CN106868538B - A kind of Carbon dioxide electrochemical reduction electrode, preparation method and applications - Google Patents
A kind of Carbon dioxide electrochemical reduction electrode, preparation method and applications Download PDFInfo
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- 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
Abstract
The invention discloses a kind of Carbon dioxide electrochemical reduction electrode and its preparations and application, and including the Sn catalyst nano layer adhered on basal layer and basal layer, the loading of Sn catalyst is 1mg/cm in electrode‑2‑6mg/cm‑2, the Sn in electrode is by one of the nano wire of 1nm-500nm, nanometer rods, nanofiber or two kinds of composition described above.The present invention significantly improves the specific surface area and active area of electrode by Sn nanometer rods of the growth in situ with abundant edge active position in substrate, improves the faradic efficiency that electrode is formic acid to the electrochemical reduction of carbon dioxide.
Description
Technical field
The present invention relates to Carbon dioxide electrochemical reduction electrodes, preparation method and applications, belong to CO_2 Resource
Change the field of utilizing.
Background technique
In recent years, with the rapid development of economy, environmental problem and energy shortage problem are on the rise.Wherein, global
It warms and also has become countries in the world problem urgently to be resolved, and CO2One of a large amount of discharge the main reason for being global warming.Cause
And how to efficiently use CO2And reduce CO2Discharge cause the extensive concern of people.
Currently, people reduce CO using a variety of methods2Discharge, including CO2Capture fixation and trans-utilization.CO2Turn
Change using including catalytic hydrogenation, catalytic reforming, electrochemistry or electronation conversion etc., to realize CO2Activation synthesizes methane, first
The organic compounds such as alcohol, formic acid or high-molecular compound.Comprehensively consider from energy consumption and cost, electrochemical reducing has can be
The advantages that normal temperature and pressure reacts, low energy consumption and transformation efficiency is higher, is CO2One of more feasible approach in transformation technology,
It is current hot research problem.ERC technology is to utilize electric energy by CO2Various small organic molecules or chemical products are reduced to, are had
Effect realizes greenhouse gases CO2A kind of technology of resource utilization.With the rapid development of renewable energy power generation technology, generate electricity skill
The cost of art is expected to sharp fall.Using renewable energy power generation, recycles electric energy by carbon dioxide synthesis of organic substance, realize
Conversion of the electric energy to chemical energy will so form the circulation and energy conversion cycles of a carbon.ERC technology can not only save stone
The fossil energies such as oil, natural gas and coal, and turn waste into wealth, make CO2It is utilized effectively, reduces CO2Caused by environment it is dirty
Dye.Therefore, ERC technology has potential economic benefit and environmental benefit.
Electrochemical reduction CO2(ERC) technology is to utilize electric energy by CO2Various small organic molecules or chemical products are reduced to, are had
Effect realizes greenhouse gases CO2A kind of technology of resource utilization.With the rapid development of renewable energy power generation technology, generate electricity skill
The cost of art is expected to sharp fall.Using renewable energy power generation, recycles electric energy by carbon dioxide synthesis of organic substance, realize
Conversion of the electric energy to chemical energy will so form the circulation and energy conversion cycles of a carbon.ERC technology can not only save stone
The fossil energies such as oil, natural gas and coal, and turn waste into wealth, make CO2It is utilized effectively, reduces CO2Caused by environment it is dirty
Dye.Therefore, ERC technology has potential economic benefit and environmental benefit.Someone is expected, the following CO2Chemical becomes one
New organic chemical industry's system, its development are of great significance to the energy and environmental problem for solving facing mankind.
CO2It is an important research direction in ERC technology that electrochemical reduction, which prepares organic acid such as formic acid, acetic acid,.System
Standby organic acid can be used for medicine, pesticide, organic synthesis etc., therefore have very high application value and economic value.Mesh
Before, the catalyst for being used to prepare organic acid mainly has In, Hg, Pb, Sn, Zn, Cu etc., electrochemical reduction CO2Activity sequence: In
>Hg>Pb>Sn>Zn≈Cu.In catalysis carbon dioxide reduction generate organic acid efficiency be it is relatively high, such as K Ito utilize
Metal In does cathode and restores CO in water-soluble medium2Formic acid processed, faradic efficiency reach as high as 80%, but since In, Bi belong to
In rare metal, global reserves are little, therefore its cost of material price is more expensive, limits its development prospect.The metals such as Pb, Hg
Belong to heavy metal, toxicity is bigger, limits its practical application.
