CN113652699A - Method for improving activity of hydrogen production by electrocatalysis of graphene - Google Patents
Method for improving activity of hydrogen production by electrocatalysis of graphene Download PDFInfo
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- CN113652699A CN113652699A CN202110759471.0A CN202110759471A CN113652699A CN 113652699 A CN113652699 A CN 113652699A CN 202110759471 A CN202110759471 A CN 202110759471A CN 113652699 A CN113652699 A CN 113652699A
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- 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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
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- 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
- C25B11/055—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
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a method for improving the hydrogen production activity of graphene electrocatalysis, which comprises the following steps: s1, preparing graphene oxide by using graphite as a raw material through a chemical oxidation method; s2, preparing reduced graphene oxide from the graphene oxide prepared in the step S1 by a chemical reduction method; s3, processing the reduced graphene oxide prepared in the step S2 by adopting a plurality of times of linear voltammetry scanning methods. According to the invention, graphene is not subjected to any chemical modification and modification, and is activated by multiple linear volt-ampere scanning, so that the electrocatalytic hydrogen evolution current of graphene is greatly improved, and the catalyst can replace a noble metal Pt/C catalyst to perform electrocatalytic hydrolysis hydrogen production.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a method for improving the activity of hydrogen production by electrocatalysis of graphene.
Background
In order to solve the increasingly serious energy crisis and environmental problems, the development of clean and efficient hydrogen energy is a sustainable and promising method. Due to the single-layer sheet-shaped special structure formed by carbon atoms, the graphene has excellent properties such as high theoretical specific surface area, excellent mechanical strength, good flexibility, high conductivity and the like, and has exciting application prospects in photocatalytic and electrocatalytic hydrogen production.
The hydrogen production catalyst is needed for water electrolysis, photocatalysis and photoelectrocatalysis decomposition of water to produce hydrogen. The best hydrogen production catalyst at present is metal platinum, but platinum is expensive and has a small content in the earth crust, so that the industrial hydrogen production is limited. Therefore, the search for high-efficiency and cheap substitutes is of great significance to the actual industrialization.
The reduction of graphene oxide is an important and low-cost way for preparing graphene, and the obtained graphene is used for electrocatalytic hydrogen production. Yanguang Li et al reported in Journal of American Chemistry Society, 133, 7296, 2011 that reduced graphene oxide was modified on a glassy carbon electrode at 0.5mol/L H2SO4Linear voltammetric scans were performed and showed that the hydrogen evolution current was small even at very negative voltages. Therefore, few documents report that graphene is modified. Yao Zheng et al reported in Nature Communication, 4, 4783, 2014 that N-doped graphene has an overvoltage of-0.56V vs RHE and a current density of 10mA/cm2. Bharskar r.Sathe et al Catalysis Science&Technology, 4, 2023, 2014 reports that B-doped graphene is modified on a glassy carbon electrode at 0.5mol/L of H2SO4Linear voltammetric scanning was performed in solution and the results showed a current density of 10mA/cm2When the hydrogen evolution overvoltage is-0.46V vs RHE. Yuanfu Chen et al reported in International Journal of Hydrogen Energy, 42, 2017 that treatment with Ar plasma and N, S co-doping resulted in graphene foam, which has a much improved electrocatalytic Hydrogen evolution activity compared to undoped graphene foam, with a Hydrogen evolution overpotential of-0.30V vs RHE at 10mA/cm 2. Although the doped modified graphene is improved to a certain extent in electrocatalytic hydrogen production compared with unmodified graphene, the activity is still low, and the difference with the catalytic activity of the traditional noble metal Pt/C is large. The graphene is not chemically modified and modified in the invention, but is modifiedBy electrochemical means: multiple linear volt-ampere scanning treatment greatly reduces the overpotential of the graphene for the electrocatalytic hydrogen evolution at 10mA/cm2At current density, the hydrogen evolution overpotential is about-110 mV.
Disclosure of Invention
Aiming at the defects and problems in the prior art, the invention aims to provide a method for improving the activity of hydrogen production by electrocatalysis of graphene.
The invention is realized by the following technical scheme:
a method for improving the activity of hydrogen production by electrocatalysis of graphene, which comprises the following steps:
s1, preparing graphene oxide by using graphite as a raw material through a chemical oxidation method;
s2, preparing reduced graphene oxide from the graphene oxide prepared in the step S1 by a chemical reduction method;
s3, processing the reduced graphene oxide prepared in the step S2 by adopting a plurality of times of linear voltammetry scanning methods.
