CN113353989A - Rambutan-shaped Co3O4-N, S doped porous carbon composite material and preparation method thereof - Google Patents
Rambutan-shaped Co3O4-N, S doped porous carbon composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of batteries, and discloses rambutan-shaped Co3O4-N, S doped porous carbon composite, synthetic porous carbon and rambutan-like Co3O4All having a large specific surface area and a plurality of pore structures, in Co3O4Adding N and S doping in the hydrothermal process to form Co3O4Can be uniformly dispersed on a carbon substrate, avoids the agglomeration of transition metal oxide materials, simultaneously, the carbon material has excellent conductivity, effectively improves the conductivity of the composite material, and cobalt ions exist in different valence states, so that the composite material has excellent oxygen reduction capability and can be used as reversible adsorptionThe carbon material can generate more active sites rich in electrons or lack of electrons on the surface of the carbon material by doping S atoms, and the doping of nitrogen can generate an electronic modulation effect on the material and provide a carrier for a metal catalyst, so that rambutan-shaped Co is formed3O4the-N, S doped porous carbon composite material has good conductivity and oxygen reduction capability.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to rambutan-shaped Co3O4-N, S doped porous carbon composite material and preparation method.
Background
Along with the development of industrialization, people are increasing to the demand of fossil energy, and as non-renewable energy, the storage capacity of traditional fossil energy faces the situation that the supply is short of the demand, it has important meaning to develop novel sustainable energy, the battery is regarded as a novel energy storage device, and is occupying more and more important position in human modern society, metal-air battery is a novel energy battery in the battery, has a series of advantages such as green, the memory space is big, with low costs, safety and stability, is a novel battery that has a great prospect of development.
The metal-air battery has the working principle that chemical energy is converted into electric energy, the electric energy is generated through the chemical reaction of oxygen reduction reaction and fuel oxidation reaction, wherein the metal is usually zinc, magnesium, aluminum and the like and oxygen is used as dye in the battery, the oxygen used as a positive electrode material is derived from air, is a renewable substance which is inexhaustible, so that the metal-air battery can be effectively and conveniently used, in order to enable the fuel battery to rapidly convert the chemical energy into the electric energy, an efficient oxygen reduction catalyst needs to be developed to replace the traditional noble metal catalyst, metal oxide taking carbon as a substrate has good oxygen reduction capability, the carbon material can improve the conductivity of the whole material, and the doping of sulfur, nitrogen, phosphorus and other miscellaneous elements can well generate electronic modulation effect on the material to provide an ideal electronic structure, can better provide a carrier for a metal catalyst, common metal oxides include manganese oxide and cobalt oxide, and Co in the cobalt oxide3O4The composite material has high electrocatalytic activity, can form different composite materials, is a bifunctional catalyst with excellent properties, is easy to agglomerate, is used as an oxide of a transition metal, has poor conductive performance, can well solve the problem after being compounded with a carbon material, and simultaneously improves the stability of the carbon material.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides rambutan-shaped Co3O4The (E) -N, S doped porous carbon composite material and the preparation method solve the problem of transition metal oxide Co3O4Poor conductivity and poor oxygen reduction effect.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: rambutan-shaped Co3O4-N, S doped porous carbon composite, said rambutan-like Co3O4The preparation method of the-N, S doped porous carbon composite material comprises the following steps:
(1) mixing polyoxyethylene polyoxypropylene ether with a hydrochloric acid solution, stirring for dissolving, adding chitosan and an acetic acid solution, stirring for mixing, and drying to obtain a porous carbon precursor;
(2) placing the porous carbon precursor in a tubular furnace, and calcining in an argon and hydrogen sulfide mixed gas atmosphere to obtain N and S doped porous carbon;
(3) mixing glycerol and a cobalt chloride aqueous solution, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, carrying out hydrothermal reaction, washing, centrifuging and drying after the reaction is finished, so as to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, and calcining in a nitrogen atmosphere to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Preferably, the temperature for stirring and mixing in the step (1) is 25-45 ℃, and the time for stirring and mixing is 24-36 h.
