 powder, and the mixture was dispersed in ethanol and then added dropwise to a foamed nickel-iron, and then placed in a porcelain boat, and another porcelain boat was placed with 0.5 g of NaH2PO2·H2O, and the two porcelain boats were placed in a tube furnace, with NaH2PO2·H2O at the rear end, and then calcined at 500°C for 1 h under Ar atmosphere to obtain a P-WO3-Ni5P4 heterostructure material loaded on nitrogen-doped carbon. The above preparation method, the Ni5P4 belongs to standard card JCPDS #18-0883, and the WO3 belongs to standard card JCPDS #43-1035. Application of the P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material prepared by the above preparation method in water treatment reaction; in electrocatalytic decomposition of water, the reaction current density is 10 mA / cm 2 , and the voltage is 1.58 V.

[0015] Example 2

[0016] Disperse 1.5 g of chitosan into 60 mL of ethanol, add 1.5 g of salicylaldehyde, and react at 60 °C for 10 h. After drying, a solid is obtained. Mix 0.2 g of the solid with 15 mL of ethanol and 0.5 g of Ni(NO3)2·6H2O, and react at 100 °C for 8 h. After drying and grinding, a powder is obtained. Mix 0.6 g of the powder with 0.5 g of WO3 powder, disperse in ethanol, and drop onto a foamed nickel-iron. Put into a porcelain boat, and put 0.5 g of NaH2PO2·H2O into another porcelain boat. Place the two porcelain boats in a tube furnace, with the NaH2PO2·H2O at the rear end. Under an Ar atmosphere, calcine at 400 °C for 1 h to obtain a P-WO3-Ni5P4 heterostructure material loaded on nitrogen-doped carbon. The above preparation method, the Ni5P4 belongs to standard card JCPDS #18-0883, and the WO3 belongs to standard card JCPDS #43-1035. Application of the P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material prepared by the above preparation method in a water treatment reaction; in electrocatalytic decomposition of water, the reaction current density is 10 mA / cm 2 , and the voltage is 1.65 V.

[0017] Example 3

[0018] Disperse 0.5 g of chitosan into 60 mL of ethanol, add 0.5 g of salicylaldehyde, and react at 60 °C for 10 h. After drying, a solid is obtained. Mix 0.2 g of the solid with 15 mL of ethanol and 0.5 g of Ni(NO3)2·6H2O, and react at 70 °C for 8 h. After drying and grinding, a powder is obtained. Mix 0.6 g of the powder with 0.1 g of WO3 powder, disperse in ethanol, and drop onto a foamed nickel-iron. Put into a porcelain boat, and put 0.5 g of NaH2PO2·H2O into another porcelain boat. Place the two porcelain boats in a tube furnace, with the NaH2PO2·H2O at the rear end. Under an Ar atmosphere, calcine at 400 °C for 1 h to obtain a P-WO3-Ni5P4 heterostructure material loaded on nitrogen-doped carbon. The above preparation method, the Ni5P4 belongs to standard card JCPDS #18-0883, and the WO3 belongs to standard card JCPDS #43-1035. Application of the P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material prepared by the above preparation method in a water treatment reaction; in electrocatalytic decomposition of water, the reaction current density is 10 mA / cm 2 , and the voltage is 1.62 V.

Claims

1. A preparation method of P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon, characterized in that, Comprising the following steps: Disperse 0.5-1.5 g chitosan into 40-60 mL ethanol, then add 0.5-1.5 g salicylaldehyde, react at 60 ℃ for 10 h, dry to obtain a solid; mix 0.1-0.2 g of the solid with 15 mL ethanol and 0.5 g Ni(NO3)2·6H2O, react at 70-100 ℃ for 8 h, dry and grind to obtain a powder; mix 0.1-0.6 g of the powder with 0.1-0.5 g WO3 powder, disperse in ethanol, drop onto a foamed nickel-iron, put into a porcelain boat, put 0.5 g NaH2PO2·H2O into another porcelain boat, place the two porcelain boats in a tube furnace, NaH2PO2·H2O at the rear end, calcine at 400-500 ℃ for 1 h under Ar atmosphere, to obtain a P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon.

2. The production method according to claim 1, wherein The Ni5P4 belongs to standard card JCPDS #18-0883, and the WO3 belongs to standard card JCPDS #43-1035.

3. The application of the P-WO3-Ni5P4 heterostructure / nitrogen-doped carbon material prepared by the preparation method of any one of claims 1-2 in a water treatment reaction, wherein the water treatment reaction is an electrocatalytic water splitting reaction, and in the electrocatalytic water splitting reaction, a reaction current density is 10 mA / cm2, and a voltage is 1.58-1.65 V. 2 .

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