CN114807981A - High-efficiency synthesis of H 2 O 2 Preparation method and application of Zn-N-C electrocatalyst - Google Patents

High-efficiency synthesis of H 2 O 2 Preparation method and application of Zn-N-C electrocatalyst Download PDF

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CN114807981A
CN114807981A CN202210318319.3A CN202210318319A CN114807981A CN 114807981 A CN114807981 A CN 114807981A CN 202210318319 A CN202210318319 A CN 202210318319A CN 114807981 A CN114807981 A CN 114807981A
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electrocatalyst
acid
preparation
polypyrrole
synthesis
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高书燕
位港亚
刘旭坡
杨天芳
张静
张风仙
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Henan Normal University
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    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/065—Carbon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound

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Abstract

The invention discloses a high-efficiency synthesis method of H 2 O 2 The preparation method and the application of the Zn-N-C electrocatalyst synthesize H with the synthesis by taking polypyrrole nano-wires as a carbon nitrogen source and ZIF-8 with a zeolite structure as a metal zinc source 2 O 2 A high selectivity Zn-N-C electrocatalyst, wherein metallic Zn is loaded on a nitrogen-doped carbon material in a single atom form, and the loading of the metallic Zn is 5wt% -25 wt%. The Zn-N-C electrocatalyst catalyzes and synthesizes H 2 O 2 The selectivity of (a) is close to 100%. The polypyrrole is used as a carbon-nitrogen source, so that metal zinc ions are easier to anchor. The catalyst is prepared by thermally decomposing the composite material of polypyrrole and ZIF-8 in one step, the preparation process is simple, the source of the raw materials of the electrocatalyst is wide, and the cost is low.

