CN113718279A - Wood-based porous activated carbon/Ni0.2Mo0.8N electro-catalytic material and preparation method thereof - Google Patents
Wood-based porous activated carbon/Ni0.2Mo0.8N electro-catalytic material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 239000002023 wood Substances 0.000 title claims abstract description 138
- 239000000463 material Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000008367 deionised water Substances 0.000 claims abstract description 27
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011592 zinc chloride Substances 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims abstract description 9
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 9
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 9
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 9
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 9
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000007598 dipping method Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 14
- 235000005074 zinc chloride Nutrition 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910005809 NiMoO4 Inorganic materials 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 241000208140 Acer Species 0.000 claims description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 4
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 4
- 241001330002 Bambuseae Species 0.000 claims description 4
- 241000219071 Malvaceae Species 0.000 claims description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 4
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims description 4
- 241000018646 Pinus brutia Species 0.000 claims description 4
- 235000011613 Pinus brutia Nutrition 0.000 claims description 4
- 241000219000 Populus Species 0.000 claims description 4
- 239000011425 bamboo Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 44
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 239000002585 base Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000010411 electrocatalyst Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- -1 transition metal nitrides Chemical class 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 150000002751 molybdenum Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- PLMFYJJFUUUCRZ-UHFFFAOYSA-M decyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCC[N+](C)(C)C PLMFYJJFUUUCRZ-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910000457 iridium oxide Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
-
- 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
-
- 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
-
- 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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to wood-based porous activated carbon/Ni0.2Mo0.8N electrocatalytic material and a preparation method thereof. The technical scheme is as follows: dipping the pretreated wood block in 15-30 wt% of ZnCl2Treating the solution at 105-115 ℃ for 45-50 hours, then treating the solution at 800-900 ℃ for 2-4 hours in a high-purity argon atmosphere, and washing to obtain a wood-based porous activated carbon material; mixing Na2MoO4·2H2O and NiCl2·6H2Adding O into deionized water, stirring, adding into a hydrothermal reaction kettle after stirring, then adding the wood-based porous activated carbon material, and carrying out reaction at the temperature of 150-170 DEG CPerforming heat treatment for 5-7 hours, naturally cooling, taking out, washing and drying, and finally performing heat treatment for 10-30 minutes in an ammonia atmosphere at 550-650 ℃ to obtain the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material. The invention has simple process, low cost and environmental protection, and the prepared product can stably electrolyze water under acidic and alkaline conditions.
Description
Technical Field
The invention belongs to the technical field of electrocatalytic materials. In particular to wood-based porous activated carbon/Ni0.2Mo0.8N electrocatalytic material and a preparation method thereof.
Background
The electrolysis of water to produce high purity hydrogen is considered an effective method to meet the growing energy demands. Electrolyzed water comprises two half-reactions: the hydrogen evolution reaction at the cathode and the oxygen evolution reaction at the anode. Therefore, the research and synthesis of the electrocatalyst with low cost, high performance and strong stability has great significance for industrial electrolyzed water. At present, although platinum-based materials and iridium oxide show good activity in hydrogen evolution and oxygen evolution reactions, respectively, the high cost and scarcity of noble metals hinder large-scale industrial application, so research and development of low-cost, high-activity and stable non-noble metal-based electrocatalysts for application in practical industrial electrolytic water become hot spots. Among many non-noble metal-based electrolytic water materials, transition metal nitrides, particularly NiMoN compounds, are widely concerned by researchers because the bonding energy of compounds formed by Ni and Mo and active hydrogen atoms is moderate and the compounds are favorable for hydrogen evolution reaction, and the nitrides have the characteristics of good conductivity and corrosion resistance.
For example, the patent technology of "a preparation method of vanadium doped transition metal nitride and application thereof" (CN110787824A) synthesizes V-NiMoN material on nickel foam by hydrothermal method, but nickel foam is easy to dissolve under acidic condition and is unstable during use.
Such as document I (Sangg H P, Jo T H, Min H L, et al. high ply active and stable nickel-molybdenum nitride (Ni)2Mo3N)electrocatalyst for hydrogen evolution[J]Journal of Materials Chemistry A,2021,9: 4945-4951) reports direct mixing of foamed nickel as a nickel source with molybdenum salt and urea, heat treatment under nitrogen atmosphere, and one-step synthesis of Ni2Mo3N electrocatalytic material, but the electrocatalytic hydrogen evolution reaction can be carried out only under alkaline conditions.
