Preparation method of nitrogen, phosphorus and oxygen co-doped porous graphitized carbon nanosheet

Abstract

The invention provides a preparation method of a nitrogen, phosphorus and oxygen co-doped porous graphitized carbon nanosheet, and belongs to the field of preparation of porous carbon materials. According to the method, phytic acid organic matter serves as a phosphorus source and a carbon precursor, melamine sponge serves as a nitrogen source and a supporting framework, iron, cobalt and nickel salt serve as graphitizing agents, and a cross-linked network structure is formed through the complexing action between rich hydroxyl oxygen in the phytic acid organic matter and metal ions; in the carbonization process, the complex forms a sheet-shaped or planar structure under the confinement and shape selection effects of metal ions, and meanwhile, the nitrogen, phosphorus and oxygen co-doped porous graphitized carbon nanosheet is obtained based on the catalytic graphitization effect of transition metal and the activation effect of phosphoric acid. Compared with a technology for preparing thecarbon nanosheet by adopting the template method, the method is simple and relatively low in cost, and the obtained carbon nanosheet has a two-dimensional vertically-distributed pore structure and relatively high graphitization degree, and has a huge application prospect in the fields of energy storage, catalysis, adsorption and the like.

Description

technical field

[0001] The invention belongs to the technical field of preparation of porous carbon materials, in particular to a preparation method of nitrogen, phosphorus and oxygen co-doped porous graphitized carbon nanosheets. Background technique

[0002] The two-dimensional structure of carbon nanosheets has an open planar structure, high specific surface area, and excellent electrical conductivity, which can provide shorter ion diffusion paths and fast electron transport channels. Its unique structure and properties make it attract extensive attention in the field of energy storage and conversion. However, traditionally prepared carbon nanosheets, such as graphene, are prone to agglomeration, and the surface lacks vertical channels, which means that when ions diffuse in the vertical direction, electrolyte ions must find the edges or defects of the graphene planes, thereby extending The ion transport path is disrupted, resulting in slow ion mobility. In recent years,...

Examples

Embodiment 1

[0026] (1) Weigh 1 g of phytic acid and dissolve it in 10 mL of deionized water, then add 10 mL of 0.05 g / mL ferric nitrate solution dropwise into the phytic acid solution under stirring, and after stirring continuously for 1 hour, add 0.05 g The melamine sponge was added to the above mixed solution, stirred to make it fully impregnated, and the self-assembled iron-phytic acid complex was obtained through the complexation of metal ions and phytic acid, and then dried in an oven at 80°C.

[0027] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 700°C at a rate of 5°C / min, keep it warm for 1 hour, cool naturally, and wash repeatedly with acid and deionized water to remove metals in the product elements, and then dried at 80°C to obtain the porous graphitized carbon nanosheets.

[0028] The prepared carbon nanosheets were measured by D / max-2500 X-ray diffractometer. The corresponding test conditions and parameters were: Cu target, Ni filter materia...

Embodiment 2

[0031] (1) Weigh 1 g of sodium phytate and dissolve it in 10 mL of deionized water, then add 10 mL of 0.1 g / mL potassium ferricyanide solution dropwise into the sodium phytate solution under stirring, and continue stirring for 1 hour , add 0.1 g melamine sponge to the above mixed solution, stir to make it fully impregnated, and obtain a self-assembled iron-phytic acid-based complex through the complexation of metal and hydroxyl oxygen in phytic acid, and then place it in an oven at 80 °C dry.

[0032] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 800°C at a rate of 20°C / min, keep warm for 2 hours after carbonization, cool naturally, and wash repeatedly with acid and deionized water to remove metals in the product elements, and then dried at 80°C to obtain the porous graphitized carbon nanosheets.

[0033] The method of testing its degree of graphitization and specific surface area is the same as in Example 1.

[0034] The specific surface a...

Embodiment 3

[0036] (1) Weigh 2 g of phytic acid and dissolve it in 10 mL of deionized water, then add 10 mL of 0.20 g / mL potassium trioxalate ferrate solution dropwise into the phytic acid solution under stirring, and keep stirring for 1 hour , Add 0.15 g melamine sponge into the above mixed solution, stir to make it fully impregnated. The self-assembled iron-phytic acid complex was obtained by the complexation of the metal with the hydroxyl oxygen in phytic acid, and then dried in an oven at 80°C.