Sn base catalyst is catalysis CO2Reduction generates one of the effective catalyst of organic acid.Since Sn metal largely exists
In the earth's crust, less expensive, for large-scale industrial application, it will substantially reduce cost.Finally, relative to other
For restoring CO2The catalyst (Pb, Cd, Hg etc.) of organic acid processed, Sn metal are also very little for the pollution of environment, are a kind of
Environmental-friendly metallic catalyst.Therefore Sn base catalyst is a kind of ERC catalyst with very big Research Prospects.But current Sn
The performance of catalyst is also relatively low.
Many people are by recycling PTFE as binder, being sprayed using catalyst such as chemical method synthesizing tin oxide, tin
It is coated onto diffusion layer surface, obtains electrode.However this preparation method is more complicated, and the lower (faradic efficiency of performance of electrode
Lower than 60%).In addition, above-mentioned electrode mainly by various methods by Sn catalyst preparation on tinfoil paper and glassy carbon electrode,
It in actual application, needs on the electrode to scrape off the catalyst of preparation, then by adhesive coated to carbon-based bottom surface,
It is cumbersome so as to cause electrode fabrication process, and cladding of the catalyst due to binder is prepared, active specific surface decline, so as to cause
Activity reduces.
Summary of the invention
The present invention is in order to solve the above technical problems, by electrochemical method, and in-situ deposition Sn nanometer rods are catalyzed in substrate
Agent, the porous gas diffusive electrode that Sn catalyst is prepared establish stable gas liquid solid three phase boundary, shorten gas diffusion
Electrode reaction rate is improved in path, not only can simplify the preparation process of catalyst, and can effectively control the advantage of catalyst
Crystal face and pattern, to regulate and control the performance of electrode.
To achieve the above object, the specific technical solution that the present invention uses is as follows:
A kind of Carbon dioxide electrochemical reduction electrode, including the Sn catalyst nano adhered on basal layer and basal layer
Layer, the loading of Sn catalyst is 1mg/cm-2-6mg/cm in electrode-2, Sn in electrode by 1nm-500nm nano wire, receive
One of rice stick, nanofiber or two kinds of composition described above.
A kind of Carbon dioxide electrochemical reduction electrode preparation method,
1) charcoal felt, carbon paper or carbon slab are subjected to processing 6-24 hours at 200~600 DEG C in air, then in ethyl alcohol or
Substrate is used as after carrying out oil removal treatment cleaning in acetone；
It 2) is 0.01M-0.5M SnSO by concentration4Solution, with 0.05M-3M H2SO4With the additive of 0.01M~1.0M,
It is 50:1~1:30 and SnSO with Sn and additive molar ratio4With H2SO4Molar ratio be 1:1~1:50 mixed
Polymer solution is as electrolyte solution；
3) in electrolyte solution, constant current density or constant potential are carried out under inert atmosphere protection in depositing in substrate
Sn 10s~5000s；
4) substrate with Sn layers of deposition restores 30s- in -0.8V~-1.1V in 0.05-0.8M post-processing electrolyte
900s；
5) it washs, the electrode with Sn Nanorods Catalyst is prepared after drying.
SnSO in the step 2) electrolyte solution4With H2SO4Preferred molar ratio example be 1:1-1:10；Additive and Sn
The preferred molar ratio example of salt is 20:1-1:10.
Step 3) the constant current is -5mA/cm2~-200mA/cm2, preferably -20mA/cm2~-100mA/cm2；It is permanent
Current potential is -0.2V~-4V, preferably -0.3V~-1.5V；
The additive is octyl phenyl polyoxyethylene ether (trixton-100), polysorbas20 (TWEEN-20), tween 21
(TWEEN-21), polysorbate40 (TWEEN-40), polysorbate60 (TWEEN-60), Tween61 (TWEEN-61), Tween 80 (TWEEN-
80), sorbimacrogol oleate100 (TWEEN-81), polysorbate85 (TWEEN-85)；Sapn；Gelatin；Polyethylene glycol, gathers polyalkylene glycol alkyl alcohol ether
One of ethylene glycol propylene glycol block copolymer, OP (alkyl phenol polyoxyethylene ether) or two kinds or more.
Step 3) the sedimentation time is preferably 30s-2500s..
HCl, H that step 4) the post-processing electrolyte is 0.05M-0.5M3PO4Or NaHCO3、NaOH、NaCl、KCl、
KHCO3, one of KOH.
The inert atmosphere is that one of nitrogen, argon gas or helium atmosphere or two kinds or more mix.