The chemical reduction method of step S2 uses sodium borohydride or hydrazine hydrate as a reducing agent; the chemical reduction method is any one of a hydrothermal method, a solvothermal method, a hydrogen-assisted thermal reduction method and a thermal stripping method.
Step S3 specifically includes:
s31, dispersing the reduced graphene oxide prepared in the step S2 in a dispersing agent to form a reduced graphene oxide dispersion liquid, wherein the solubility of the reduced graphene oxide dispersion liquid is 0.5-10 mg/mL, and the dispersing agent is 0.025-0.15 wt% of Nafion water solution;
s32, coating the reduced graphene oxide dispersion liquid on a working electrode, wherein the amount of loaded graphene is 0.01-1.0 mg/cm2The working electrode is a glassy carbon electrode;
s33, putting the working electrode loaded with the reduced graphene oxide on N2Performing linear voltammetric scanning for multiple times in a saturated sulfuric acid solution; the counter electrode is a platinum wire (disk, net) electrode, and the reference electrode can be a saturated calomel electrode or an Ag/AgCl electrode; the initial voltage of linear volt-ampere scanning is-1.2 to-0.7V, the final voltage is 0 to 0.6V, the scanning speed is 5 to 100mV/s, and the scanning times are 400 to 2000.
After the multiple linear volt-ampere scanning is finished, when the hydrogen evolution current density is 10mA/cm2And the overvoltage is about-0.1V, so that the electro-catalysis hydrogen production performance of the graphene is greatly improved.
Compared with the prior art, the method does not carry out any chemical modification and modification on the graphene, only carries out activation through multiple times of linear volt-ampere scanning, greatly improves the electrocatalytic hydrogen evolution current of the graphene, and can replace a noble metal Pt/C catalyst to carry out electrocatalytic hydrolysis hydrogen production.
Drawings
FIG. 1 is a linear voltammetric scan of graphene before and after activation in example 1 of the present invention;
FIG. 2 is a plot of a linear voltammetric scan of a Pt/C catalyst of example 1 of the present invention;
FIG. 3 is a plot of linear voltammetric scans of graphene before and after activation in example 2 of the present invention;
FIG. 4 is a linear voltammetric scan of graphene before and after activation in example 3 of the present invention;
FIG. 5 is a plot of linear voltammetric scans of graphene before and after activation in example 4 of the present invention;
fig. 6 is a linear voltammogram of graphene before and after activation in example 5 of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1
The technical route is as follows: (1) graphite → (2) graphite oxide → (3) graphene oxide → (4) hydrazine hydrate reduction of graphene oxide to graphene → (5) graphene working electrode → (6) multiple linear voltammetry scans of activated graphene.
(1) Graphite: the purity is 99.9 percent
(2) And (3) graphite oxide: weighing 12g of graphite with the purity of 99.9% in the step (1), adding 10g of potassium peroxodisulfate (analytically pure), 10g of phosphorus pentoxide (analytically pure) and 48mL of concentrated sulfuric acid (mass fraction of 98%) into a round-bottom flask, stirring in a water bath at 80 ℃ for reacting for 4.5h, adding 500mL of deionized water after the reaction is finished, filtering and washing to be neutral, and drying at 60 ℃ to obtain pre-oxidized graphite. Weighing 2g of the pre-oxidized graphite, adding 1g of sodium nitrate (analytically pure) and 46mL of concentrated sulfuric acid, stirring for 30min under ice bath, slowly adding 6g of potassium permanganate (analytically pure), and reacting for 45min under ice bath; then heating the mixture to 35 ℃, stirring and reacting for 2 hours, and then slowly dropwise adding 90mL of deionized water; the mixture was rapidly heated to 95 ℃ and stirred for 15 min. And finally, adding 144mL of deionized water for dilution, adding 30mL of hydrogen peroxide (mass fraction of 30%), stirring for 30min, performing centrifugal washing on the mixture until the pH value is 6, and drying for 48h at 80 ℃ to obtain the graphite oxide sheet.
(3) Ultrasonically dispersing graphite oxide in water to obtain graphene oxide with the concentration of 1 mg/mL.
(4) And (3) taking 200mL of graphene oxide in the step (3), adding 0.2mL of hydrazine hydrate (80 wt%) into water bath at 90 ℃, stirring for reaction for 2h, filtering, washing with water for several times, and drying at 80 ℃.