Preferably, the volume ratio of the argon gas to the hydrogen sulfide mixed gas in the step (2) is 15-25: 1.
Preferably, the heating rate of the calcination in the step (2) is 3-6 ℃/min, the calcination temperature is 850-.
Preferably, the mass ratio of the glycerol to the cobalt chloride to the N, S doped porous carbon in the step (3) is 6-10:50-65: 100.
Preferably, the temperature of the hydrothermal reaction in the step (3) is 120-180 ℃, and the time of the hydrothermal reaction is 12-24 h.
Preferably, the temperature rise rate of the calcination in the step (4) is 1-3 ℃/min, the calcination temperature is 300-450 ℃, and the calcination time is 2-4 h.
(III) advantageous technical effects
Compared with the prior art, the invention has the following chemical mechanism and beneficial technical effects:
the rambutan-shaped Co3O4-N, S doped porous carbon compositeIn the synthesis process, a chitosan carbon skeleton is used as a carbon source, side chain amino is used as a nitrogen source, polyoxyethylene polyoxypropylene ether is used as a pore-foaming agent, hydrogen sulfide gas is introduced under the condition of high-temperature calcination, the hydrogen sulfide gas is used as a sulfur source, and the thermal reaction is carried out on the hydrogen sulfide gas and a carbon precursor to obtain N and S doped porous carbon, and a Co doped porous carbon prepared by a solvothermal method by adopting a template-free method3O4Has a large number of pores and internally communicated pore passages to form rambutan-shaped Co3O4Adding N, S doped porous carbon before hydrothermal treatment, and calcining to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
The rambutan-shaped Co3O4-N, S doped porous carbon composite, porous carbon and rambutan-like Co3O4All having a large specific surface area and a plurality of pore structures, in Co3O4Adding N and S doping in the hydrothermal process to form Co3O4Can be uniformly dispersed on a carbon matrix, avoids the agglomeration of transition metal oxide materials, has excellent conductivity, effectively improves the conductivity of the composite material, and avoids transition metal Co3O4The problem of poor conductivity exists, cobalt ions exist in different valence states, so that the carbon material has excellent oxygen reduction capacity and can serve as reversible adsorption, oxygen analysis and acceptor chemical adsorption sites, thereby playing a role of catalysis, S atoms are doped, more active sites rich in electrons or lacking electrons are generated on the surface of the carbon material in the transportation and transfer processes of battery ions and charges, and nitrogen is doped, so that the carbon material can well generate an electronic modulation effect on the material, an ideal electronic structure is provided, a carrier can be better provided for a metal catalyst, and the rambutan-shaped Co has the advantages of good red lead shape3O4the-N, S doped porous carbon composite material has good conductivity and oxygen reduction capability.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: rambutan-shaped Co3O4-N, S doped porous carbon composite material, the preparation method comprising the steps of:
(1) adding polyoxyethylene polyoxypropylene ether and a hydrochloric acid solution into a beaker, mixing, stirring for dissolving, adding chitosan and an acetic acid solution, stirring and mixing at the temperature of 25-45 ℃ for 24-36h, mixing, and drying in a drying oven to obtain a porous carbon precursor;
(2) placing the porous carbon precursor in a tubular furnace, calcining in a mixed gas atmosphere of argon and hydrogen sulfide at a volume ratio of 15-25:1, wherein the calcining heating rate is 3-6 ℃/min, the calcining temperature is 850-950 ℃, the calcining time is 5-8h, and after calcining, obtaining N and S doped porous carbon;
(3) adding a mixed solution of glycerol and cobalt chloride water into a beaker, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, wherein the mass ratio of the glycerol to the cobalt chloride to the N and S doped porous carbon is 6-10:50-65:100, carrying out hydrothermal reaction at the temperature of 120-180 ℃ for 12-24h, washing with ethanol and deionized water after the reaction is finished, centrifuging, and drying to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, calcining in nitrogen atmosphere at a temperature rise rate of 1-3 ℃/min at a temperature of 300-450 ℃ for 2-4h to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Example 1
