CN113278985A - Preparation method of nickel oxide and lignin carbon electrochemical catalysis nano composite material - Google Patents
Preparation method of nickel oxide and lignin carbon electrochemical catalysis nano composite material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 23
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 22
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229920005610 lignin Polymers 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 15
- 239000002114 nanocomposite Substances 0.000 title description 17
- 238000006555 catalytic reaction Methods 0.000 title description 4
- 230000003197 catalytic effect Effects 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 108010010803 Gelatin Proteins 0.000 claims abstract description 11
- 229920000159 gelatin Polymers 0.000 claims abstract description 11
- 239000008273 gelatin Substances 0.000 claims abstract description 11
- 235000019322 gelatine Nutrition 0.000 claims abstract description 11
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920001732 Lignosulfonate Polymers 0.000 claims abstract description 5
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 4
- 239000002121 nanofiber Substances 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229960000583 acetic acid Drugs 0.000 claims description 16
- 239000012362 glacial acetic acid Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 239000000835 fiber Substances 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 8
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 abstract 1
- 238000003763 carbonization Methods 0.000 abstract 1
- 229910001453 nickel ion Inorganic materials 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 13
- 239000001257 hydrogen Substances 0.000 description 13
- 229910052739 hydrogen Inorganic materials 0.000 description 13
- 238000001816 cooling Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000001523 electrospinning Methods 0.000 description 8
- 239000012456 homogeneous solution Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 8
- 238000009987 spinning Methods 0.000 description 8
- 239000012300 argon atmosphere Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229920006125 amorphous polymer Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007603 infrared drying Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- 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
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Fibers (AREA)
- Catalysts (AREA)
Abstract
A preparation method of a nickel oxide and lignin carbon composite electrochemical catalytic material comprises the steps of taking lignosulfonate and gelatin as raw materials, introducing nickel ions in a solution state, and finally obtaining nickel oxide/lignin carbon composite nano fibers through electrostatic spinning and high-temperature carbonization. The raw materials used in the invention are natural, pollution-free, wide in source and cheap, and the preparation method is simple; the prepared nano nickel oxide/carbon composite material has the characteristics of high specific surface area, excellent catalytic performance and the like.
Description
Technical Field
The invention belongs to the field of electrochemistry and new energy materials, and relates to a preparation method of a nickel oxide and lignin carbon electrochemical catalysis nano composite material.
Background
At present, with the increase of the world population, the development of technology and the improvement of living standard, the demand of people for energy sources is continuously increased, and chemical fuels with the largest usage ratio are gradually replaced by some novel renewable energy sources (such as hydrogen energy, wind energy, solar energy, nuclear energy and the like) due to the problems of resource shortage, serious pollution and the like. Among them, hydrogen energy is widely paid attention to by virtue of its light weight, convenient transportation, non-toxicity, innocuity, etc. The commonly used methods for preparing hydrogen at present comprise hydrogen production by mineral fuel, microbial hydrogen production, hydrogen production by photocatalytic water decomposition and hydrogen production by electrocatalytic water decomposition. Among them, the hydrogen production method by fossil fuel is relatively simple, simple in process and high in industrialization degree, but consumes a large amount of fossil energy and produces a large amount of carbon dioxide, and the efficiency is low. Compared with the prior art, the method has the advantages of higher hydrogen production efficiency by electrolyzing water, no pollution, high controllability and the like. However, the overpotential of the electrode reaction for water electrolysis is high in industry, a large amount of electric energy is consumed, the cost for hydrogen production is greatly increased, and the industrial application of hydrogen production by water electrolysis is limited to a great extent.
In order to reduce the influence of over potential, many researches find that the addition of noble metal catalysts (platinum, palladium, ruthenium, rhodium and the like) can improve the efficiency and stability of hydrogen evolution reaction, but the defects of expensive noble metal, scarce source and the like greatly hinder the industrial production of the method. To address this problem, research has been directed to certain non-noble metals and non-metallic catalysts, such as molybdenum disulfide (MoS)2) Compounds of the metal tungsten (W) and various types of compounds of some transition metals. Wherein, the composite of metal oxides such as nickel oxide and the like and carbon materials with excellent conductivity has high-efficiency catalytic stability and excellent catalytic activity.
