CN110117797B - Electrolytic cell and application thereof in hydrogen production by electrolyzing water - Google Patents
Electrolytic cell and application thereof in hydrogen production by electrolyzing water Download PDFInfo
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- CN110117797B CN110117797B CN201810120771.2A CN201810120771A CN110117797B CN 110117797 B CN110117797 B CN 110117797B CN 201810120771 A CN201810120771 A CN 201810120771A CN 110117797 B CN110117797 B CN 110117797B
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- C—CHEMISTRY; METALLURGY
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B1/02—Hydrogen or oxygen
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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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
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- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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- 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
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Abstract
The application discloses an electrolytic cell, which is characterized by comprising an anode electrode plate, a cathode electrode plate, a bipolar membrane, anode chamber electrolyte and cathode chamber electrolyte; wherein the anode electrode plate comprises an anode catalyst, and the cathode electrode plate comprises a cathode catalyst; the anode catalyst and the cathode catalyst are both Ru-RuO2a/CNT composite catalyst; the anolyte and the catholyte are separated by the bipolar membrane; the electrolyte of the anode chamber is alkaline solution, and the electrolyte of the cathode chamber is acidic solution. The electrolytic cell can drive the generation of electrolytic water under the potential of 0.65V and reach 10mA cm under the potential of 0.73V‑2The current density of the electrolytic cell is far lower than the theoretical potential of the electrolytic water in the traditional electrolytic cell of 1.23V, so that the energy consumption is greatly reduced, and the electrolytic cell has potential application value.
Description
Technical Field
The present application relates to a Ru-RuO2/CNT composite material based on Ru-RuO2An acid-alkali hybrid electrolytic cell of a/CNT composite material catalyst and a water electrolysis hydrogen production device belong to the field of materials, batteries and water electrolysis hydrogen production.
Background
Hydrogen energy, which is the simplest energy source and the most abundant resource on the earth, has been recognized as the most potential clean energy source because H2Almost has no pollution, and can reduce the dependence on fossil energy to deal with future energySafety issues with source supply and reduced greenhouse gas increase. Currently, the biggest challenge in limiting hydrogen energy to large-scale applications is the high cost and energy consumption in the hydrogen production process. The electrolysis of water is regarded as the most promising hydrogen production technology, and in this way, the influence of instability of renewable energy sources such as wind energy, solar energy and the like can be eliminated. However, the use of low efficiency, high energy demand electrolysis is a deliberate consideration when evaluating the benefits and economic viability of hydrogen production. There is therefore still much room for exploring low-cost, highly active electrocatalysts and for selecting an electrolytic cell which maximizes the utilization of the activity of the electrocatalyst.
The electrochemical reactions of electrolyzed water include cathodic Hydrogen Evolution Reaction (HER) and anodic Oxygen Evolution Reaction (OER). However, most hydrogen-producing catalysts are best active in acidic media (such as Pt/C), and most oxygen-producing catalysts are best active in basic media (such as RuO)2). The above-mentioned maladjustment of the matching of the electrocatalyst and the electrolyte makes the need for rational design of the cell unit, development of low-cost and highly active electrocatalysts urgent, since only then the energy consumption for the electrolysis of water is significantly reduced.
Disclosure of Invention
According to one aspect of the present application, there is provided an electrolytic cell employing Ru-RuO2the/CNT composite catalyst is used as an anode catalyst and a cathode catalyst at the same time, can drive the generation of electrolytic water under the potential of 0.65V and reaches 10mA cm under the potential of 0.73V-2The current density of the electrolytic cell is far lower than the theoretical potential of the electrolytic water in the traditional electrolytic cell, namely 1.23V, so that the energy consumption is greatly reduced.
The electrolytic cell is characterized by comprising an anode electrode plate, a cathode electrode plate, a bipolar membrane, anode chamber electrolyte and cathode chamber electrolyte;
wherein the anode electrode plate comprises an anode catalyst, and the cathode electrode plate comprises a cathode catalyst;
the anode catalyst and the cathode catalyst are both Ru-RuO2a/CNT composite catalyst;
the anolyte and the catholyte are separated by the bipolar membrane;
the electrolyte of the anode chamber is alkaline solution, and the electrolyte of the cathode chamber is acidic solution.