(1) Adding polyoxyethylene polyoxypropylene ether and a hydrochloric acid solution into a beaker, mixing, stirring for dissolving, adding chitosan and an acetic acid solution, stirring and mixing at the temperature of 25 ℃, stirring and mixing for 24 hours, and drying in a drying oven after mixing to obtain a porous carbon precursor;
(2) placing a porous carbon precursor in a tubular furnace, calcining in a mixed gas atmosphere of argon and hydrogen sulfide with a volume ratio of 15:1, wherein the calcining heating rate is 3 ℃/min, the calcining temperature is 850 ℃, the calcining time is 5h, and after calcining, obtaining N and S doped porous carbon;
(3) adding a mixed solution of glycerol and cobalt chloride water into a beaker, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, wherein the mass ratio of the glycerol to the cobalt chloride to the S doped porous carbon is 6:50:100, carrying out hydrothermal reaction at the temperature of 120 ℃ for 12h, washing with ethanol and deionized water after the reaction is finished, centrifuging, and drying to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, calcining in nitrogen atmosphere at the temperature rise rate of 1 ℃/min at the calcining temperature of 300 ℃ for 2h to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Example 2
(1) Adding polyoxyethylene polyoxypropylene ether and a hydrochloric acid solution into a beaker, mixing, stirring for dissolving, adding chitosan and an acetic acid solution, stirring and mixing at the temperature of 30 ℃ for 28h, mixing, and drying in a drying oven to obtain a porous carbon precursor;
(2) placing a porous carbon precursor in a tubular furnace, calcining in a mixed gas atmosphere of argon and hydrogen sulfide with a volume ratio of 18:1, wherein the calcining heating rate is 4 ℃/min, the calcining temperature is 880 ℃, the calcining time is 6h, and after calcining, obtaining N and S doped porous carbon;
(3) adding a mixed solution of glycerol and cobalt chloride water into a beaker, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, wherein the mass ratio of the glycerol to the cobalt chloride to the S doped porous carbon is 7:55:100, carrying out hydrothermal reaction at the temperature of 140 ℃ for 15h, washing with ethanol and deionized water after the reaction is finished, centrifuging, and drying to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, calcining in nitrogen atmosphere at the temperature rise rate of 2 ℃/min at the calcining temperature of 350 ℃ for 2.5h to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Example 3
(1) Adding polyoxyethylene polyoxypropylene ether and a hydrochloric acid solution into a beaker, mixing, stirring for dissolving, adding chitosan and an acetic acid solution, stirring and mixing at the temperature of 35 ℃ for 32 hours, and drying in a drying oven after mixing to obtain a porous carbon precursor;
(2) placing a porous carbon precursor in a tubular furnace, calcining in a mixed gas atmosphere of argon and hydrogen sulfide at a volume ratio of 20:1, wherein the calcining heating rate is 5 ℃/min, the calcining temperature is 900 ℃, the calcining time is 7h, and after calcining, obtaining N and S doped porous carbon;
(3) adding a mixed solution of glycerol and cobalt chloride water into a beaker, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, wherein the mass ratio of the glycerol to the cobalt chloride to the S doped porous carbon is 7:58:100, carrying out hydrothermal reaction at the temperature of 150 ℃ for 18h, washing with ethanol and deionized water after the reaction is finished, centrifuging, and drying to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, calcining in nitrogen atmosphere at the temperature rise rate of 2 ℃/min at the temperature of 400 ℃ for 3h to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Example 4
(1) Adding polyoxyethylene polyoxypropylene ether and a hydrochloric acid solution into a beaker, mixing, stirring for dissolving, adding chitosan and an acetic acid solution, stirring and mixing at the temperature of 40 ℃ for 35 hours, and drying in a drying oven after mixing to obtain a porous carbon precursor;