As reported in document II (Chang B, Yang J, Shao Y L, et al. metallurgical NiMoN nanowines with a reactive function: an ultra-effective biological activity for over water splitting [ J ]. ChemUSchem, 2018,11(18): 3198. cake 3207.), a DTAB surfactant was used in addition to a nickel salt and a molybdenum salt to synthesize NiMoN materials, and the synthesis steps were complicated and could not stabilize electrolyzed water under acidic conditions.
As reported in document III (Yin Z X, Sun Y, Zhu C L, et al, metallurgical Ni-Mo nitride nanoparticles as active and stable biochemical electrolytes for full water splitting [ J ]. Journal of Materials Chemistry A,2017,5: 13648-.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide wood-based porous activated carbon/Ni which is simple in process, low in cost and environment-friendly0.2Mo0.8A preparation method of the N electrocatalytic material; the wood-based porous activated carbon/Ni prepared by the method0.2Mo0.8The N electrocatalytic material can stabilize electrolyzed water under acidic and alkaline conditions.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
step one, cutting the wood into blocks, washing with deionized water 2Drying for 3 times at 55-65 ℃ to obtain pretreated wood blocks; dipping 1 part by mass of the pretreated wood block into 3-5 parts by mass of 15-30 wt% ZnCl2Treating the wood blocks in the solution at 105-115 ℃ for 45-50 hours to obtain wood blocks treated by zinc chloride; and (3) carrying out heat treatment on the wood blocks treated by the zinc chloride for 2-4 hours under the conditions of high-purity argon atmosphere and 800-900 ℃, washing with deionized water for 3-4 times, and drying to obtain the wood-based porous activated carbon material.
Step two, adding 1 part by mass of Na2MoO4·2H2O and 1-2 parts by mass of NiCl2·6H2Adding O into 97-98 parts by mass of deionized water, and stirring for 10-20 minutes to obtain a mixed solution; adding the mixed solution into a hydrothermal reaction kettle, adding 3-5 parts by mass of the wood-based porous activated carbon material, carrying out heat treatment at 150-170 ℃ for 5-7 hours, naturally cooling to room temperature, taking out, washing with deionized water for 2-3 times, and drying for 24-48 hours to obtain wood-based porous activated carbon/NiMoO4A material.
Step three, carrying out porous activated carbon/NiMoO on the wood head base4The material is subjected to heat treatment for 10-30 minutes under the conditions of ammonia atmosphere and 550-650 ℃ to prepare the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material.
The wood is one of poplar, pine, basswood, bamboo, sapelli wood and maple wood.
The length, width and height of the wood block are (30-40) x (10-20) x (5-10) mm.
The purity of the high-purity argon is more than 99.999%.
The purity of the ammonia gas is more than 99.6 percent.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the invention firstly soaks the pretreated wood block in ZnCl2In the solution, performing heat treatment in a high-purity argon atmosphere at 800-900 ℃ to obtain a wood-based porous activated carbon material; then adding Na2MoO4·2H2O、NiCl2·6H2O andadding the mixed solution of deionized water into a hydrothermal reaction kettle, adding a wood-based porous activated carbon material for hydrothermal reaction, and finally carrying out heat treatment in an ammonia atmosphere at 550-650 ℃ to obtain the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material. The invention does not need to use a surfactant, has simple process, saves the production cost and is environment-friendly.
2. The wood-based porous activated carbon/Ni synthesized by the invention0.2Mo0.8The N electrocatalysis material has strong corrosion resistance because the substrate material is a wood-based porous activated carbon material, and cannot be corroded by acid or alkali, so that the N electrocatalysis material can stabilize electrolyzed water under acidic and alkaline conditions.
3. The raw material of the substrate material is wood with abundant reserves, low cost and environmental protection, and the prepared wood-based porous activated carbon/Ni0.2Mo0.8The production cost of the N electrocatalytic material is low.
Therefore, the method has the characteristics of simple process, low cost and environmental friendliness, and the prepared wood-based porous activated carbon/Ni0.2Mo0.8The N electrocatalytic material can stabilize electrolyzed water under acidic and alkaline conditions.
Drawings
FIG. 1 shows a wood-based porous activated carbon/Ni prepared according to the present invention0.2Mo0.8SEM photograph of N electrocatalytic material;
FIG. 2 shows the wood-based porous activated carbon/Ni shown in FIG. 10.2Mo0.8An electro-catalytic hydrogen evolution LSV curve diagram of the N electro-catalytic material under an acidic condition;
FIG. 3 is the wood-based porous activated carbon/Ni shown in FIG. 10.2Mo0.8An electro-catalytic oxygen evolution LSV curve diagram of the N electro-catalytic material under an acidic condition;
FIG. 4 is the wood-based porous activated carbon/Ni shown in FIG. 10.2Mo0.8And (3) a full hydrolysis stability test chart of the N electro-catalytic material under an acidic condition.
