CN116024601A - Carbon nano tube-based porous hollow fiber electrode for electrocatalytic reduction reaction and application - Google Patents
Carbon nano tube-based porous hollow fiber electrode for electrocatalytic reduction reaction and application Download PDFInfo
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- CN116024601A CN116024601A CN202211696352.6A CN202211696352A CN116024601A CN 116024601 A CN116024601 A CN 116024601A CN 202211696352 A CN202211696352 A CN 202211696352A CN 116024601 A CN116024601 A CN 116024601A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 51
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 51
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 47
- 238000006722 reduction reaction Methods 0.000 title claims abstract description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- UBAZGMLMVVQSCD-UHFFFAOYSA-N carbon dioxide;molecular oxygen Chemical compound O=O.O=C=O UBAZGMLMVVQSCD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 239000002101 nanobubble Substances 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 239000002109 single walled nanotube Substances 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 3
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 21
- 238000009792 diffusion process Methods 0.000 description 15
- 239000010949 copper Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229920005596 polymer binder Polymers 0.000 description 2
- 239000002491 polymer binding agent Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000010757 Reduction Activity Effects 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite alkyne Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- Y02E60/50—Fuel cells
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Abstract
The invention belongs to the field of electrochemistry, and discloses a carbon nano tube-based porous hollow fiber electrode for electrocatalytic reduction reaction and application thereof, wherein the electrode is provided with a self-supporting porous hollow fiber tubular structure, the outer diameter of the tube is 500-1500 mu m, the wall of the tube is of a staggered mesh structure, the wall thickness is 50-600 mu m, and the porosity is 50-95%. The carbon nano tube-based porous hollow fiber electrode has the advantages of high reaction activity, high efficiency, good stability and the like in the electro-reduction of oxygen, carbon dioxide, nitrogen and the like, is an electro-reduction electrode with excellent performance and low price, and is easy to realize large-scale application.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and relates to a carbon nano tube-based porous hollow fiber electrode for electrocatalytic reduction reaction and application thereof.
Background
The technology utilizes clean and efficient electrons as reactants to convert gas micromolecules into high-value chemicals at normal temperature and normal pressure, realizes recycling and energy utilization, pollution reduction and carbon reduction, has the characteristics of simplicity in operation, mild condition, environment friendliness and the like, and can solve the bottleneck of harsh conditions, high energy consumption and large carbon emission generation of industrial synthetic ammonia or urea. The prior electro-reduction reaction has low catalytic activity, low efficiency and poor stability, which are main factors limiting the application of the electro-reduction reaction, and the key to solve the problem is to develop a high-efficiency electro-catalytic reduction material.
The electric reduction oxygen, carbon dioxide, nitrogen and the like are gas-solid-liquid three-phase interface reactions, and the traditional electrode adopts a solution gas explosion mode to cause limited mass transfer and low gas concentration at a reaction interface, so that the reaction rate and efficiency are limited. The gas diffusion electrode can overcome the problem of limited mass transfer, the current gas diffusion electrode is mainly formed by coating a mixed solution of a powder catalyst and a polymer binder on a commercial gas diffusion electrode substrate to form a planar electrode, such as a planar gas diffusion electrode based on graphene, carbon nano tubes, metal oxides, porous carbon, noble metals (Pt, au, ag and the like) and the like, and patent CN114790555A discloses a selenium-doped porous carbon-based nitrogen reduction electrocatalyst which improves electrochemical reduction activity by loading non-noble metals on a support material with high specific surface area; despite certain advances, the following disadvantages exist: the use of a polymer binder can prevent the exposure of the active sites of the catalyst, the catalyst is easy to fall off and water flooded after long-term operation, and the reaction activity is reduced. Therefore, it is very important to develop an electrocatalytic reduction electrode with high efficiency and stability and rich components on earth.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and provides a high-efficiency and stable carbon nano tube-based porous hollow fiber electrode with a self-supporting structure, which is used for the fields of electrocatalytic reduction of oxygen, carbon dioxide, nitrogen and the like by improving the self-structure of a catalyst.
The electric reduction of oxygen, carbon dioxide and nitrogen plays an important role in pollution control, energy conversion, chemical synthesis and other pollution reduction and carbon reduction fields, and the lack of catalytic materials with excellent performance is a main factor limiting the application of the catalytic materials. The carbon nanotube-based porous hollow fiber electrode is a self-supporting gas diffusion electrode which is used for the explosion of hollow fibers from inside to outside and does not use a binder, and the bottleneck that the planar gas diffusion electrode has few effective catalytic active sites and is unstable can be solved. Meanwhile, the carbon nanotube-based porous hollow fiber electrode prepared by the invention has the advantages of high specific surface area, good conductivity and capability of improving the gas concentration at the three-phase interface by micro-nano bubbles formed by inner cavity explosion gas, and is beneficial to further improving the electrocatalytic reduction performance.
