CN113036166B - Porous CoNi-coated carbon microtubule H2O2 electro-oxidation electrode prepared from endive flower template - Google Patents
Porous CoNi-coated carbon microtubule H2O2 electro-oxidation electrode prepared from endive flower template Download PDFInfo
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- CN113036166B CN113036166B CN202110239522.7A CN202110239522A CN113036166B CN 113036166 B CN113036166 B CN 113036166B CN 202110239522 A CN202110239522 A CN 202110239522A CN 113036166 B CN113036166 B CN 113036166B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 22
- 229910002441 CoNi Inorganic materials 0.000 title claims abstract description 20
- 238000006056 electrooxidation reaction Methods 0.000 title claims abstract description 18
- 235000003733 chicria Nutrition 0.000 title claims abstract description 11
- 102000029749 Microtubule Human genes 0.000 title claims abstract description 5
- 108091022875 Microtubule Proteins 0.000 title claims abstract description 5
- 210000004688 microtubule Anatomy 0.000 title claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title abstract description 54
- 244000116025 chicria Species 0.000 title 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 240000006740 Cichorium endivia Species 0.000 claims abstract description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 229910001868 water Inorganic materials 0.000 claims abstract description 6
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 241000488874 Sonchus Species 0.000 claims abstract 4
- 235000008132 Sonchus arvensis ssp. uliginosus Nutrition 0.000 claims abstract 4
- 238000003756 stirring Methods 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000000643 oven drying Methods 0.000 abstract description 3
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000446 fuel Substances 0.000 description 12
- 210000004027 cell Anatomy 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 244000113428 Sonchus oleraceus Species 0.000 description 5
- 235000006745 Sonchus oleraceus Nutrition 0.000 description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910005949 NiCo2O4 Inorganic materials 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
- H01M4/8885—Sintering or firing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
-
- 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
Abstract
The invention provides a porous CoNi coated carbon micro-tube H2O2 electro-oxidation electrode prepared by a endive flower template, wherein endive flowers are washed with acetone and deionized water for several times, impurities are removed, and the endive flowers are dried for later use; soaking herba Sonchi Oleracei flower in NaClO2 water solution at 80 deg.C, decocting for 10 hr, filtering, and oven drying; weighing Co (NO3) 2.6H 2O and Ni (NO3) 2.6H 2O, and dissolving in deionized water; soaking the treated sowthistle flowers in the solution, stirring for 6 hours at room temperature, and then putting the sowthistle flowers in an oven until all the solvent is evaporated to obtain a CoNi microtubule precursor; and putting the impregnated and dried precursor into a crucible, and calcining in an argon atmosphere to finally obtain the porous CoNi coated carbon microtube H2O2 electro-oxidation electrode. The method overcomes the defects of low electrooxidation rate and large concentration polarization of H2O2, and solves the problems of low utilization rate of H2O2 and the like caused by the escape of O2 generated by self-decomposition reaction from the surface of an electrode.
Description
Technical Field
The invention relates to an electrooxidation electrode, in particular to a porous CoNi coated carbon microtubule H2O2 electrooxidation electrode prepared by a endive flower template.
Background
H2O2 not only can be used as the oxidant of the battery, but also can be used as the fuel of the battery by the electrochemical oxidation reaction and the oxygen generated by oxidation. The hydrogen peroxide (H2O2) is used as a liquid fuel and an oxidant, and the problems of raw materials required by the fuel cell in the storage and transportation process are solved to a great extent. Therefore, the direct hydrogen peroxide fuel cell has great development prospect as a novel fuel cell. Compared with other types of direct liquid fuel cells such as a direct sodium borohydride fuel cell, the DPPFC has the following advantages: since both the oxidant and the fuel are H2O2, there is no "breakthrough" phenomenon, i.e. no longer affected by fuel permeation. Secondly, the H2O2 is non-toxic and harmless, and has no carbon element, the reaction product only contains water and oxygen, and products such as CO which can cause catalyst poisoning can not be generated, so that the stability of the catalyst is improved, and the service life of the battery is prolonged. ③ the electrochemical oxidation and reduction reaction process of H2O2 are both 2 e-reaction, and the electric reduction and electric oxidation activities are respectively higher than O2(4e-) and methanol (6 e-).