Description

High-efficiency synthesis of H 2 O 2 Preparation method and application of Zn-N-C electrocatalyst
Technical Field
The invention belongs to the technical field of synthesis of metal-supported electrocatalysts, and particularly relates to efficient synthesis of H 2 O 2 A preparation method and application of the Zn-N-C electrocatalyst.
Background
H 2 O 2 As a high-value oxidant, the high-value oxidant is widely applied to industries such as wastewater treatment, papermaking and chemical synthesis. 2020 Global H 2 O 2 The production is about 450 ten thousand tons, and the worldwide production is expected to reach 600 ten thousand tons by 2027 years. However, currently about 99% of H 2 O 2 Is synthesized by the anthraquinone process with high energy consumption, and the process can only be carried out in a centralized plant, which can generate a large amount of waste chemicals. Therefore, under the carbon neutralization large background, energy-saving, efficient and green H is searched 2 O 2 The preparation process is particularly important. Electrochemical two-electron oxygen reduction method (2 e) − ORR) to O 2 Reduction to H 2 O 2 Synthesized H 2 O 2 The solution has no impurities and high purity, and can be directly used for sewage treatment and the like. The electrochemical oxygen reduction method has the advantages of simple reaction conditions, clean production process, low time consumption and the like, and is safe, energy-saving, green and sustainable H 2 O 2 The production method.
At present, for the electrocatalytic synthesis of H 2 O 2 The catalyst of (2) mainly includes noble metals and alloys thereof, a single-atom catalyst (SAC) and a carbon-based material. Monatomic catalysts are favored by researchers because of their high atom utilization and fully exposed active sites. Unlike conventional nanoparticle catalysts, SAC has the following characteristics: first, isolated atomic sites in monatomic catalysts can promote O 2 And the tail end of the reaction intermediate is adsorbed, so that the breaking of an O-O bond is hindered and the O-O bond is completely reduced into water; secondly, the electronic structure of the surface of the catalyst can be regulated and controlled through the coordination of metal-substrate, so as to regulate the adsorption of a reaction intermediate and optimize the electrocatalytic activity and selectivity. In many studies, SACs have shown more stable physicochemical properties and properties than conventional nanoparticlesLonger cycle life, however, synthesizing high performance monatomic catalysts is still limiting for the electrocatalytic synthesis of H 2 O 2 Is a key bottleneck. Therefore, the monatomic catalyst with high efficiency and selectivity is designed to realize green H production 2 O 2 Is urgent.
Disclosure of Invention
The invention solves the technical problem of providing a high-efficiency synthetic H 2 O 2 The method takes polypyrrole nano-wires as a carbon-nitrogen source and ZIF-8 with a zeolite structure as a metal zinc source to synthesize high-selectivity synthesized H 2 O 2 The Zn-N-C electrocatalyst.
The invention adopts the following technical scheme for solving the technical problems, and the H is efficiently synthesized 2 O 2 The preparation method of the Zn-N-C electrocatalyst is characterized by comprising the following steps: in the Zn-N-C electrocatalyst, metal Zn is loaded on a nitrogen-doped carbon material in a single atom form, and the loading amount of the metal Zn is 5-25 wt%;
the specific preparation process of the Zn-N-C electrocatalyst is as follows:
step S1: stirring pyrrole at 0-5 ℃ by taking CTAB as a template agent and ammonium persulfate as an oxidant to react to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing the polypyrrole nanowires obtained in the step S1 in methanol, adding zinc nitrate, stirring, adding 2-methylimidazole, standing, performing solid-liquid separation, and drying;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 1-10 ℃/min under an inert gas atmosphere, keeping the temperature for 2-4h, and naturally cooling to room temperature;
step S4: and (5) soaking the material obtained in the step (S3) in an acid solution, then carrying out suction filtration, washing with water to be neutral, and drying to obtain the Zn-N-C electrocatalyst.
Further, in step S3, the inert gas is one or more of nitrogen, argon or helium.
Further limiting, in the step S4, the acid solution is one or more of hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, or acetic acid, the concentration of the acid solution is 0.5 to 4mol/L, the acid treatment temperature is 25 to 100 ℃, and the acid treatment time is 2 to 24 hours.
The invention relates to a high-efficiency synthesis method of H 2 O 2 The preparation method of the Zn-N-C electrocatalyst is characterized by comprising the following specific steps:
step S1: stirring and reacting 600 mu L of pyrrole at 0-5 ℃ for 12h by taking 0.22g of CTAB as a template agent and 2.0g of ammonium persulfate as an oxidant to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing 0.1g of the polypyrrole nanowires obtained in the step S1 in 120mL of methanol, adding 2.38g of zinc nitrate, stirring for 12 hours, then adding 1.64g of 2-methylimidazole, standing for 12 hours, carrying out solid-liquid separation, and drying at 80 ℃;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, keeping the temperature for 3 hours, and then naturally cooling to room temperature;
step S4: and (5) soaking the material obtained in the step (S3) in 2mol/L hydrochloric acid at normal temperature for 24h, then carrying out suction filtration, washing with water to be neutral, and drying at 80 ℃ to obtain the Zn-N-C electrocatalyst.