As an embodiment, the Ru-RuO2The preparation method of the/CNT composite catalyst at least comprises the following steps:
a) contacting a solution containing Ru ions with the carbon nano tube subjected to acid treatment, and reducing to obtain a Ru/CNT precursor;
b) partially oxidizing the Ru/CNT precursor obtained in the step a) to obtain the Ru-RuO2a/CNT composite catalyst.
As an embodiment, the acid-treated carbon nanotube is prepared by a method comprising the steps of: and (2) placing the carbon nano tube in an acid solution, treating for not less than 6 hours at 80-100 ℃, washing and drying to obtain the carbon nano tube. Preferably, the carbon nanotube is prepared by placing the carbon nanotube in an acid solution, treating the carbon nanotube at 90 ℃ for 8 hours, washing the carbon nanotube with ionized water, and freeze-drying the carbon nanotube.
Preferably, the acid solution is a mixture of concentrated nitric acid (mass fraction of 68%) and concentrated sulfuric acid (mass fraction of 98%), and the volume ratio is VHNO3：VH2SO4= 3：1。
In one embodiment, the step a) is to mix a solution containing Ru ions with a solution containing acid-treated carbon nanotubes, adjust the pH of the system to 6.5-7.5, and add a reducing agent to obtain the Ru/CNT precursor.
Preferably, step a) is mixing the solution containing Ru ions with the solution containing acid-treated carbon nanotubes, followed by NaHCO3And (3) adjusting the pH value of the system to 7 by using the solution, stirring for not less than 10 hours, placing the system in an inactive atmosphere, adding a reducing agent, and reacting for not less than 1 hour at 70-90 ℃ to obtain the Ru/CNT precursor.
The inert atmosphere is at least one selected from nitrogen, helium, neon, argon and xenon.
Preferably, the solution containing Ru ions is obtained by dissolving a Ru soluble salt in water. Further preferably, the Ru is solubleThe salt being RuCl3Or RuCl containing water of crystallization3。
As an embodiment, the mass ratio of the number of moles of Ru element in the solution containing Ru ions in the step a) to the acid-treated carbon nanotube CNT is:
Ru：CNT = 0.01~ 0.05mol：1 g。
in one embodiment, the concentration of Ru ions in the solution containing Ru ions in step a) is 0.01-0.05 mol/L.
Preferably, the reducing agent is NaBH4。
As an embodiment, step b) is a partial oxidation of the Ru/CNT precursor to: and (3) calcining the Ru/CNT precursor in air at 150-250 ℃ for 2-4 hours.
Preferably, the anode compartment electrolyte is a KOH solution. Further preferably, the electrolyte in the anode chamber is 0.8-1.2M KOH solution. Still further preferably, the anode compartment electrolyte is a 1.0M KOH solution.
Preferably, the electrolyte in the cathode chamber is H2SO4And (3) solution. Further preferably, the electrolyte of the anode chamber is 0.3-0.8M of H2SO4And (3) solution. Even more preferably, the anodic compartment electrolyte is 0.5M H2SO4And (3) solution.
As an embodiment, the anode electrode sheet and the cathode electrode sheet are both Ru-RuO-containing2The slurry of the/CNT composite catalyst is coated on a glassy carbon electrode and dried to obtain the catalyst.
