CN110117797A - A kind of electrolytic cell and its application in water electrolysis hydrogen production - Google Patents
A kind of electrolytic cell and its application in water electrolysis hydrogen production Download PDFInfo
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- CN110117797A CN110117797A CN201810120771.2A CN201810120771A CN110117797A CN 110117797 A CN110117797 A CN 110117797A CN 201810120771 A CN201810120771 A CN 201810120771A CN 110117797 A CN110117797 A CN 110117797A
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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
- 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
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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
- C25B11/091—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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- 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
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- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
This application discloses a kind of electrolytic cells, which is characterized in that including anode electrode film, cathode electrode sheet, bipolar membrane, anode chamber's electrolyte and cathode chamber electrolyte；Wherein, the anode electrode film includes anode catalyst, and the cathode electrode sheet includes cathod catalyst；The anode catalyst and the cathod catalyst are Ru-RuO2/ CNT complex catalyst；The anolyte and the catholyte are separated by the bipolar membrane；Anode chamber's electrolyte is alkaline solution, and the cathode chamber electrolyte is acid solution.The generation of electrolysis water can be driven in the electrolytic cell under the current potential of 0.65V, and reaches 10mA cm under the current potential of 0.73V‑2Current density greatly reduce energy consumption well below the theoretical potential 1.23V of electrolysis water in traditional electrolyte pond, have potential using value.
Description
Technical field
This application involves a kind of Ru-RuO2/ CNT composite material is based on Ru-RuO2The Acid-Base of/CNT composite catalyst
Heterozygosis electrolytic cell and device for preparing hydrogen belong to material, battery, water electrolysis hydrogen production field.
Background technique
Hydrogen Energy, most simple as forming, a kind of the most abundant energy of resource, has been acknowledged as most potential on the earth
Clean energy resource, because of H2It is almost pollution-free, the dependence to fossil energy can be reduced, is asked with coping with the safety of future energy supply
Inscribe and reduce the increase of greenhouse gases.Currently, the ultimate challenge that limitation Hydrogen Energy obtains large-scale application is in hydrogen production process
Cost and energy consumption it is too high.Electrolysis water is considered as most promising production hydrogen technology, in this way, can eliminate wind energy, too
The instable influence of the renewable energy such as positive energy.However, use is low when to assess the interests and economic feasibility that produce hydrogen
Efficiency, high energy demand electrolysis mode must consider carefully.Therefore, much room still explores inexpensive, high activity
The electrolytic cell that elctro-catalyst and selection can make the activity of elctro-catalyst maximize the use.
The electrochemical reaction of electrolysis water includes that (OER) is reacted in cathode hydrogen evolution reaction (HER) with Oxygen anodic evolution.However, mostly
It is best (such as Pt/C) that number produces hydrogen catalyst activity in acid medium, most of to produce VPO catalysts activity is most in alkaline medium
Good (such as RuO2).The case where collocation imbalance of above-mentioned elctro-catalyst and electrolyte, so that rationally designing electrolytic cell device, exploitation
Low cost and the demand of high activity elctro-catalyst become extremely urgent, because only that in this way, the energy consumption of electrolysis water just can significantly drop
It is low.
Summary of the invention
According to the one aspect of the application, a kind of electrolytic cell is provided, which uses Ru-RuO2/ CNT compound is urged
Agent is used as anode catalyst and cathod catalyst simultaneously, can be driven the generation of electrolysis water under the current potential of 0.65V, and
Reach 10mA cm under the current potential of 0.73V-2Current density, well below the theoretical potential of electrolysis water in traditional electrolyte pond
1.23V greatly reduces energy consumption.
The electrolytic cell, which is characterized in that including anode electrode film, cathode electrode sheet, bipolar membrane, anode chamber's electrolyte
With cathode chamber electrolyte；
Wherein, the anode electrode film includes anode catalyst, and the cathode electrode sheet includes cathod catalyst；
The anode catalyst and the cathod catalyst are Ru-RuO2/ CNT complex catalyst；
The anolyte and the catholyte are separated by the bipolar membrane；
Anode chamber's electrolyte is alkaline solution, and the cathode chamber electrolyte is acid solution.
As an implementation, the Ru-RuO2The preparation method of/CNT complex catalyst includes at least following step
It is rapid:
A) after contacting the solution containing Ru ion with the carbon nanotube through peracid treatment, Ru/CNT forerunner is obtained through reduction
Body；
B) the resulting Ru/CNT presoma of step a) is subjected to partial oxidation, obtains the Ru-RuO2/ CNT compound is urged
Agent.
As an implementation, the carbon nanotube through peracid treatment is prepared by method comprising the following steps
To: carbon nanotube is placed in acid solution, the processing no less than after 6 hours at 80~100 DEG C, it is washed, be dried to obtain.It is preferred that
Carbon nanotube is placed in acid solution by ground, and after handling 8h at 90 DEG C, through ion water washing, freeze-drying is obtained.