Detailed Description
The invention is further described with reference to the following figures and detailed description, without limiting its scope.
Wood-based porous activated carbon/Ni0.2Mo0.8N electrocatalytic material and a preparation method thereof. The preparation method comprises the following steps:
cutting the wood into blocks, washing the blocks with deionized water for 2-3 times, and drying the blocks at the temperature of 55-65 ℃ to obtain pretreated wood blocks; dipping 1 part by mass of the pretreated wood block into 3-5 parts by mass of 15-30 wt% ZnCl2Treating the wood blocks in the solution at 105-115 ℃ for 45-50 hours to obtain wood blocks treated by zinc chloride; and (3) carrying out heat treatment on the wood blocks treated by the zinc chloride for 2-4 hours under the conditions of high-purity argon atmosphere and 800-900 ℃, washing with deionized water for 3-4 times, and drying to obtain the wood-based porous activated carbon material.
Step two, adding 1 part by mass of Na2MoO4·2H2O and 1-2 parts by mass of NiCl2·6H2Adding O into 97-98 parts by mass of deionized water, and stirring for 10-20 minutes to obtain a mixed solution; adding the mixed solution into a hydrothermal reaction kettle, adding 3-5 parts by mass of the wood-based porous activated carbon material, carrying out heat treatment at 150-170 ℃ for 5-7 hours, naturally cooling to room temperature, taking out, washing with deionized water for 2-3 times, and drying for 24-48 hours to obtain wood-based porous activated carbon/NiMoO4A material.
Step three, carrying out porous activated carbon/NiMoO on the wood head base4The material is subjected to heat treatment for 10-30 minutes under the conditions of ammonia atmosphere and 550-650 ℃ to prepare the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material.
The wood is one of poplar, pine, basswood, bamboo, sapelli wood and maple wood.
The length, width and height of the wood block are (30-40) x (10-20) x (5-10) mm.
In this embodiment:
the purity of the high-purity argon is more than 99.999 percent;
the purity of the ammonia gas is more than 99.6 percent.
The detailed description is omitted in the embodiments.
Example 1
Wood-based porous activated carbon/Ni0.2Mo0.8N electrocatalytic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
cutting wood into blocks, washing the blocks for 2 times by using deionized water, and drying the blocks at the temperature of 55 ℃ to obtain pretreated wood blocks; dipping 1 part by mass of the pretreated wood block in 5 parts by mass of 15 wt% ZnCl2Treating the wood blocks in the solution at 105 ℃ for 45 hours to obtain wood blocks treated by zinc chloride; and (3) carrying out heat treatment on the wood blocks treated by the zinc chloride for 2 hours in a high-purity argon atmosphere at 800 ℃, washing with deionized water for 3 times, and drying to obtain the wood-based porous activated carbon material.
Step two, adding 1 part by mass of Na2MoO4·2H2O and 1 part by mass of NiCl2·6H2Adding O into 98 parts by mass of deionized water, and stirring for 10 minutes to obtain a mixed solution; adding the mixed solution into a hydrothermal reaction kettle, adding 3 parts by mass of the wood-based porous activated carbon material, carrying out heat treatment at 150 ℃ for 5 hours, naturally cooling to room temperature, taking out, washing with deionized water for 2 times, and drying for 24 hours to obtain wood-based porous activated carbon/NiMoO4A material.
Step three, carrying out porous activated carbon/NiMoO on the wood head base4The material is thermally treated for 10 minutes under the conditions of ammonia atmosphere and 550 ℃, and the wood-based porous activated carbon/Ni is prepared0.2Mo0.8An N electrocatalytic material.
In this embodiment: the wood is basswood; the length × width × height of the block is 40 × 20 × 10 mm.
Example 2
Wood-based porous activated carbon/Ni0.2Mo0.8N electrocatalytic material and a preparation method thereof. The preparation method is characterized by comprising the following steps:
cutting wood into blocks, washing the blocks with deionized water for 3 times, and drying the blocks at the temperature of 60 ℃ to obtain pretreated wood blocks; dipping 1 part by mass of the pretreated wood block in 4 parts by mass of 20 wt% ZnCl2In solution, in 11Treating at 0 deg.C for 48 hr to obtain wood blocks treated with zinc chloride; and (3) carrying out heat treatment on the wood blocks treated by the zinc chloride for 3 hours under the conditions of high-purity argon atmosphere and 850 ℃, washing for 3 times by using deionized water, and drying to obtain the wood-based porous activated carbon material.