Preferably, the anode electrode sheet and the cathode electrode sheet have Ru-RuO2The loading amount of the/CNT composite catalyst is 1-2 mg cm-2。
As a specific embodiment, the method for preparing the electrolytic cell comprises the following steps:
（1）Ru-RuO2synthesis of/CNT composite catalyst: with RuCl3·xH2Slowly dripping the CNT solution treated by the acid solution by taking O as a ruthenium source and deionized water as a solvent to form a uniformly mixed solution; preparation of 0.3M NaHCO3Adjusting the solutionThe pH value of the solution is 7, and the solution is stirred for a certain time; adding a reducing agent NaBH into the solution4Preparing a precursor Ru/CNT; the obtained precursor Ru/CNT is placed in a tube furnace to be calcined at low temperature in the air atmosphere to realize Ru-RuO2Preparing a/CNT composite catalyst;
(2) assembly of acid-base hybrid cell: at 0.5M H2SO4As a catholyte, 1.0M KOH as an anolyte, using a bipolar membrane to separate the cathodic and anodic compartments, assembling an acid-base hybrid electrolytic cell with Ru-RuO2the/CNT is respectively used as a cathode catalyst and an anode catalyst of an acid-base hybrid electrolytic cell to carry out electrolytic water performance test.
According to a further aspect of the present application there is provided the use of any of the above described electrolytic cells for the electrolysis of water to produce hydrogen and/or oxygen.
Preferably, the driving potential for hydrogen production and/or oxygen production by water electrolysis is not less than 0.65V.
Preferably, the electrolytic cell achieves 10mA cm-2The potential of the current density of (a) does not exceed 0.75V.
The beneficial effects that this application can produce include at least:
1) the electrolytic cell provided by the application adopts Ru-RuO2the/CNT composite material is used as an anode catalyst and a cathode catalyst at the same time; Ru-RuO2the/CNT composite material is an electrode catalyst with low cost and high activity, and can effectively improve the hydrogen production and oxygen production activities of the catalyst under various pH media.
2) The electrolytic cell provided by the application provides a new solution for expanding the selection of the catalyst and the electrolyte, and more importantly, the acid-alkali hybrid electrolytic cell can remarkably reduce the energy consumption of water electrolysis and reach 10mA cm at the potential of 0.73V-2The current density of the electrolytic cell is far lower than the theoretical potential of the electrolytic water in the traditional electrolytic cell, namely 1.23V, and the application value is huge.
Drawings
FIG. 1 shows sample 1#X-ray diffraction pattern of (a).
FIG. 2 shows sample 1#Transmission electron micrograph (D).
FIG. 3 shows sample 1#Hydrogen production performance under different mediums.
FIG. 4 shows sample 1#Oxygen evolution performance under different media.
FIG. 5 is a schematic diagram of the electrolytic cell of the present application for producing hydrogen and oxygen by electrolyzing water.
FIG. 6 shows an electrolytic cell 1#And D1#Potential-current density comparison graph of (a).
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Unless otherwise specified, the raw materials in the examples of the present application were purchased commercially and used without treatment; the test conditions of the instrument all adopt the parameters recommended by the manufacturer.
In the examples, bipolar membranes were purchased from Beijing moisturizing membranes technology development, Inc.
In the examples, transmission electron microscopy of the samples was characterized using a high resolution transmission electron microscope (Tecnai F20).
In the examples, X-ray diffraction analysis (XRD) of the samples was characterized using Miniflex 600.
In the examples, the electrochemical performance was measured using a CHI760E model electrochemical workstation of Shanghai Chenghua, Inc. for the cell, and a CHI102 model glassy carbon electrode used in combination with a CHI760E model electrochemical workstation for the cell was used for the glassy carbon electrode.