Preferably, the acid solution is the mixing of concentrated nitric acid (mass fraction 68%) and the concentrated sulfuric acid (mass fraction 98%)
Object, volume ratio VHNO3: VH2SO4=3:1.
As an implementation, step a) be will the solution containing Ru ion with contain the carbon nanotube through peracid treatment
Solution mixing, and after system pH is adjusted to 6.5~7.5, reducing agent is added and obtains Ru/CNT presoma.
Preferably, step a) is to mix the solution containing Ru ion and the solution containing the carbon nanotube through peracid treatment
It closes, then uses NaHCO3System pH is adjusted to 7 by solution, and is stirred no less than after 10 hours, and system is placed under inert atmosphere,
Reducing agent is added, reaction is no less than 1 hour to get Ru/CNT presoma is arrived at 70~90 DEG C.
The inert atmosphere is selected from least one of nitrogen, helium, neon, argon gas, xenon.
Preferably, the solution containing Ru ion is dissolved in water by Ru soluble-salt and obtains.It is further preferred that the Ru
Soluble-salt is RuCl3Or the RuCl containing the crystallization water3。
As an implementation, the molal quantity of Ru element and described through peracid in the solution containing Ru ion in step a)
The mass ratio of the carbon nanotube CNT of processing are as follows:
Ru:CNT=0.01~0.05mol:1g.
As an implementation, in step a) in the solution containing Ru ion Ru ion concentration be 0.01~
0.05mol/L。
Preferably, the reducing agent is NaBH4。
As an implementation, step b) is that the Ru/CNT presoma is carried out partial oxidation are as follows: by the Ru/
CNT presoma is placed in air and calcines 2~4 hours for 150~250 DEG C.
Preferably, anode chamber's electrolyte is KOH solution.It is further preferred that anode chamber's electrolyte be 0.8~
The KOH solution of 1.2M.It is further preferred that anode chamber's electrolyte is the KOH solution of 1.0M.
Preferably, the cathode chamber electrolyte is H2SO4Solution.It is further preferred that anode chamber's electrolyte is 0.3
The H of~0.8M2SO4Solution.It is further preferred that anode chamber's electrolyte is the H of 0.5M2SO4Solution.
As an implementation, the anode electrode film and the cathode electrode sheet are by containing Ru-RuO2/ CNT is compound
The slurry of object catalyst is coated on glass-carbon electrode and obtains after drying.
Preferably, the anode electrode film and the cathode electrode on piece Ru-RuO2The load of/CNT complex catalyst
Amount is 1~2mg cm-2。
As a kind of specific embodiment, the preparation method of the electrolytic cell includes:
(1)Ru-RuO2The synthesis of/CNT complex catalyst: with RuCl3·xH2O is ruthenium source, and deionized water is solvent, is delayed
Slowly the CNT solution handled through peracid solutions is added dropwise, forms uniformly mixed solution；Prepare 0.3M NaHCO3Solution adjusts above-mentioned
PH value of solution stirs certain time to 7；Reducing agent NaBH is added in the above solution4Presoma Ru/CNT is made；By above-mentioned gained
Presoma Ru/CNT is placed in tube furnace low temperature calcination under air atmosphere, realizes Ru-RuO2The preparation of/CNT complex catalyst；
(2) assembling of Acid-Base heterozygosis electrolytic cell: with 0.5M H2SO4As catholyte, 1.0M KOH is as anode electricity
Xie Zhi separates cathode chamber and anode chamber using bipolar membrane, Acid-Base heterozygosis electrolytic cell is assembled, with Ru-RuO2/ CNT respectively as
The cathode and anode catalyst of Acid-Base heterozygosis electrolytic cell carry out electrolysis water performance test.
According to the another aspect of the application, application of any of the above-described electrolytic cell in water electrolysis hydrogen production and/or oxygen is provided.
Preferably, the driving current potential of the water electrolysis hydrogen production and/or oxygen is not less than 0.65V.
Preferably, the electrolytic cell realizes 10mA cm-2Current density current potential be no more than 0.75V.
The beneficial effect that the application can generate includes at least:
1) electrolytic cell provided herein, using Ru-RuO2/ CNT composite material is used as anode catalyst and yin simultaneously
Electrode catalyst；Ru-RuO2/ CNT composite material is a kind of inexpensive, high activity electrode catalyst, can be under various pH media
It effectively improves the production hydrogen of catalyst, produce oxygen activity.
2) electrolytic cell provided herein provides new solution to expand the selection of catalyst and electrolyte,
Importantly, the energy consumption of electrolysis water can be significantly reduced in the Acid-Base heterozygosis electrolytic cell, and reach under the current potential of 0.73V
10mA cm-2Current density, well below the theoretical potential 1.23V of electrolysis water in traditional electrolyte pond, application value is huge.