Step two, adding 1 part by mass of Na2MoO4·2H2O and 1.5 parts by mass of NiCl2·6H2Adding O into 97.5 parts by mass of deionized water, and stirring for 15 minutes to obtain a mixed solution; adding the mixed solution into a hydrothermal reaction kettle, adding 4 parts by mass of the wood-based porous activated carbon material, carrying out heat treatment at 160 ℃ for 6 hours, naturally cooling to room temperature, taking out, washing with deionized water for 2 times, and drying for 36 hours to obtain wood-based porous activated carbon/NiMoO4A material.
Step three, carrying out porous activated carbon/NiMoO on the wood head base4The material is thermally treated for 20 minutes under the conditions of ammonia atmosphere and 600 ℃ to prepare the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material.
In this embodiment: the wood is one of pine, poplar and sapelli wood; the length × width × height of the block is 35 × 15 × 8 mm.
Example 3
Wood-based porous activated carbon/Ni0.2Mo0.8N electrocatalytic material and a preparation method thereof. The preparation method is characterized by comprising the following steps:
cutting wood into blocks, washing the blocks for 2 times by using deionized water, and drying the blocks at the temperature of 65 ℃ to obtain pretreated wood blocks; dipping 1 part by mass of the pretreated wood block in 3 parts by mass of 30 wt% ZnCl2Treating the wood blocks in the solution at 115 deg.C for 50 hr to obtain wood blocks treated with zinc chloride; and (3) carrying out heat treatment on the wood blocks treated by the zinc chloride for 4 hours under the conditions of high-purity argon atmosphere and 900 ℃, washing for 4 times by using deionized water, and drying to obtain the wood-based porous activated carbon material.
Step two, adding 1 part by mass of Na2MoO4·2H2O and 2 parts by mass of NiCl2·6H2O is added to 97 massStirring the mixture for 20 minutes in the deionized water to obtain a mixed solution; adding the mixed solution into a hydrothermal reaction kettle, adding 5 parts by mass of the wood-based porous activated carbon material, carrying out heat treatment at 170 ℃ for 7 hours, naturally cooling to room temperature, taking out, washing with deionized water for 3 times, and drying for 48 hours to obtain the wood-based porous activated carbon/NiMoO4A material.
Step three, carrying out porous activated carbon/NiMoO on the wood head base4The material is thermally treated for 30 minutes under the condition of ammonia atmosphere and 650 ℃ to prepare the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material.
In this embodiment: the wood is bamboo or maple; the length × width × height of the block is 30 × 10 × 5 mm.
Compared with the prior art, the specific implementation mode has the following advantages:
1. in the specific embodiment, the pretreated wood block is dipped in ZnCl2In the solution, performing heat treatment in a high-purity argon atmosphere at 800-900 ℃ to obtain a wood-based porous activated carbon material; then adding Na2MoO4·2H2O、NiCl2·6H2Adding a mixed solution of O and deionized water into a hydrothermal reaction kettle, adding a wood-based porous activated carbon material for hydrothermal reaction, and finally carrying out heat treatment in an ammonia atmosphere at 550-650 ℃ to obtain the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material. The specific implementation mode does not need to use a surfactant, has simple process, saves the production cost and is environment-friendly.
2. Wood-based porous activated carbon/Ni prepared according to this embodiment0.2Mo0.8The N electrocatalytic material is shown in the attached figure: FIG. 1 is a wood-based porous activated carbon/Ni prepared in example 10.2Mo0.8SEM photograph of N electrocatalytic material; FIG. 2 shows the wood-based porous activated carbon/Ni shown in FIG. 10.2Mo0.8An electro-catalytic hydrogen evolution LSV curve diagram of the N electro-catalytic material under an acidic condition; FIG. 3 is the wood-based porous activated carbon/Ni shown in FIG. 10.2Mo0.8An electro-catalytic oxygen evolution LSV curve diagram of the N electro-catalytic material under an acidic condition; FIG. 4Is wood-based porous activated carbon/Ni shown in figure 10.2Mo0.8And (3) a full hydrolysis stability test chart of the N electro-catalytic material under an acidic condition. As can be seen from FIG. 1, the prepared wood-based porous activated carbon/Ni0.2Mo0.8A large amount of one-dimensional Ni with the size of 5-10 mu m exists in the N electro-catalysis material0.2Mo0.8The N micron lines grow on the wood-based porous activated carbon; as can be seen from fig. 2: at a current density of 10mA cm-2The prepared wood-based porous activated carbon/Ni0.2Mo0.8The electrocatalytic hydrogen evolution overpotential of the N electrocatalytic material is 23.7 mV; as can be seen from fig. 3: at a current density of 50mA cm-2The prepared wood-based porous activated carbon/Ni0.2Mo0.8The electrocatalytic oxygen evolution overpotential of the N electrocatalytic material is 455 mV; as can be seen from fig. 4: when the applied voltage is 1.7V, the prepared wood-based porous activated carbon/Ni0.2Mo0.8The N electrocatalytic material can stabilize electrolyzed water under acidic conditions. Namely, the base material is wood-based porous activated carbon material, so that the electrolytic water is strong in corrosion resistance and cannot be corroded by acid or alkali, and therefore, the electrolytic water can be stably electrolyzed under acidic and alkaline conditions.