Example 1 sample 1#~3#Preparation of
#Preparation of sample 1
First, a mixed acid solution (concentrated nitric acid with a mass fraction of 68% and concentrated sulfuric acid with a mass fraction of 98%) for carbon nanotubes was prepared at a volume ratio of V (HNO)3):V(H2SO4) = 3: 1) at 90 ℃ for 8 h, washed with deionized water, and freeze-dried for use. Then, 109 mg of RuCl was weighed3·3H2O, dissolved in 30 ml of deionized water and stirred until uniformly dispersed. To the above solution was slowly dropped a solution dissolved in 20 ml of deionized water in which 50mg of CNTs were dispersed to obtain a mixed solution. Subsequently, 0.3M NaHCO was prepared3The solution is used as a buffer solutionThe solution was slowly added dropwise to the above mixed solution to adjust pH = 7, and stirred at room temperature for 18 h. The solution was transferred to a three-necked flask, N2Heating to 80 deg.C in oil bath, and slowly adding NaBH4(5 ml, 5wt% aqueous solution) and reacted for 2 h. And cooling to room temperature after the reaction is finished, taking out the solution, performing suction filtration and washing by using deionized water, and performing freeze drying to obtain the precursor Ru/CNT. Putting the obtained precursor Ru/CNT into a tube furnace, and calcining at the low temperature of 200 ℃ for 3 h in the air atmosphere to obtain the Ru-RuO2the/CNT composite catalyst, denoted as sample 1#。
#Preparation of sample 2
The preparation steps and the raw material ratios are the same as those of sample 1#Except that RuCl3·3H2The mass of O was changed to 150mg, resulting Ru-RuO2the/CNT composite catalyst, denoted as sample 2#。
#Preparation of sample 3
The preparation steps and the raw material ratios are the same as those of sample 1#Except that the partial oxidation was carried out at 190 ℃ for 4 hours, as sample 3#。
Example 2 sample 1#~3#Is characterized by
For sample 1 respectively#~3#X-ray diffraction analysis was performed. With sample 1#As a representative, its XRD spectrum is similar to that of Ru and RuO2The standard spectrum pair of (a) is shown in figure 1. As can be seen from FIG. 1, both the metallic Ru and the oxidized RuO were present in the sample2。
For sample 1 respectively#~3#Transmission electron microscopy analysis was performed.
The scanning electron microscope shows that: ru and RuO distributed on carbon nanotubes2The particle size of the particles is uniform and is between 2 and 5 nm. With sample 1#As a representative, scanning thereofThe electron micrograph is shown in FIG. 2.
Example 3 electrochemical hydrogen and oxygen production test
5 mg of sample 1#Dispersing in 30 μ l ethanol +50 μ l Nafion +420 μ l deionized water, ultrasonically dispersing to obtain slurry, and dripping 6 μ l solution onto glassy carbon electrode surface at 0.5M H2SO4Electrochemical hydrogen and oxygen production tests are carried out in 1.0M PBS and 1.0M KOH electrolyte. The results are shown in FIGS. 4 and 5.
Example 4 electrolytic cell 1#And D1#Preparation of
Respectively with sample 1#And RuO obtained from commercial purchase2As a cathode catalyst and an anode catalyst, an electrolytic cell was prepared.
#Preparation of the electrolytic cell 1
The cell was assembled in the manner shown in figure 5.
The anode and cathode are the same: 5 mg of sample 1#Dispersing in a mixed solution of 30 mul ethanol, 50 mul Nafion and 420 mul deionized water, performing ultrasonic treatment for half an hour, and dripping 100uL slurry on a glassy carbon electrode by using a liquid transfer gun to prepare the electrode. And (4) placing the electrode under an infrared lamp, baking and drying, and then using for electrolytic cell assembly.
A diaphragm: a bipolar membrane is used.
The anode chamber and the cathode chamber separate the anolyte from the catholyte through a bipolar membrane, so that the cathode and the anolyte are prevented from undergoing a neutralization reaction.
Electrolyte in anode chamber: 1.0M KOH solution.
Electrolyte in cathode chamber: 0.5M H2SO4And (3) solution.