The Zn-N-C electrocatalyst of the invention catalyzes and synthesizes H 2 O 2 The method is characterized by comprising the following specific processes: dispersing 1mg of prepared Zn-N-C electrocatalyst in a mixed solution of water, ethanol and Nafion, after uniform ultrasonic dispersion, taking a proper amount of solution to be dripped on a ring disc electrode, airing in the air, testing by adopting a three-electrode system, wherein an Hg/HgO electrode and a platinum sheet are respectively used as a reference electrode and a counter electrode, and an electrolyte is O 2 Saturated 0.1mol/L KOH aqueous solution, Zn-N-C electrocatalyst catalyzed synthesis of H 2 O 2 The selectivity of (a) is close to 100%.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. preparation of H according to the invention 2 O 2 Compared with the traditional anthraquinone method, the method is green and environment-friendly, and can be directly used in the fields of sewage treatment and the like.
2. The polypyrrole is used as a carbon-nitrogen source, so that metal zinc ions are easier to anchor. The catalyst is prepared by thermally decomposing the composite material of polypyrrole and ZIF-8 in one step, the preparation process is simple, the source of the raw materials of the electrocatalyst is wide, and the cost is low.
The catalyst provided by the invention can be evaluated by the following method:
the catalytic performance of the catalyst was tested using a rotating ring disk electrode and an electrochemical workstation. Ultrasonically dispersing the catalyst in a mixed solution of water, ethanol and Nafion, after uniform dispersion, dropwise adding a proper amount of the catalyst on a rotating ring disc electrode, and naturally drying. The electrolyte is 0.1M KOH, and Linear Sweep Voltammetry (LSV) and Cyclic Voltammetry (CV) tests are carried out in the electrolyte saturated by oxygen, and the results show that the catalyst catalyzes and synthesizes H 2 O 2 The selectivity of (a) is almost close to 100%.
Drawings
FIG. 1 is an SEM image of a Zn-N-C electrocatalyst prepared in example 1;
FIG. 2 is an XRD pattern of a Zn-N-C electrocatalyst prepared in example 1;
FIG. 3 is a HADDF-STEM plot of a Zn-N-C electrocatalyst prepared in example 1;
FIG. 4 is H of the Zn-N-C electrocatalyst prepared in example 1 2 O 2 A selectivity curve;
FIG. 5 is the number of electrons transferred in the oxygen reduction reaction by the Zn-N-C electrocatalyst prepared in example 1.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
Step S1: stirring and reacting 600 mu L of pyrrole at 0-5 ℃ for 12h by taking 0.22g of CTAB as a template agent and 2.0g of ammonium persulfate as an oxidant to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing 0.1g of the polypyrrole nanowires obtained in the step S1 in 120mL of methanol, adding 2.38g of zinc nitrate, stirring for 12 hours, then adding 1.64g of 2-methylimidazole, standing for 12 hours, carrying out solid-liquid separation, and drying at 80 ℃;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, keeping the temperature for 3 hours, and then naturally cooling to room temperature;
step S4: and (4) soaking the material obtained in the step S3 in 2mol/L hydrochloric acid at normal temperature for 24h, then carrying out suction filtration, washing with water to be neutral, and drying at 80 ℃ to obtain the Zn-N-C electrocatalyst.
Dispersing 1mg of the prepared Zn-N-C electrocatalyst in a mixed solution of water, ethanol and Nafion, performing ultrasonic dispersion uniformly, dropwise adding a proper amount of the solution onto a ring disk electrode, and airing in the air. The test is carried out by adopting a three-electrode system, the Hg/HgO electrode and the platinum sheet are respectively used as a reference electrode and a counter electrode, and the electrolyte is O 2 Saturated 0.1mol/L KOH aqueous solution. The scanning speed is 10mV/s during the test, and the scanning range is 0V-1.2V (vs.
Example 2
Step S1: stirring and reacting 600 mu L of pyrrole at 0-5 ℃ for 12h by taking 0.22g of CTAB as a template agent and 2.0g of ammonium persulfate as an oxidant to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing 0.2g of the polypyrrole nanowires obtained in the step S1 in 480mL of methanol, adding 9.52g of zinc nitrate, stirring for 12 hours, adding 9.84g of 2-methylimidazole, standing for 12 hours, performing solid-liquid separation, and drying at 80 ℃;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 5 ℃/min under a nitrogen atmosphere, keeping the temperature for 4 hours, and then naturally cooling to room temperature;
step S4: and (5) soaking the material obtained in the step (S3) in 2mol/L hydrochloric acid at normal temperature for 24h, then carrying out suction filtration, washing with water to be neutral, and drying at 80 ℃ to obtain the Zn-N-C electrocatalyst.
Example 3
Step S1: stirring and reacting 600 mu L of pyrrole at 0-5 ℃ for 12h by taking 0.22g of CTAB as a template agent and 2.0g of ammonium persulfate as an oxidant to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing 0.2g of the polypyrrole nanowires obtained in the step S1 in 240mL of methanol, adding 2.38g of zinc nitrate, stirring for 12 hours, adding 13.14g of 2-methylimidazole, standing for 10 hours, performing solid-liquid separation, and drying at 80 ℃;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 5 ℃/min under a nitrogen atmosphere, keeping the temperature for 2 hours, and then naturally cooling to room temperature;
step S4: and (4) soaking the material obtained in the step (S3) in 1mol/L hydrochloric acid at normal temperature for 12h, then carrying out suction filtration, washing with water to be neutral, and drying at 80 ℃ to obtain the Zn-N-C electrocatalyst.
Example 4
Step S1: stirring and reacting 600 mu L of pyrrole at 0-5 ℃ for 12h by taking 0.22g of CTAB as a template agent and 2.0g of ammonium persulfate as an oxidant to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing 0.1g of the polypyrrole nanowires obtained in the step S1 in 120mL of methanol, adding 2.38g of zinc nitrate, stirring for 5 hours, then adding 1.64g of 2-methylimidazole, standing for 10 hours, performing solid-liquid separation, and drying at 80 ℃;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 5 ℃/min under a nitrogen atmosphere, keeping the temperature for 2 hours, and then naturally cooling to room temperature;
step S4: and (5) soaking the material obtained in the step (S3) in 2mol/L hydrochloric acid at normal temperature for 24h, then carrying out suction filtration, washing with water to be neutral, and drying at 80 ℃ to obtain the Zn-N-C electrocatalyst.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.