(5) And (3) adding 5mg of the graphene obtained in the step (4) into 2mL of Nafion solution (0.075 wt%), performing ultrasonic dispersion for 2h, dropwise coating 6 mu L of graphene suspension on a clean glassy carbon electrode, and naturally drying.
(6) The working electrode prepared in the step (5) is at 0.5mol/L of N2Saturated H2SO4In the solution, a counter electrode is a Pt wire electrode, a reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 600 times for activation.
Fig. 1 is a linear voltammogram of graphene before and after activation in this example, and fig. 2 is a linear voltammogram of Pt/C in this example. As can be seen from the graphs 1 and 2, the electrocatalytic hydrogen evolution current of the activated graphene is greatly increased, and the current density is 10mA/cm2When the catalyst is used, the overvoltage is-0.117V, and the Pt/C ratio of the traditional noble metal catalyst is 10mA/cm2At current density, the overvoltage was-0.1V.
Example 2
The technical route is as follows: (1) graphite → (2) graphite oxide → (3) graphene oxide → (4) sodium borohydride reduction of graphene oxide to graphene → (5) graphene working electrode → (6) multiple linear voltammetry scans activate graphene.
(1) Same as example 1
(2) Same as example 1
(3) Same as example 1
(4) And (4) taking 200mL of graphene oxide in the step (3), adding sodium borohydride, and stirring in a water bath at 80 ℃ to react for 10 hours. Filtering, washing with water for several times, and drying at 80 deg.C.
(5) Same as example 1
(6) The working electrode prepared in the step (5) is at 0.5mol/L of N2Saturated H2SO4In the solution, a counter electrode is a Pt wire electrode, a reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 500 times for activation.
FIG. 3 is a linear voltammetry scan of graphene before and after activation in this example, and it can be seen from FIG. 3 that the current density of graphene after activation is 10mA/cm2The overvoltage was-0.116V.
Example 3
The technical route is as follows: (1) graphite → (2) graphite oxide → (3) graphene oxide → (4) reduction of the graphene oxide by a hydrothermal method to graphene → (5) graphene working electrode → (6) multiple times of linear voltammetry scanning to activate the graphene.
(1) Same as example 1
(2) Same as example 1
(3) Same as example 1
(4) Adding 80mL of the graphene oxide in the step (3) into a reaction kettle of 100mL of polytetrafluoroethylene, reacting for 12h at 160 ℃, filtering, washing with water for several times, and drying at 80 ℃.
(5) Same as example 1
(6) The working electrode prepared in the step (5) is at 0.5mol/L of N2Saturated H2SO4In the solution, a counter electrode is a Pt wire electrode, a reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 800 times for activation.
FIG. 4 is a linear voltammetry scan of graphene before and after activation in this example, and it can be seen from FIG. 4 that the current density of graphene after activation is 10mA/cm2The overvoltage was-0.125V.
Example 4
The technical route is as follows: (1) the method comprises the steps of preparing graphene oxide from graphite → (2) graphite oxide → (3) graphene oxide → (4) a solvothermal method for reducing the graphene oxide into graphene → (5) a graphene working electrode → (6) multiple times of linear voltammetry scanning for activating the graphene.
(1) Same as example 1
(2) Same as example 1
(3) Taking 80mg of graphite oxide in the step (2), adding the graphite oxide into 80mL of dimethyl sulfoxide, and ultrasonically dispersing for 2h
(4) And (3) adding the graphene oxide in the step (3) into a 100mL reaction kettle made of polytetrafluoroethylene, reacting for 12h at 180 ℃, filtering ethanol, washing for a plurality of times, and drying at 80 ℃.
(5) Same as example 1
(6) The working electrode prepared in the step (5) is at 0.5mol/L of N2Saturated H2SO4In the solution, a counter electrode is a Pt wire electrode, a reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 600 times for activation.
FIG. 5 is a linear voltammetry scan of graphene before and after activation in this example, and it can be seen from FIG. 5 that the current density of graphene after activation is 10mA/cm2The overvoltage was-0.119V.
Example 5
The technical route is as follows: (1) graphite → (2) graphite oxide → (3) hydrogen-assisted thermal reduction of graphite oxide to graphene → (4) graphene working electrode → (5) multiple linear voltammetry scans activate graphene.