Detailed description of the invention
Fig. 1 is sample 1#X-ray diffractogram.
Fig. 2 is sample 1#Transmission electron microscope picture.
Fig. 3 is sample 1#H2-producing capacity figure under different medium.
Fig. 4 is sample 1#Production oxygen performance map under different medium.
Fig. 5 is the schematic diagram that the application electrolytic cell is electrolysed aquatic products hydrogen and oxygen.
Fig. 6 be electrolytic cell 1#With D1#Potential-current density comparison diagram.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein is bought by commercial sources, unprocessed directly to make
With；The test condition of instrument is all made of manufacturer's recommended parameter.
In embodiment, Bipolar Membrane is purchased from Beijing Tingrun Membrane Technology Development Co., Ltd..
In embodiment, the transmission electron microscope of sample is characterized using high resolution transmission electron microscopy (Tecnai F20).
In embodiment, the X-ray diffraction analysis (XRD) of sample is characterized using Miniflex 600.
In embodiment, chemical property measurement using the CHI760E type electrochemical workstation of Shanghai Chen Hua company to battery,
Glass-carbon electrode uses and CHI760E type electrochemical workstation CHI102 type glass-carbon electrode matching used to battery.
1 sample 1 of embodiment#~3#Preparation
Sample 1#Preparation
Firstly, carbon nanotube with mixed acid solution (concentrated nitric acid and mass fraction that mass fraction is 68% be 98% it is dense
Sulfuric acid, volume ratio are V (HNO3):V(H2SO4)=3:1) it after processing 8h, is washed with deionized, is freeze-dried standby at 90 DEG C
With.Then, 109mg RuCl is weighed3·3H2O is dissolved in 30ml deionized water, is stirred until homogeneous dispersion.Delay into above-mentioned solution
Slow be added dropwise is dissolved in the deionized water solution that 20ml is dispersed with 50mg CNT, obtains mixed solution.Then, 0.3M NaHCO is prepared3
Solution is slowly added dropwise to above-mentioned mixed solution as buffer solution and adjusts its pH=7, stirs 18h at room temperature.By above-mentioned solution
It is transferred in three-necked flask, N2After being warming up to 80 DEG C in oil bath pan under atmosphere, it is slowly added to NaBH4(5ml, 5wt% are water-soluble
Liquid), react 2h.It is cooled to room temperature after reaction, takes out solution, filtered, washing, be freeze-dried to get arriving with deionized water
Presoma Ru/CNT.Above-mentioned gained presoma Ru/CNT is placed in tube furnace, under air atmosphere, 200 DEG C of low temperature calcination 3h,
Obtain the Ru-RuO2/ CNT composite catalyst, is denoted as sample 1#。
Sample 2#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, RuCl3·3H2The quality of O is changed into
150mg, gained Ru-RuO2/ CNT composite catalyst, is denoted as sample 2#。
Sample 3#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, the condition of partial oxidation is 190 DEG C low
Temperature calcining 4h, is denoted as sample 3#。
2 sample 1 of embodiment#~3#Characterization
Respectively to sample 1#~3#Carry out X-ray diffraction analysis.With sample 1#For Typical Representative, XRD spectra and Ru and
RuO2Standard spectrogram comparison it is as shown in Figure 1.As seen from Figure 1, in sample existing metallic state Ru, also have oxidation state
RuO2。
Sample 2#With 3#XRD spectra and sample 1#It is similar, that is, peak position is identical, according to the difference of preparation condition, peak intensity
Spend the range changing ± 5%.
Respectively to sample 1#~3#Transmission electron microscope analysis is carried out.
Scanning electron microscope is as the result is shown: being distributed Ru and RuO on the carbon nanotubes2Uniform particle sizes, between 2~5nm.With
Sample 1#For Typical Representative, stereoscan photograph is as shown in Figure 2.
3 electrochemistry of embodiment produces hydrogen, produces oxygen test
By 5mg sample 1#It is scattered in the mixed solution of+50 μ l Nafion+420 μ l deionized water of 30 μ l ethyl alcohol, ultrasound
Slurries are made in dispersion, take 6 μ l to drop in glassy carbon electrode surface, respectively in 0.5M H2SO4, 1.0M PBS and 1.0M KOH electrolyte
Middle progress electrochemistry produces hydrogen, produces oxygen test.As a result as shown in Figure 4 and Figure 5.
4 electrolytic cell 1 of embodiment#And D1#Preparation
Respectively with sample 1#With the RuO of commercially available acquisition2As cathod catalyst and anode catalyst, electrolytic cell is prepared.
Electrolytic cell 1#Preparation
According to mode shown in Fig. 5, electrolytic cell is assembled.