(2) placing the porous carbon precursor in a tubular furnace, calcining in a mixed gas atmosphere of argon and hydrogen sulfide with a volume ratio of 24:1, wherein the calcining heating rate is 5 ℃/min, the calcining temperature is 920 ℃, the calcining time is 7h, and after calcining, obtaining N and S doped porous carbon;
(3) adding a mixed solution of glycerol and cobalt chloride water into a beaker, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, wherein the mass ratio of the glycerol to the cobalt chloride to the S doped porous carbon is 9:64:100, carrying out hydrothermal reaction at 160 ℃ for 22h, washing with ethanol and deionized water after the reaction is finished, centrifuging, and drying to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, calcining in nitrogen atmosphere at the temperature rise rate of 2 ℃/min, the calcining temperature of 420 ℃ and the calcining time of 3.5h to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Example 5
(1) Adding polyoxyethylene polyoxypropylene ether and a hydrochloric acid solution into a beaker, mixing, stirring for dissolving, adding chitosan and an acetic acid solution, stirring and mixing at the temperature of 45 ℃, for 36 hours, mixing, and drying in a drying oven to obtain a porous carbon precursor;
(2) placing the porous carbon precursor in a tubular furnace, calcining in a mixed gas atmosphere of argon and hydrogen sulfide at a volume ratio of 25:1, wherein the calcining heating rate is 6 ℃/min, the calcining temperature is 950 ℃, the calcining time is 8h, and after calcining, obtaining N and S doped porous carbon;
(3) adding a mixed solution of glycerol and cobalt chloride water into a beaker, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, wherein the mass ratio of the glycerol to the cobalt chloride to the S doped porous carbon is 10:65:100, carrying out hydrothermal reaction at the temperature of 180 ℃ for 24 hours, washing with ethanol and deionized water after the reaction is finished, centrifuging, and drying to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, calcining in nitrogen atmosphere at the temperature rise rate of 3 ℃/min at the temperature of 450 ℃ for 4h to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Comparative example 1
(1) Adding polyoxyethylene polyoxypropylene ether and a hydrochloric acid solution into a beaker, mixing, stirring for dissolving, adding chitosan and an acetic acid solution, stirring and mixing at the temperature of 35 ℃ for 32 hours, and drying in a drying oven after mixing to obtain a porous carbon precursor;
(2) placing a porous carbon precursor in a tubular furnace, calcining in a mixed gas atmosphere of argon and hydrogen sulfide with a volume ratio of 10:1, wherein the calcining heating rate is 4 ℃/min, the calcining temperature is 900 ℃, the calcining time is 6h, and after calcining, obtaining N and S doped porous carbon;
(3) adding a mixed solution of glycerol and cobalt chloride water into a beaker, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, wherein the mass ratio of the glycerol to the cobalt chloride to the S doped porous carbon is 2:15:100, carrying out hydrothermal reaction at the temperature of 150 ℃ for 18h, washing with ethanol and deionized water after the reaction is finished, centrifuging, and drying to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N, S-doped porous carbon into a tubular furnace, calcining in nitrogen atmosphere at the temperature rise rate of 2 ℃/min at the calcining temperature of 350 ℃ for 3h to obtain rambutan-shaped Co3O4-N, S doped porous carbon composite.
Taking 50mg rambutan-shaped Co prepared in the experimental process3O4the-N, S doped porous carbon composite material is used as a catalyst, is ultrasonically mixed with absolute ethyl alcohol and Nafion solution to form uniform slurry, and is transferred to a position with the area of 0.25cm2The carbon paper is dried to obtain an air electrode, then the air electrode, the polished zinc sheet, the battery shell and 6mol/L potassium hydroxide electrolyte form a zinc-air battery, air is continuously introduced in the testing process, the MSR rotating disc electrode is used for testing the initial potential and half-wave potential of an oxygen reduction material in the electrolyte, and the rotating speed is 1600 rmp.