(1) Same as example 1
(2) Same as example 1
(3) And (2) placing graphite oxide in a nitrogen-hydrogen mixed gas flow, wherein the volume concentration of hydrogen is 5%, the flow rate is 60mL/min, heating the mixture to 500 ℃ at the heating rate of 15 ℃/min, keeping for 2h, and finally cooling to room temperature in the nitrogen-hydrogen mixed gas (the flow rate is 60mL/min) to obtain the graphene.
(4) 5mg of the obtained graphene is added into 2mL of Nafion solution (0.075 wt%), ultrasonic dispersion is carried out for 2h, 6 mu L of graphene suspension is taken out and is dripped on a clean glassy carbon electrode, and natural drying is carried out.
(5) The prepared working electrode has N of 0.5mol/L2Saturated H2SO4In the solution, a counter electrode is a Pt wire electrode, a reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, and the scanning electrode is used for scanningThe activation was carried out at a scanning speed of 50mV/s and at 900 scanning times.
FIG. 6 is a linear voltammetry scan of graphene before and after activation in this example, and it can be seen from FIG. 6 that the current density of graphene after activation is 10mA/cm2The overvoltage was-0.115V.
The foregoing merely represents preferred embodiments of the invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes, modifications and substitutions can be made without departing from the spirit of the present invention, and these are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A method for improving the activity of hydrogen production by electrocatalysis of graphene, which is characterized by comprising the following steps:
s1, preparing graphene oxide by using graphite as a raw material through a chemical oxidation method;
s2, preparing reduced graphene oxide from the graphene oxide prepared in the step S1 by a chemical reduction method;
s3, processing the reduced graphene oxide prepared in the step S2 by adopting a plurality of times of linear voltammetry scanning methods.
2. The method for improving the activity of graphene in electrocatalytic hydrogen production according to claim 1, wherein the method comprises the following steps: the chemical reduction method of step S2 uses sodium borohydride or hydrazine hydrate as a reducing agent; the chemical reduction method is any one of a hydrothermal method, a solvothermal method, a hydrogen-assisted thermal reduction method and a thermal stripping method.
3. The method for improving the activity of hydrogen production by electrocatalysis of graphene according to claim 1, wherein the step S3 specifically comprises:
s31, dispersing the reduced graphene oxide prepared in the step S2 in a dispersing agent to form a reduced graphene oxide dispersion liquid;
s32, coating the reduced graphene oxide dispersion liquid on a working electrode;
s33, putting the working electrode loaded with the reduced graphene oxide on N2Multiple linear voltammetric scans were performed in saturated sulfuric acid solution.
4. The method for improving the hydrogen production activity of graphene electrocatalysis according to claim 3, characterized in that: the solubility of the reduced graphene oxide in the dispersion liquid prepared in the step S31 is 0.5-10 mg/mL; the dispersant is 0.025-0.15 wt% Nafion water solution.
5. The method for improving the hydrogen production activity of graphene electrocatalysis according to claim 3, characterized in that: the amount of graphene loaded on the working electrode in the step S32 is 0.01-1.0 mg/cm2The working electrode is a glassy carbon electrode.
6. The method for improving the hydrogen production activity of graphene electrocatalysis according to claim 3, characterized in that: in the step S33, the initial voltage of linear voltammetry scanning is-1.2 to-0.7V, the final voltage is 0 to 0.6V, the scanning speed is 5 to 100mV/S, and the scanning times are 400 to 2000.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114293218A (en) * | 2021-12-08 | 2022-04-08 | 国网辽宁省电力有限公司经济技术研究院 | Water electrolysis hydrogen production electrode based on graphene aerogel and synthesis method thereof |
| CN114875430A (en) * | 2022-04-19 | 2022-08-09 | 中国科学院过程工程研究所 | Graphite-based bifunctional electrosynthesis hydrogen peroxide catalytic material and preparation method thereof |
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Cited By (3)
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| CN114293218A (en) * | 2021-12-08 | 2022-04-08 | 国网辽宁省电力有限公司经济技术研究院 | Water electrolysis hydrogen production electrode based on graphene aerogel and synthesis method thereof |
| CN114875430A (en) * | 2022-04-19 | 2022-08-09 | 中国科学院过程工程研究所 | Graphite-based bifunctional electrosynthesis hydrogen peroxide catalytic material and preparation method thereof |
| CN114875430B (en) * | 2022-04-19 | 2024-05-03 | 中国科学院过程工程研究所 | Graphite-based bifunctional electrosynthesis hydrogen peroxide catalytic material and preparation method thereof |
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