The technical scheme of the invention is as follows:
the porous hollow fiber electrode has self-supporting porous hollow fiber tubular structure with outer diameter of 500-1500 microns, wall of staggered mesh structure, wall thickness of 50-600 microns, porosity of 50-95%, and ventilation of inner cavity to form micro-nano bubbles of 10-20 microns.
The carbon nano tube-based porous hollow fiber electrode mainly comprises a single-wall carbon nano tube, a multi-wall carbon nano tube, an oxidation modified carbon nano tube, one or more elements of nitrogen, phosphorus, sulfur and fluorine doped carbon nano tubes, and one or more catalysts of metal, metal oxide, rare earth elements, graphene, carbon quantum dots, graphite alkyne, porous carbon, mxene and MOF are loaded on the carbon nano tube-based porous hollow fiber electrode.
The carbon nano tube-based porous hollow fiber electrode is applied as a working electrode, constant potential or current is applied, and the electrode is applied to electrocatalytic reduction reaction of electrocatalytic reduction of oxygen, carbon dioxide and nitrogen.
The working electrode is one or more carbon nanotube-based porous hollow fiber electrodes connected in parallel.
The invention has the beneficial effects that:
1. the carbon nano tube-based porous hollow fiber electrode is a self-supporting structure and has the advantages of high reaction activity and efficiency, good stability and the like.
2. The micro-nano pore canal of the porous hollow fiber electrode has a nano finite field effect, and can improve the selectivity and the reaction efficiency of a target product.
3. The porous hollow fiber electrode explodes gas outwards from the inner cavity, reduces the thickness of the diffusion layer, accelerates mass transfer, forms micro-nano bubbles, increases the concentration and the residence time of a gas reactant at a reaction interface, and improves the electrocatalytic reduction performance.
4. The main component of the carbon nano tube-based porous hollow fiber electrode is carbon elements with rich contents in the crust, and the material is very stable, can be repeatedly used for a plurality of times, and is easy to realize large-scale application.
Drawings
FIG. 1 (a) is a schematic representation of a carbon nanotube-based porous hollow fiber electrode of the present invention;
fig. 1 (b) is a schematic structural view of the carbon nanotube-based porous hollow fiber electrode of the present invention.
FIG. 2 is a scanning electron microscope image of the surface of a carbon nanotube-based porous hollow fiber electrode of the present invention.
Fig. 3 is a hydrogen peroxide yield comparison of a carbon nanotube porous hollow fiber electrode of the present invention and a carbon nanotube planar gas diffusion electrode.
FIG. 4 shows the CO of the Cu/carbon nanotube porous hollow fiber electrode and Cu/carbon nanotube planar gas diffusion electrode of the present invention 2 Saturated 0.1M KHCO 3 Ethanol production in (a).
Detailed Description
The electrocatalytic reduction performance of the carbon nanotube-based porous hollow fiber electrode prepared by the above method is further described below with reference to examples
Example 1 carbon nanotube porous hollow fiber electrode electro-reduction oxygen Performance
Adopting a carbon nano tube porous hollow fiber electrode as a working electrode, pt as a counter electrode and a saturated calomel electrode as a reference electrode, and adding the carbon nano tube porous hollow fiber electrode in O 2 Measurement of the electro-reduced oxygen Synthesis H in saturated 0.1M KOH 2 O 2 Is a product of the above process. The parameters of the carbon nano tube porous hollow fiber electrode are as follows: the outer diameter of the tube is 956 mu m, the wall thickness is 158 mu m, the effective length is 2.5cm, and the effective area is 0.75cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The parameters of the carbon nano tube planar gas diffusion electrode are as follows: the carbon nano tube is smeared on carbon paper, and the effective area is 1cm 2 The loading was 2.5mg/cm 2 The operating conditions were identical to those of the examples. As can be seen from FIG. 3, the carbon nanotube porous hollow fiber electrode was H at-0.6V 2 O 2 Yield of about 9 mmol/cm -2 ·h -1 The hydrogen peroxide yield is far higher than that of the carbon nano tube planar gas diffusion electrode, and the H is produced by the porous hollow fiber electrode 2 O 2 The Faraday efficiency of the electrode can reach more than 80 percent and is far higher than that of a planar gas diffusion electrode, which shows that the special structure of the carbon nano tube porous hollow fiber electrode can improve the H production of electrocatalytic reduction oxygen 2 O 2 Is a performance of the (c).