After assembly into the cell, 1.0M KOH solution and 0.5M H was added2SO4Respectively injected into the anode chamber and the cathode chamber to obtain an electrolytic cell, denoted as electrolytic cell 1#。
#Preparation of comparative electrolytic cell D1
The preparation steps and the raw material ratio are the same as those of the electrolytic cell 1#Except as a commercial RuO2Substitute for sample 1#As anode catalysisAgent, replacement of sample 1 by Pt/C#As cathode catalyst, the resulting cell was designated D1#。
Example 5 electrolytic cell 1#And D1#Performance measurement of
Respectively to the electrolytic cell 1#And D1#The electrochemical performance of (2) was measured, and the results are shown in FIG. 6. As can be seen from the figure, the electrolytic cell 1 adopting the technical scheme of the application#The drive of the electrolyzed water is realized only by 0.65V and reaches 10mA cm under the potential of 0.73V-2The current density of the electrolytic cell is far lower than the theoretical potential of the electrolytic water in the traditional electrolytic cell, namely 1.23V, so that the energy consumption is greatly reduced.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (14)
1. An electrolytic cell is characterized by comprising an anode electrode plate, a cathode electrode plate, a bipolar membrane, anode chamber electrolyte and cathode chamber electrolyte;
wherein the anode electrode plate comprises an anode catalyst, and the cathode electrode plate comprises a cathode catalyst;
the anode catalyst and the cathode catalyst are both Ru-RuO2a/CNT composite catalyst;
the anode compartment electrolyte and the cathode compartment electrolyte are separated by the bipolar membrane;
the electrolyte of the anode chamber is alkaline solution, and the electrolyte of the cathode chamber is acidic solution.
2. The electrolytic cell of claim 1 wherein the Ru-RuO2The preparation method of the/CNT composite catalyst at least comprises the following steps:
a) contacting a solution containing Ru ions with the carbon nano tube subjected to acid treatment, and reducing to obtain a Ru/CNT precursor;
b) partially oxidizing the Ru/CNT precursor obtained in the step a) to obtain the Ru-RuO2a/CNT composite catalyst.
3. The electrolytic cell of claim 2, wherein the step a) is to mix a solution containing Ru ions with a solution containing acid-treated carbon nanotubes, adjust the pH of the system to 6.5-7.5, and add a reducing agent to obtain the Ru/CNT precursor.
4. The electrolytic cell of claim 3 wherein the reducing agent is NaBH4。
5. The electrolytic cell of claim 2, wherein step b) is a partial oxidation of the Ru/CNT precursor to: and (3) calcining the Ru/CNT precursor in air at 150-250 ℃ for 2-4 hours.
6. The electrolytic cell of claim 1 wherein the anode compartment electrolyte is a KOH solution.
7. The electrolytic cell of claim 6, wherein the electrolyte in the anode chamber is a KOH solution of 0.8-1.2 mol/L.
8. The electrolytic cell of claim 7 wherein the anode compartment electrolyte is a 1.0mol/L KOH solution.
9. The electrolytic cell of claim 1 wherein the cathode compartment electrolyte is H2SO4And (3) solution.
10. The electrolytic cell of claim 9, wherein the electrolyte in the cathode chamber is 0.3 to 0.8mol/LH2SO4And (3) solution.
11. The electrolytic cell of claim 10 wherein the cathode compartment electrolyte is 0.5mol/L H2SO4And (3) solution.
12. The electrolytic cell of claim 1, wherein the anode and cathode electrode tabs are each Ru-RuO containing2The slurry of the/CNT composite catalyst is coated on a glassy carbon electrode and dried to obtain the catalyst.
13. Use of an electrolytic cell according to any one of claims 1 to 12 for the electrolysis of water to produce hydrogen and/or oxygen.
14. Use according to claim 13, wherein the driving potential for hydrogen production and/or oxygen production from water electrolysis is not less than 0.65V.
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| CN111534830B (en) * | 2020-05-20 | 2021-07-16 | 南京工业大学 | Device and method for producing high-purity hydrogen by electrolyzing water |
| CN115159574B (en) * | 2021-03-17 | 2023-11-17 | 中国科学院福建物质结构研究所 | Preparation method and application of two-dimensional transition metal sulfur compound |
| CN113774417B (en) * | 2021-09-14 | 2022-05-31 | 合肥工业大学 | Water electrolysis device for producing hydrogen and oxygen by bipolar capacitance instead of ion diaphragm separation |
| CN114000164A (en) * | 2021-11-03 | 2022-02-01 | 深圳市橘井舒泉技术有限公司 | Novel oxygen evolution electrode and preparation method thereof |
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