3. The base material of the embodiment is wood with abundant reserves, low cost and environmental protection, so the prepared wood-based porous activated carbon/Ni0.2Mo0.8The production cost of the N electrocatalytic material is low.
Therefore, the specific implementation mode has the characteristics of simple process, low cost and environmental friendliness, and the prepared wood-based porous activated carbon/Ni0.2Mo0.8The N electrocatalytic material can stabilize electrolyzed water under acidic and alkaline conditions.
Claims (6)
1. Wood-based porous activated carbon/Ni0.2Mo0.8The preparation method of the N electrocatalytic material is characterized by comprising the following steps:
cutting the wood into blocks, washing the blocks with deionized water for 2-3 times, and drying the blocks at the temperature of 55-65 ℃ to obtain pretreated wood blocks; dipping 1 part by mass of the pretreated wood block into 3-5 parts by mass of the pretreated wood block15 to 30 wt% of ZnCl2Treating the wood blocks in the solution at 105-115 ℃ for 45-50 hours to obtain wood blocks treated by zinc chloride; carrying out heat treatment on the wood block treated by the zinc chloride for 2-4 hours under the conditions of high-purity argon atmosphere and 800-900 ℃, washing with deionized water for 3-4 times, and drying to obtain a wood-based porous activated carbon material;
step two, adding 1 part by mass of Na2MoO4·2H2O and 1-2 parts by mass of NiCl2·6H2Adding O into 97-98 parts by mass of deionized water, and stirring for 10-20 minutes to obtain a mixed solution; adding the mixed solution into a hydrothermal reaction kettle, adding 3-5 parts by mass of the wood-based porous activated carbon material, carrying out heat treatment at 150-170 ℃ for 5-7 hours, naturally cooling to room temperature, taking out, washing with deionized water for 2-3 times, and drying for 24-48 hours to obtain wood-based porous activated carbon/NiMoO4A material;
step three, carrying out porous activated carbon/NiMoO on the wood head base4The material is subjected to heat treatment for 10-30 minutes under the conditions of ammonia atmosphere and 550-650 ℃ to prepare the wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material.
2. The wood-based porous activated carbon/Ni of claim 10.2Mo0.8The preparation method of the N electro-catalysis material is characterized in that the wood is one of poplar wood, pine wood, basswood, bamboo, sapelli wood and maple wood.
3. The wood-based porous activated carbon/Ni of claim 10.2Mo0.8The preparation method of the N electrocatalytic material is characterized in that the length, the width and the height of the wood block are (30-40) x (10-20) x (5-10) mm.
4. The wood-based porous activated carbon/Ni of claim 10.2Mo0.8The preparation method of the N electrocatalytic material is characterized in that the purity of the high-purity argon is more than 99.999 percent.
5. The wood-based porous activated carbon/Ni of claim 10.2Mo0.8The preparation method of the N electrocatalytic material is characterized in that the purity of the ammonia gas is more than 99.6 percent.
6. Wood-based porous activated carbon/Ni0.2Mo0.8N electrocatalytic material, characterized in that said wood-based porous activated carbon/Ni0.2Mo0.8The N electrocatalytic material is the wood-based porous activated carbon/Ni as claimed in any one of claims 1 to 50.2Mo0.8Preparation method of N-electrocatalytic material for preparing wood-based porous activated carbon/Ni0.2Mo0.8An N electrocatalytic material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115044920A (en) * | 2022-08-16 | 2022-09-13 | 河南师范大学 | Preparation method of self-supporting ultralow-crystallinity nano-array electrocatalyst for hydrogen production by water electrolysis |
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