Claims (5)

1. High-efficiency synthesis of H 2 O 2 The preparation method of the Zn-N-C electrocatalyst is characterized by comprising the following steps: in the Zn-N-C electrocatalyst, metal Zn is loaded on a nitrogen-doped carbon material in a single atom form, and the loading amount of the metal Zn is 5wt% -25 wt%;
the specific preparation process of the Zn-N-C electrocatalyst is as follows:
step S1: stirring pyrrole at 0-5 ℃ by taking CTAB as a template agent and ammonium persulfate as an oxidant to react to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing the polypyrrole nanowires obtained in the step S1 in methanol, adding zinc nitrate, stirring, adding 2-methylimidazole, standing, performing solid-liquid separation, and drying;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 1-10 ℃/min under an inert gas atmosphere, keeping the temperature for 2-4h, and naturally cooling to room temperature;
step S4: and (5) soaking the material obtained in the step (S3) in an acid solution, then carrying out suction filtration, washing with water to be neutral, and drying to obtain the Zn-N-C electrocatalyst.
2. The efficient synthesis of H according to claim 1 2 O 2 The preparation method of the Zn-N-C electrocatalyst is characterized by comprising the following steps: in step S3, the inert gas is one or more of nitrogen, argon or helium.
3. The efficient synthesis of H according to claim 1 2 O 2 The preparation method of the Zn-N-C electrocatalyst is characterized by comprising the following steps: in the step S4, the acid solution is one or more of hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid or acetic acid, the concentration of the acid solution is 0.5-4mol/L, the acid treatment temperature is 25-100 ℃, and the acid treatment time is 2-24 h.
4. The efficient synthesis of H according to claim 1 2 O 2 The preparation method of the Zn-N-C electrocatalyst is characterized by comprising the following specific steps:
step S1: stirring and reacting 600 mu L of pyrrole at 0-5 ℃ for 12h by taking 0.22g of CTAB as a template agent and 2.0g of ammonium persulfate as an oxidant to obtain a polypyrrole nanowire;
step S2: ultrasonically dispersing 0.1g of the polypyrrole nanowires obtained in the step S1 in 120mL of methanol, adding 2.38g of zinc nitrate, stirring for 12 hours, then adding 1.64g of 2-methylimidazole, standing for 12 hours, carrying out solid-liquid separation, and drying at 80 ℃;
step S3: placing the material obtained in the step S2 in a tube furnace, heating to 600 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, keeping the temperature for 3 hours, and then naturally cooling to room temperature;
step S4: and (5) soaking the material obtained in the step (S3) in 2mol/L hydrochloric acid at normal temperature for 24h, then carrying out suction filtration, washing with water to be neutral, and drying at 80 ℃ to obtain the Zn-N-C electrocatalyst.
5. Catalytic synthesis of H by Zn-N-C electrocatalyst prepared according to any one of claims 1-4 2 O 2 The method is characterized by comprising the following specific processes: dispersing 1mg of prepared Zn-N-C electrocatalyst in a mixed solution of water, ethanol and Nafion, after uniform ultrasonic dispersion, taking a proper amount of solution to be dripped on a ring disc electrode, airing in the air, testing by adopting a three-electrode system, wherein an Hg/HgO electrode and a platinum sheet are respectively used as a reference electrode and a counter electrode, and an electrolyte is O 2 Saturated 0.1mol/L KOH aqueous solution, Zn-N-C electrocatalyst catalyzed synthesis of H 2 O 2 The selectivity of (a) is close to 100%.
CN202210318319.3A 2022-03-29 2022-03-29 High-efficiency synthesis of H 2 O 2 Preparation method and application of Zn-N-C electrocatalyst Pending CN114807981A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116646539A (en) * 2023-07-26 2023-08-25 河南工学院 Single-atom-loaded carbon nanotube catalyst and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116646539A (en) * 2023-07-26 2023-08-25 河南工学院 Single-atom-loaded carbon nanotube catalyst and preparation method and application thereof
CN116646539B (en) * 2023-07-26 2023-10-10 河南工学院 Single-atom-loaded carbon nanotube catalyst and preparation method and application thereof

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