EXAMPLE 2 Cu/carbon nanotube porous hollow fiber electrode electro-reduction carbon dioxide Performance
Adopting a Cu/carbon nano tube porous hollow fiber electrode as a working electrode, pt as a counter electrode and a saturated calomel electrode as a reference electrode, and carrying out CO reaction on the electrode 2 Saturated 0.1M KHCO 3 And measuring the ethanol yield of the Cu/carbon nano tube porous hollow fiber electrode and the Cu/carbon nano tube planar gas diffusion electrode under different potentials. The preparation parameters of the Cu/carbon nano tube porous hollow fiber electrode are as follows: the outer diameter of the tube is 956 mu m, the wall thickness is 158 mu m, the effective length is 2.5cm, and the effective area is 0.75cm 2 Mixing with 2mg of copper phthalocyanine, N 2 Calcining at 900 ℃ for 3 hours; the parameters of the Cu/carbon nano tube planar gas diffusion electrode are as follows: 10mg of carbon nanotubes were mixed with 2mg of copper phthalocyanine, N 2 Calcining at 900deg.C for 3 hr, and applying on carbon paper with effective area of 1cm 2 The loading was 2.5mg/cm 2 The operating conditions were identical to those of the examples. As can be seen from fig. 4The yield of ethanol at-1V of the Cu/carbon nano tube porous hollow fiber electrode is 5mg (ml. H) -1 The electrode is 5 times of a Cu/carbon nano tube planar gas diffusion electrode, which shows that the special structure of the Cu/carbon nano tube porous hollow fiber electrode can improve the selectivity of multiple carbons and the ethanol production performance of electrocatalytic reduction of carbon dioxide.
Claims (4)
1. The carbon nanotube-based porous hollow fiber electrode for electrocatalytic reduction reaction is characterized in that the carbon nanotube-based porous hollow fiber electrode has a self-supporting porous hollow fiber tubular structure, the outer diameter of the tube is 500-1500 mu m, the wall of the tube is of a staggered mesh structure, the wall thickness is 50-600 mu m, the porosity is 50-95%, and the inner cavity is ventilated, so that micro-nano bubbles with the size of 10 nm-20 mu m can be formed.
2. The carbon nanotube-based porous hollow fiber electrode according to claim 1, wherein the carbon nanotube-based porous hollow fiber electrode is mainly composed of one or more of single-walled carbon nanotubes, multi-walled carbon nanotubes, oxidation-modified carbon nanotubes, one or more of nitrogen, phosphorus, sulfur, fluorine doped carbon nanotubes, and one or more of metal, metal oxide, rare earth element, graphene, carbon quantum dots, graphene, porous carbon, mxene, MOF supported on the carbon nanotube-based porous hollow fiber electrode.
3. The use of the carbon nanotube-based porous hollow fiber electrode of claim 1 or 2 as a working electrode, applying a constant potential or current, and applying it to electrocatalytic reduction reactions of electrocatalytic reduction of oxygen, carbon dioxide and nitrogen.
4. The use according to claim 3, wherein the working electrode is a carbon nanotube-based porous hollow fiber electrode connected in parallel with one or more electrodes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211696352.6A CN116024601A (en) | 2022-12-28 | 2022-12-28 | Carbon nano tube-based porous hollow fiber electrode for electrocatalytic reduction reaction and application |
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| CN202211696352.6A CN116024601A (en) | 2022-12-28 | 2022-12-28 | Carbon nano tube-based porous hollow fiber electrode for electrocatalytic reduction reaction and application |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254916A (en) * | 2008-04-11 | 2008-09-03 | 北京工业大学 | Method for in-situ synthesis of metal phthalocyanine/carbon nano-tube compound |
| CN105457500A (en) * | 2015-12-28 | 2016-04-06 | 中国科学院城市环境研究所 | Carbon nano tube/porous ceramic hollow fiber composite ultrafiltration membrane as well as preparation method and application thereof |
| CN110124531A (en) * | 2019-05-21 | 2019-08-16 | 大连理工大学 | A kind of porous carbon-Carbon-nanotube hollow fiber membrane preparation method can produce hydroxyl radical free radical under electrochemically strengthening effect |
| CN111644168A (en) * | 2020-04-20 | 2020-09-11 | 北京邮电大学 | Method for preparing atomic-scale catalyst by slowly raising temperature to greatly improve yield of hydrogen peroxide |
| CN113862699A (en) * | 2021-10-21 | 2021-12-31 | 大连理工大学 | Method for rapidly preparing phthalocyanine molecule and derivative thereof/carbon composite catalyst by microwave and application thereof |
-
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- 2022-12-28 CN CN202211696352.6A patent/CN116024601A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254916A (en) * | 2008-04-11 | 2008-09-03 | 北京工业大学 | Method for in-situ synthesis of metal phthalocyanine/carbon nano-tube compound |
| CN105457500A (en) * | 2015-12-28 | 2016-04-06 | 中国科学院城市环境研究所 | Carbon nano tube/porous ceramic hollow fiber composite ultrafiltration membrane as well as preparation method and application thereof |
| CN110124531A (en) * | 2019-05-21 | 2019-08-16 | 大连理工大学 | A kind of porous carbon-Carbon-nanotube hollow fiber membrane preparation method can produce hydroxyl radical free radical under electrochemically strengthening effect |
| CN111644168A (en) * | 2020-04-20 | 2020-09-11 | 北京邮电大学 | Method for preparing atomic-scale catalyst by slowly raising temperature to greatly improve yield of hydrogen peroxide |
| CN113862699A (en) * | 2021-10-21 | 2021-12-31 | 大连理工大学 | Method for rapidly preparing phthalocyanine molecule and derivative thereof/carbon composite catalyst by microwave and application thereof |
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