The electrode can be used as the cathode of Carbon dioxide electrochemical reduction reaction.
Using
By made electrode, as carbon dioxide reduction formic acid cathode.And electrochemistry is carried out by three-electrode system
Test: working electrode is electrode obtained；It is Pt piece, reference electrode Hg/Hg to electrode2Cl2/ saturation KCl.Between WE and RE
Distance be 0.5cm, use salt bridge to reduce liquid potential.Catholyte is 0.5M NaHCO3Aq.sol., electrolyte
Product is 180ml.Anolyte is 0.1M H2SO4aq.sol.
Compared with prior art, the beneficial effects of the present invention are:
A kind of electrode structure without binder is provided, this kind of electrode does not need additionally to add binder, and can be complete
All risk insurance holds the pattern of surface catalyst, avoids because of activity bit-loss caused by addition binder；
It is prepared in substrate compared to re-coating after the above-mentioned Sn catalyst on tinfoil paper and glassy carbon electrode and directly synthesized
The method of electrode, the gas-diffusion electrode being prepared in situ using the present invention are had excellent faradic efficiency and to carboxylic acid products
Selectivity.The effective active area of electrode not only can be improved in prepared gas-diffusion electrode, can also improve reactant
Transmission improves its performance, is more advantageous to the practical application of ERC to reduce mass transfer polarization.Furthermore method provided by the present invention
Simply, easily-controllable, it is conducive to large-scale production.
Provide a kind of new CO2The preparation method of electrochemical reduction electrode, i.e., with one kind with octyl phenyl polyoxy second
Alkene ether (trixton-100), polysorbas20 (TWEEN-20), tween 21 (TWEEN-21), polysorbate40 (TWEEN-40), polysorbate60
(TWEEN-60), Tween61 (TWEEN-61), Tween 80 (TWEEN-80), sorbimacrogol oleate100 (TWEEN-81), polysorbate85 (TWEEN-
85)；Sapn；Gelatin；(alkyl phenol is poly- by polyethylene glycol, polyalkylene glycol alkyl alcohol ether, polyethylene glycol propylene glycol block copolymer, OP
Ethylene oxide ether) it is additive, ordered structure electrode is prepared by electrochemical deposition, i.e., growth in situ has excellent in substrate
The Sn nanometer rods of gesture crystal face significantly improve the specific surface area and effective active area of electrode, improve catalyst to titanium dioxide
The electrochemical reduction activity of carbon, and to the selectivity of organic acid；
The effective active area of electrode not only can be improved with prepared gas-diffusion electrode for this method, can also improve
The transmission of reactant improves its performance, is more advantageous to the practical application of ERC to reduce mass transfer polarization；Preparation method of the present invention
Simply, it easily grasps, conventional production device, is suitble to large-scale production, the electrode specific surface area of preparation is big, has very high carbon dioxide
Hydrogen reduction catalytic performance.
Detailed description of the invention
Fig. 1 embodiment 1,2,3 and comparative example 1 prepare the XRD spectra of electrode
The SEM photograph of electrode prepared by Fig. 2 embodiment 2；
The SEM photograph of electrode prepared by Fig. 3 embodiment 4；
The SEM photograph of electrode prepared by Fig. 4 comparative example 1；
Fig. 5 embodiment 1 and comparative example 1 prepare the faradic efficiency of electrode.
Specific embodiment
Below by embodiment, the present invention is described in detail, but the present invention is not limited only to embodiment.
Embodiment 1
Carbon paper is handled in air at 550 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.25M SnSO by concentration4Solution, with 0.7M H2SO4With the Trix100 of 0.06M, it is uniformly mixed that obtain mixture molten
Liquid is as electrolyte solution；In electrolyte solution, in N2Constant current density -60mA cm is carried out under atmosphere protection-2Constant potential is heavy
Product 2000s；The 0.5M NaHCO in post-processing electrolyte3900s is restored with -1.2V in electrolyte solution；It is made after washing, drying
It is standby to obtain Sn Nanorods Catalyst.Show from Fig. 5 relative to comparative example 1, electrode performance significantly improves in embodiment 1.
Embodiment 2
Carbon paper is handled in air at 550 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.25M SnSO by concentration4Solution, with 0.8M H2SO4With the OP of 0.06 2M, it is uniformly mixed and obtains mixture solution
As electrolyte solution；In electrolyte solution, in N2Constant current density -60mA cm is carried out under atmosphere protection-2Potentiostatic electrodeposition
2000s；The 0.5M NaHCO in post-processing electrolyte3900s is restored with -1.2V in electrolyte solution；It is prepared after washing, drying
Obtain Sn Nanorods Catalyst.