[0037] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 750°C at a rate of 5°C / min, keep it warm for 2 hours, cool naturally, and wash repeatedly with acid and deionized water to remove metals in the product elements, and then dried at 80°C to obtain the porous graphitized carbon nanosheets.

[0038] The method of testing its degree of graphitization and specific surface area is the same as in Example 1.

[0039] The specific surface area of ​​the porous graphi...

technical field

[0001] The invention belongs to the technical field of preparation of porous carbon materials, in particular to a preparation method of nitrogen, phosphorus and oxygen co-doped porous graphitized carbon nanosheets. Background technique

[0002] The two-dimensional structure of carbon nanosheets has an open planar structure, high specific surface area, and excellent electrical conductivity, which can provide shorter ion diffusion paths and fast electron transport channels. Its unique structure and properties make it attract extensive attention in the field of energy storage and conversion. However, traditionally prepared carbon nanosheets, such as graphene, are prone to agglomeration, and the surface lacks vertical channels, which means that when ions diffuse in the vertical direction, electrolyte ions must find the edges or defects of the graphene planes, thereby extending The ion transport path is disrupted, resulting in slow ion mobility. In recent years,...

Examples

Embodiment 1

[0026] (1) Weigh 1 g of phytic acid and dissolve it in 10 mL of deionized water, then add 10 mL of 0.05 g / mL ferric nitrate solution dropwise into the phytic acid solution under stirring, and after stirring continuously for 1 hour, add 0.05 g The melamine sponge was added to the above mixed solution, stirred to make it fully impregnated, and the self-assembled iron-phytic acid complex was obtained through the complexation of metal ions and phytic acid, and then dried in an oven at 80°C.

[0027] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 700°C at a rate of 5°C / min, keep it warm for 1 hour, cool naturally, and wash repeatedly with acid and deionized water to remove metals in the product elements, and then dried at 80°C to obtain the porous graphitized carbon nanosheets.

[0028] The prepared carbon nanosheets were measured by D / max-2500 X-ray diffractometer. The corresponding test conditions and parameters were: Cu target, Ni filter materia...

Embodiment 2

[0031] (1) Weigh 1 g of sodium phytate and dissolve it in 10 mL of deionized water, then add 10 mL of 0.1 g / mL potassium ferricyanide solution dropwise into the sodium phytate solution under stirring, and continue stirring for 1 hour , add 0.1 g melamine sponge to the above mixed solution, stir to make it fully impregnated, and obtain a self-assembled iron-phytic acid-based complex through the complexation of metal and hydroxyl oxygen in phytic acid, and then place it in an oven at 80 °C dry.

[0032] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 800°C at a rate of 20°C / min, keep warm for 2 hours after carbonization, cool naturally, and wash repeatedly with acid and deionized water to remove metals in the product elements, and then dried at 80°C to obtain the porous graphitized carbon nanosheets.

[0033] The method of testing its degree of graphitization and specific surface area is the same as in Example 1.

[0034] The specific surface a...

Embodiment 3

[0036] (1) Weigh 2 g of phytic acid and dissolve it in 10 mL of deionized water, then add 10 mL of 0.20 g / mL potassium trioxalate ferrate solution dropwise into the phytic acid solution under stirring, and keep stirring for 1 hour , Add 0.15 g melamine sponge into the above mixed solution, stir to make it fully impregnated. The self-assembled iron-phytic acid complex was obtained by the complexation of the metal with the hydroxyl oxygen in phytic acid, and then dried in an oven at 80°C.

[0037] (2) Carbonize the dried solid in a nitrogen atmosphere, raise the temperature to 750°C at a rate of 5°C / min, keep it warm for 2 hours, cool naturally, and wash repeatedly with acid and deionized water to remove metals in the product elements, and then dried at 80°C to obtain the porous graphitized carbon nanosheets.

[0038] The method of testing its degree of graphitization and specific surface area is the same as in Example 1.

[0039] The specific surface area of ​​the porous graphi...

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