| Item | Initial potential (V) | Half-wave potential (V) |
| Example 1 | 1.53 | 0.750 |
| Example 2 | 1.62 | 0.783 |
| Example 3 | 1.70 | 0.859 |
| Example 4 | 1.78 | 0.825 |
| Example 5 | 1.49 | 0.731 |
| Comparative example 1 | 1.25 | 0.548 |
Claims (7)
1. Rambutan-shaped Co3O4-N, S doped porous carbon composite characterized in that: the preparation method of the rambutan-shaped Co3O4-N, S-doped porous carbon composite material comprises the following steps:
(1) mixing polyoxyethylene polyoxypropylene ether with a hydrochloric acid solution, stirring for dissolving, adding chitosan and an acetic acid solution, stirring for mixing, and drying to obtain a porous carbon precursor;
(2) placing the porous carbon precursor in a tubular furnace, and calcining in an argon and hydrogen sulfide mixed gas atmosphere to obtain N and S doped porous carbon;
(3) mixing glycerol and a cobalt chloride aqueous solution, adding urea, stirring and mixing uniformly, adding N and S doped porous carbon, carrying out hydrothermal reaction, washing, centrifuging and drying after the reaction is finished, so as to obtain a cobalt precursor loaded N and S doped porous carbon;
(4) transferring the cobalt precursor loaded with N and S doped porous carbon into a tubular furnace, and calcining in a nitrogen atmosphere to obtain the rambutan-shaped Co3O4-N and S doped porous carbon composite material.
2. The rambutan-like Co3O4-N, S doped porous carbon composite material according to claim 1, characterized in that: the stirring and mixing temperature in the step (1) is 25-45 ℃, and the stirring and mixing time is 24-36 h.
3. The rambutan-like Co3O4-N, S doped porous carbon composite material according to claim 1, characterized in that: the volume ratio of the mixed gas of argon and hydrogen sulfide in the step (2) is 15-25: 1.
4. The rambutan-like Co3O4-N, S doped porous carbon composite material according to claim 1, characterized in that: in the step (2), the heating rate of the calcination is 3-6 ℃/min, the calcination temperature is 850-950 ℃, and the calcination time is 5-8 h.
5. The rambutan-like Co3O4-N, S doped porous carbon composite material according to claim 1, characterized in that: in the step (3), the mass ratio of the glycerol to the cobalt chloride to the N, S doped porous carbon is 6-10:50-65: 100.
6. The rambutan-like Co3O4-N, S doped porous carbon composite material according to claim 1, characterized in that: the temperature of the hydrothermal reaction in the step (3) is 120-180 ℃, and the time of the hydrothermal reaction is 12-24 h.
7. The rambutan-like Co3O4-N, S doped porous carbon composite material according to claim 1, characterized in that: in the step (4), the temperature rise rate of the calcination is 1-3 ℃/min, the calcination temperature is 300-450 ℃, and the calcination time is 2-4 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115050977A (en) * | 2022-06-20 | 2022-09-13 | 江苏展鸣新能源有限公司 | Porous carbon loaded Co applied to zinc-air battery 3 O 4 Electrocatalyst and method of making |
| CN115475660A (en) * | 2022-10-11 | 2022-12-16 | 福建师范大学 | Preparation of Co with high catalytic oxidation activity by using chitosan-assisted sol method 3 O 4 Method (2) |
| CN116013698A (en) * | 2023-03-28 | 2023-04-25 | 今朝时代(青岛)新能源科技有限公司 | Composite electrode material for super capacitor and preparation process thereof |
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2021
- 2021-05-24 CN CN202110562934.4A patent/CN113353989A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115050977A (en) * | 2022-06-20 | 2022-09-13 | 江苏展鸣新能源有限公司 | Porous carbon loaded Co applied to zinc-air battery 3 O 4 Electrocatalyst and method of making |
| CN115475660A (en) * | 2022-10-11 | 2022-12-16 | 福建师范大学 | Preparation of Co with high catalytic oxidation activity by using chitosan-assisted sol method 3 O 4 Method (2) |
| CN115475660B (en) * | 2022-10-11 | 2023-11-24 | 福建师范大学 | Co with high catalytic oxidation activity prepared by chitosan auxiliary sol method 3 O 4 Is a method of (2) |
| CN116013698A (en) * | 2023-03-28 | 2023-04-25 | 今朝时代(青岛)新能源科技有限公司 | Composite electrode material for super capacitor and preparation process thereof |
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Application publication date: 20210907 |