During the electro-oxidation of H2O2, H2O2 is prone to self-decomposition to form O2, and if the generated O2 escapes from the electrode surface, the utilization rate of H2O2 is reduced. See, in particular, Chenweiwei, Zhang Fei, Du Jia Liang, et al, preparation of NiCo2O4 electrode supported on foamed nickel and its performance of catalyzing the electrical oxidation of H2O2 [ J ]. electrochemistry 2020,26(1):96-102, and Wang X, Ye K, Zhang HY, et al, enhanced performance of direct oxide fuel cells by applying same-dimensional Ni and Co @ TiCnanoarrays antibodies [ J ]. International Journal of Hydrogen energy.2017,42(22): 15044-.
Disclosure of Invention
The invention aims to provide a method for preparing a porous CoNi coated carbon micro-tube electrooxidation H2O2 by using a common sowthistle flower template, which overcomes the defects of low electrooxidation rate and large concentration polarization of H2O2, and solves the problems of low utilization rate of H2O2 and the like caused by the escape of O2 generated by a self-decomposition reaction from the surface of an electrode. .
The purpose of the invention is realized as follows:
washing the flowers of the endive with acetone and deionized water for several times, removing impurities, and drying at 60 ℃ for later use. Soaking 1g of herba Sonchi Oleracei flower in NaClO2(1 wt%) water solution, decocting at 80 deg.C for 10 hr, filtering, and oven drying. 0.3mmol of Co (NO3) 2.6H 2O (0.087g) and 0.6mmol of Ni (NO3) 2.6H 2O (0.174g) were weighed out and dissolved in 30ml of deionized water. 0.5g of treated flowers of endive were soaked in the above solution, stirred at room temperature for 6 hours, then placed in an oven at 80 ℃ until the solvent was totally evaporated (about 24 hours) to give a precursor of CoNi microtubes. And putting the impregnated and dried precursor into a crucible, and calcining for 2 hours at 900 ℃ under the argon atmosphere to finally obtain the porous CoNi coated carbon micro-tube H2O2 electro-oxidation electrode.
The invention takes a porous CoNi coated carbon micro-tube as a working electrode, an Ag/AgCl (saturated KCl solution) electrode as a reference electrode and a carbon rod as a counter electrodeAt 2 mol. L-1KOH and 2 mol. L-1H2O2 is used as electrolyte, so that the electrochemical performance and stability of H2O2 electrooxidation can be obtained.
The essence of the invention is that the porous CoNi coated carbon microtube is used as an electrode material of the direct hydrogen peroxide fuel cell, and the alkaline aqueous solution of H2O2 is used as electrolyte to assemble the direct hydrogen peroxide fuel cell to obtain an electrochemical power supply.
Compared with the prior art, the invention has the beneficial effects that:
the carbon of the sonchus oleraceus flowers is calcined at high temperature to reduce cobalt ions and nickel ions into simple substances, the original tubular shape of the sonchus oleraceus flowers is reserved, the hollow tubular shape is composed of a large number of mutually cross-linked nano particles and carbon (the particle diameter is about 200-500nm), a large number of gaps are distributed on the surface, mutual transmission among ions is facilitated, and a large specific surface area provides more active sites for H2O2 adsorption. Secondly, the graphitization degree of the biomass carbon can be improved by high-temperature calcination at 900 ℃, and the carbon is used as a substrate, so that the electronic conduction capability is effectively enhanced, and the electrochemical catalytic performance of the catalyst is favorably improved. More importantly, the porous CoNi coated carbon micro-tube can adsorb and capture O2 generated by H2O2 self-decomposition reaction, so that the escape of O2 is reduced, and the utilization rate of H2O2 is improved.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
A porous CoNi-coated carbon microtube H2O2 electrooxidation electrode prepared from a common sowthistle flower template is prepared by cleaning common sowthistle flower with acetone and deionized water for several times, removing impurities, and drying at 60 deg.C. Soaking 1g of herba Sonchi Oleracei flower in NaClO2(1 wt%) water solution, decocting at 80 deg.C for 10 hr, filtering, and oven drying. 0.3mmol of Co (NO3) 2.6H 2O (0.087g) and 0.6mmol of Ni (NO3) 2.6H 2O (0.174g) were weighed out and dissolved in 30ml of deionized water. 0.5g of treated flowers of endive were soaked in the above solution, stirred at room temperature for 6 hours, then placed in an oven at 80 ℃ until the solvent was totally evaporated (about 24 hours) to give a precursor of CoNi microtubes. And putting the impregnated and dried precursor into a crucible, and calcining for 2 hours at 900 ℃ under the argon atmosphere to finally obtain the porous CoNi coated carbon micro-tube H2O2 electro-oxidation electrode.