Anode and cathode is identical: by 5mg sample 1#It is scattered in+50 μ l Nafion+420 μ l deionized water of 30 μ l ethyl alcohol
In mixed solution, ultrasonic half an hour takes 100uL slurry drop coating on glass-carbon electrode, electrode is made with liquid-transfering gun.Electrode is placed in
After toasting drying under infrared lamp, assembled for electrolytic cell.
Diaphragm: Bipolar Membrane is used.
Anode chamber and cathode chamber are separated anolyte and catholyte by Bipolar Membrane, prevent anode and cathode electrolyte
Neutralization reaction occurs.
Anode chamber's electrolyte: 1.0M KOH solution.
Cathode chamber electrolyte: 0.5M H2SO4Solution.
After being assembled into electrolytic cell, by 1.0M KOH solution and 0.5M H2SO4It is injected separately into anode chamber and cathode chamber, obtains
Electrolytic cell is denoted as electrolytic cell 1#。
Compare electrolytic cell D1#Preparation
Preparation step and raw material proportioning are the same as electrolytic cell 1#Preparation, the difference is that, with RuO2Instead of sample 1#, gained
Electrolytic cell is denoted as D1#。
5 electrolytic cell 1 of embodiment#And D1#Performance measurement
Respectively to electrolytic cell 1#And D1#Chemical property be measured, as a result as shown in Figure 6.As seen from the figure, it adopts
With the electrolytic cell 1 of technical scheme#It only needs 0.65V to realize the driving of electrolysis water, and reaches 10mA under the current potential of 0.73V
cm-2Current density greatly reduce energy consumption well below the theoretical potential 1.23V of electrolysis water in traditional electrolyte pond.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (10)
1. a kind of electrolytic cell, which is characterized in that including anode electrode film, cathode electrode sheet, bipolar membrane, anode chamber's electrolyte and
Cathode chamber electrolyte；
Wherein, the anode electrode film includes anode catalyst, and the cathode electrode sheet includes cathod catalyst；
The anode catalyst and the cathod catalyst are Ru-RuO2/ CNT complex catalyst；
The anolyte and the catholyte are separated by the bipolar membrane；
Anode chamber's electrolyte is alkaline solution, and the cathode chamber electrolyte is acid solution.
2. electrolytic cell according to claim 1, which is characterized in that the Ru-RuO2The preparation side of/CNT complex catalyst
Method at least includes the following steps:
A) after contacting the solution containing Ru ion with the carbon nanotube through peracid treatment, Ru/CNT presoma is obtained through reduction；
B) the resulting Ru/CNT presoma of step a) is subjected to partial oxidation, obtains the Ru-RuO2/ CNT complex catalyst.
3. electrolytic cell according to claim 2, which is characterized in that step a) be will the solution containing Ru ion with containing warp
The solution of the carbon nanotube of peracid treatment mixes, and after system pH is adjusted to 6.5~7.5, reducing agent is added and obtains Ru/CNT
Presoma.
4. electrolytic cell according to claim 3, which is characterized in that the reducing agent is NaBH4。
5. electrolytic cell according to claim 2, which is characterized in that step b) is that the Ru/CNT presoma is carried out part
Oxidation are as follows: the Ru/CNT presoma is placed in air and is calcined 2~4 hours for 150~250 DEG C.
6. electrolytic cell according to claim 1, which is characterized in that anode chamber's electrolyte is KOH solution；
Preferably, anode chamber's electrolyte is the KOH solution of 0.8~1.2mol/L；
It is further preferred that anode chamber's electrolyte is the KOH solution of 1.0mol/L.
7. electrolytic cell according to claim 1, which is characterized in that the cathode chamber electrolyte is H2SO4Solution；
Preferably, the cathode chamber electrolyte is 0.3~0.8mol/L H2SO4Solution；
It is further preferred that the cathode chamber electrolyte is the H of 0.5mol/L2SO4Solution.
8. electrolytic cell according to claim 1, which is characterized in that the anode electrode film and the cathode electrode sheet by
Containing Ru-RuO2The slurry of/CNT complex catalyst is coated on glass-carbon electrode and obtains after drying.
9. application of any one of claim 1 to 8 electrolytic cell in water electrolysis hydrogen production and/or oxygen.
10. application according to claim 9, which is characterized in that the driving current potential of the water electrolysis hydrogen production and/or oxygen is not
Less than 0.65V.
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| CN113774417A (en) * | 2021-09-14 | 2021-12-10 | 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 |
| CN115159574A (en) * | 2021-03-17 | 2022-10-11 | 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 |
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| CN115159574A (en) * | 2021-03-17 | 2022-10-11 | 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 |
| 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 |
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| 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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| CN110117797B (en) | 2020-10-02 |
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