Embodiment 3
Carbon paper is handled in air at 550 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.25M SnSO by concentration4Solution, with 0.8M H2SO4With the gelatin of 0.06M, it is uniformly mixed and obtains mixture solution
As electrolyte solution；In electrolyte solution, in N2Constant current density -60mA cm is carried out under atmosphere protection-2Potentiostatic electrodeposition
2000s；The 0.5M NaHCO in post-processing electrolyte3900s is restored with -1.2V in electrolyte solution；It is prepared after washing, drying
Obtain Sn Nanorods Catalyst.
Embodiment 4
Carbon paper is handled in air at 550 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.25M SnSO by concentration4Solution, with 0.8M H2SO4With the Tween-80 of 0.06M, it is uniformly mixed and obtains mixture
Solution is as electrolyte solution；In electrolyte solution, in N2Constant current density -60mA cm is carried out under atmosphere protection-2Constant potential
Deposit 2000s；The 0.5M NaHCO in post-processing electrolyte3900s is restored with -0.9V in electrolyte solution；After washing, drying
Sn Nanorods Catalyst is prepared.From figure 3, it can be seen that the electrode surface catalyst being prepared is received in polygon flechette-type
Rice stick structure.
Embodiment 5
Carbon paper is handled in air at 550 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.25M SnSO by concentration4Solution, with 1.0M H2SO4With the gelatin -80 of 0.03M, it is uniformly mixed that obtain mixture molten
Liquid is as electrolyte solution；In electrolyte solution, constant current density -20mA cm is carried out under Ar atmosphere protection-2Constant potential is heavy
Product 2000s；The 0.5M NaHCO in post-processing electrolyte3900s is restored with -0.9V in electrolyte solution；It is made after washing, drying
It is standby to obtain Sn Nanorods Catalyst.
Embodiment 6
Carbon paper is handled in air at 450 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.5M SnSO by concentration4Solution, with 1.5M H2SO4With the OP of 0.02M, it is uniformly mixed and obtains mixture solution conduct
Electrolyte solution；In electrolyte solution, in N2Constant current density -150mA cm is carried out under atmosphere protection-2Potentiostatic electrodeposition
200s；The 0.8M KHCO in post-processing electrolyte3100s is restored with -1.0V in electrolyte solution；It is prepared into after washing, drying
To Sn Nanorods Catalyst.
Embodiment 7
Carbon paper is handled in air at 300 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.4M SnSO by concentration4Solution, with 1.0M H2SO4With the TW-20 of 0.10M, it is uniformly mixed and obtains mixture solution
As electrolyte solution；In electrolyte solution, constant potential -0.5V Vs.SCE is carried out under He atmosphere protection and deposits 4000s；
500s is restored with -0.7V in 0.1M NaOH electrolyte solution in post-processing electrolyte；Sn is prepared after washing, drying to receive
Rice stick catalyst.
Embodiment 8
Carbon paper is handled in air at 300 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.25M SnSO by concentration4Solution, with 0.7M H2SO4With the sapn of 0.15M, it is uniformly mixed and obtains mixture solution
As electrolyte solution；In electrolyte solution, constant potential -1.25V Vs.SCE is carried out under He atmosphere protection and deposits 500s；
700s is restored with -0.8V in 0.1M HCl electrolyte solution in post-processing electrolyte；Sn nanometers are prepared after washing, drying
Stick catalyst.
Comparative example 1
Carbon paper is handled in air at 550 DEG C, conduct after oil removal treatment cleaning is then carried out in ethyl alcohol, acetone
Substrate；It is 0.25M SnSO by concentration4Solution, with 0.8M H2SO4, it is uniformly mixed that obtain mixture solution molten as electrolyte
Liquid；In electrolyte solution, in N2Constant current density -60mA cm is carried out under atmosphere protection-2Potentiostatic electrodeposition 2000s；In Hou Chu
Manage 0.5M NaHCO in electrolyte3900s is restored with -0.9V in electrolyte solution；Sn nanometer rods are prepared after washing, drying
Catalyst.
From figure 1 it appears that different additives, which is added, obtains the catalyst of different advantage crystal faces.It is prepared by embodiment 1
Catalyst (220) and (211) face are advantage crystal face；And Sn-OP in embodiment 2.
As can be seen that the electrode surface catalyst being prepared is in gyroscope-like nanorod structure in Fig. 2.