Taking a glassy carbon electrode (diameter of 3mm) of a porous CoNi coated carbon micro-tube as a working electrode, an Ag/AgCl (saturated KCl solution) electrode as a reference electrode, a carbon rod as a counter electrode, and 2 mol.L electrolyte-1KOH and 2 mol. L-1The maximum electrooxidation current of the cyclic voltammetry curve at 0.5V is 1.486A cm-2 mg-1 at H2O 2. After a stability test of 1800s, the oxidation current density stabilized at 0.89A. cm-2. mg-1 at a potential of 0.3V.
Claims (1)
1. Porous CoNi coated carbon microtube H prepared from endive flower template2O2An electro-oxidation electrode, comprising the steps of:
cleaning the flower of the endive with acetone and deionized water for several times, removing impurities, and drying at 60 ℃ for later use;
soaking 1g of herba Sonchi Oleracei flower in 1 wt% NaClO2Boiling the water solution at 80 ℃ for 10 hours, then carrying out suction filtration and drying;
0.087g Co (NO) was weighed out3)2·6H2O and 0.174gNi (NO)3)2·6H2Dissolving O in 30ml of deionized water;
soaking 0.5g of treated sowthistle flowers in the solution, stirring for 6 hours at room temperature, and then putting the sowthistle flowers in an oven at 80 ℃ until all the solvent is evaporated for about 24 hours to obtain a CoNi microtubule precursor;
placing the immersed and dried CoNi microtube precursor in a crucible, and calcining for 2 hours at 900 ℃ under the argon atmosphere to finally obtain the porous CoNi coated carbon microtube H2O2An electric oxidation electrode.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106252619A (en) * | 2016-08-05 | 2016-12-21 | 宁波高智科技咨询服务有限公司 | A kind of preparation method of high specific energy serondary lithium battery electrode material |
| CN107697914A (en) * | 2017-08-22 | 2018-02-16 | 河南师范大学 | A kind of method for preparing nitrogen-doped porous carbon material |
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| DE102004004625B3 (en) * | 2004-01-29 | 2005-07-28 | Siemens Ag | Power supply system for submarine has hydrogen peroxide fuel cell device consisting of individual modules |
| CN103346332B (en) * | 2013-05-31 | 2016-01-27 | 哈尔滨工程大学 | The three-dimensional porous H of all-metal of carbon-free binder free 2o 2the preparation method of electro-oxidizing-catalyzing electrode |
| CN103400996B (en) * | 2013-08-20 | 2015-06-17 | 哈尔滨工程大学 | Method of taking carbon-modified and palladium-loaded cosmetic cotton as cathode material of H2O2 based fuel cell |
| CN104916451A (en) * | 2015-05-08 | 2015-09-16 | 中国科学院山西煤炭化学研究所 | Method for preparing super capacitor electrode material made of nickel oxide nanosheet grown on micro carbon tube |
| CN106669762A (en) * | 2016-12-30 | 2017-05-17 | 华南理工大学 | Nitrogen-doped carbon nanotube/Co composite catalyst and preparation method and application thereof |
| CN108736012B (en) * | 2018-04-23 | 2021-03-09 | 江汉大学 | Biomass microtube and carbon nanotube hybrid carbon material and preparation method thereof |
| CN110993969A (en) * | 2019-12-03 | 2020-04-10 | 哈尔滨工程大学 | Coquassia flower pistil hollow carbonization tube composite Co3O4H of (A) to (B)2O2Electro-reduction catalyst |
| CN111146013A (en) * | 2020-01-10 | 2020-05-12 | 厦门理工学院 | Hollow micro-tube electrode material based on ramie, and synthesis method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106252619A (en) * | 2016-08-05 | 2016-12-21 | 宁波高智科技咨询服务有限公司 | A kind of preparation method of high specific energy serondary lithium battery electrode material |
| CN107697914A (en) * | 2017-08-22 | 2018-02-16 | 河南师范大学 | A kind of method for preparing nitrogen-doped porous carbon material |
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Effective date of registration: 20231115 Address after: 150000 Room 301, building a, No. 20 Xinghai Road, Hanan industrial new town, economic development zone, Harbin, Heilongjiang Patentee after: Heilongjiang Graphite Manufacturing Innovation Center Co.,Ltd. Address before: Room 103, 1st Floor, East Zone, Building 2, Science and Technology Innovation Headquarters, Shenzhen (Harbin) Industrial Park, No. 288 Zhigu Street, Songbei District, Harbin City, Heilongjiang Province, 150029 Patentee before: Heilongjiang Nuokang Graphite New Material Technology Co.,Ltd. |