Claims (8)
1. a kind of Carbon dioxide electrochemical reduction electrode, it is characterised in that: the Sn including adhering on basal layer and basal layer is urged
Agent nanometer layer, the loading of Sn catalyst is in electrode
1 mg/cm2-6 mg/cm2, Sn in electrode by one of the nano wire of 1nm-500nm, nanometer rods, nanofiber or
Two kinds of composition described above；
A kind of Carbon dioxide electrochemical reduction electrode the preparation method comprises the following steps:
1) by charcoal felt, carbon paper or carbon slab 200~600oC carries out processing 6-24 hours in air, then in ethyl alcohol or acetone
Substrate is used as after carrying out oil removal treatment cleaning；
It 2) is 0.01 M-0.5 M SnSO by concentration4Solution, with 0.05 M-3 M H2SO4With the addition of the M of 0.01 M~1.0
Agent is 50:1~1:30 and SnSO with Sn and additive molar ratio4With H2SO4Molar ratio be 1:1~1:50 be uniformly mixed obtain
Mixture solution is as electrolyte solution；
3) in electrolyte solution, constant current density or constant potential are carried out under inert atmosphere protection in depositing Sn in substrate
10s~5000s；
4) substrate with Sn layers of deposition restores 30 s-900 in -0.8 V of V~-1.2 in 0.05-0.8 M post-processing electrolyte
s ；
5) it washs, the electrode with Sn Nanorods Catalyst is prepared after drying；
The additive is octyl phenyl polyoxyethylene ether (trixton-100), polysorbas20 (TWEEN-20), tween 21
(TWEEN-21), polysorbate40 (TWEEN-40), polysorbate60 (TWEEN-60), Tween61 (TWEEN-61), Tween 80 (TWEEN-
80), sorbimacrogol oleate100 (TWEEN-81), polysorbate85 (TWEEN-85), sapn, gelatin, polyethylene glycol, polyalkylene glycol alkyl alcohol ether, poly-
One of ethylene glycol propylene glycol block copolymer, alkyl phenol polyoxyethylene ether or two kinds or more.
2. electrode described in accordance with the claim 1, it is characterised in that: SnSO in electrolyte solution described in step 24With H2SO4's
Molar ratio is 1:1-1:10；The molar ratio of additive and Sn salt is 20:1-1:10.
3. electrode described in accordance with the claim 1, it is characterised in that: constant current described in step 3) is -5 mA/cm2~-200
mA/cm2；Constant potential is -0.2 V of V~-4.
4. electrode described in accordance with the claim 1, it is characterised in that: constant current described in step 3) is -20 mA/cm2~-100
mA/cm2；Constant potential is -0.3 V of V~-1.5.
5. electrode described in accordance with the claim 1, it is characterised in that: sedimentation time described in step 3) is 30s-2500s..
6. electrode described in accordance with the claim 1, it is characterised in that: post-processing electrolyte described in step 4) is 0.05 M-0.5
HCl, H of M3PO4Or NaHCO3、NaOH、NaCl、KCl、KHCO3, one of KOH.
7. electrode described in accordance with the claim 1, it is characterised in that: the inert atmosphere is in nitrogen, argon gas or helium atmosphere
One or two or more kinds of mixing.
8. a kind of application of electrode described in claim 1, it is characterised in that: the electrode can be used as Carbon dioxide electrochemical reduction
The cathode of reaction.
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| JP6779849B2 (en) * | 2017-09-19 | 2020-11-04 | 株式会社東芝 | Carbon dioxide reduction catalyst and its production method, reduction electrode, and reduction reactor |
| CN109852990B (en) * | 2017-11-30 | 2020-10-30 | 中国科学院大连化学物理研究所 | CO (carbon monoxide)2Electrode for electrochemical reduction, preparation and application thereof |
| CN109972162A (en) * | 2019-05-13 | 2019-07-05 | 中国人民解放军军事科学院防化研究院 | A kind of electro-chemistry oxygen-producing method |
| CN111519207B (en) * | 2020-05-19 | 2021-06-29 | 大连大学 | Preparation and application of Sn electrode for electrochemical reduction of carbon dioxide |
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| Electrodeposition of Tin Needle-Like Structures;C. Lizzul Rinne等;《Journal of The Electrochemical Society》;20020129;第149卷(第3期);C150-C158 * |
| Template-Free Electrochemical Synthesis of Sn Nanofibers as High-Performance Anode Materials for Na-Ion Batteries;Do-Hwan Nam等;《ACS Nano》;20141028;第8卷(第11期);11824-11835 * |
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