As a matrix of the loaded carbon material, lignin is a heterogeneous and amorphous polymer, can be extracted from various low-cost papermaking wastewater, and has the content inferior to that of cellulose. Meanwhile, the lignin contains a large number of active groups such as hydroxyl, carboxyl, sulfonic acid group and the like, and the lignin and partial groups form a synergistic effect to further promote the catalytic performance of the composite material.
The method utilizes the electrostatic spinning technology to greatly improve the length-diameter ratio of the fibers and the specific surface area of the carbon material, thereby improving the catalytic performance of the nickel oxide/carbon nano composite fibers. Meanwhile, the method has the advantages of low cost, simple process, high catalytic performance and the like, and has very wide application prospect.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a nickel oxide and lignin carbon electrochemical catalysis nano composite material.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a nickel oxide and lignin carbon composite electrochemical catalytic material comprises the following steps:
(1) adding 2g-6g of gelatin into a glacial acetic acid/water mixed solution, wherein the mass of glacial acetic acid/water in the glacial acetic acid/water mixed solution is 5-10g and 3-8g respectively, and magnetically stirring for 2-3 hours at room temperature;
(2) adding 10-20 wt% of lignosulfonate into the solution, uniformly stirring, adding a nickel source, and magnetically stirring at room temperature for 6-8 hours to obtain a brown viscous solution;
(3) preparing the obtained brown viscous liquid into nano fibers by an electrostatic spinning technology;
(4) vacuum drying the obtained fiber in a vacuum oven for 24-48h, and calcining at high temperature for 2-3 h in a tube furnace under the protection of inert gas;
(5) and taking out the carbonized product, grinding and drying in vacuum to obtain the required product.
Further, in the step (1), the mass ratio of the glacial acetic acid/water mixed solution is 5:2-5: 4.
Still further, in the step (2), the lignosulfonate is sodium lignosulfonate or calcium lignosulfonate.
Furthermore, in the step (2), the nickel source is one or a mixture of two or more of nickel nitrate, nickel sulfate and nickel chloride.
In the step (4), the drying temperature is 60-80 ℃.
In the step (4), the inert gas is one or a mixture of two or more of dried nitrogen, argon and helium.
In the step (4), the high-temperature calcination temperature is 800-1000 ℃.
The invention has the following beneficial effects: the preparation method is simple and environment-friendly, and has wide raw material sources and low price. The catalyst has higher specific surface area and stable catalytic performance and is very suitable for hydrogen evolution.
Drawings
Fig. 1 is an SEM image of a nickel oxide and lignin carbon electrochemically catalyzed nanocomposite prepared using the present invention.
FIG. 2 is a drawing of nitrogen desorption of nickel oxide and lignin carbon electrochemically catalyzed nanocomposites prepared with the present invention.
FIG. 3 is a CV curve of nickel oxide and lignocellulosic carbon electrochemically catalyzed nanocomposites prepared with the present invention;
fig. 4 is an impedance curve of a nickel oxide and lignin carbon electrochemically catalyzed nanocomposite prepared using the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1
Referring to fig. 1 to 4, a method for preparing a nickel oxide/carbon composite nano electrochemical catalytic material,
2g of gelatin granules were weighed, added to a mixed solution of 5g of glacial acetic acid and 3g of deionized water, and magnetically stirred at room temperature for 2 hours. Subsequently, 10% wt of sodium lignosulfonate (i.e. 1.11g of sodium lignosulfonate) was added and stirred magnetically at room temperature for 6 hours until homogeneous. Subsequently, 0.25g of nickel nitrate hexahydrate was added, and stirring was continued until uniform. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground with a mortar and then placed in a vacuum oven at 60 ℃ to be vacuum-dried for 24 hours. And putting the dried product into a tubular furnace, calcining for 150 minutes at 800 ℃ in an argon atmosphere, cooling and grinding to obtain the nano composite fiber.
Preparing an electrode: adding 0.004g of product sample powder into 0.9ml of absolute ethyl alcohol, adding 0.1ml of Nafion solution, after uniformly mixing by ultrasonic waves, dripping the mixture on the surface of 1 x 1 carbon paper, drying the mixture by using an infrared drying lamp, putting the dried mixture into a vacuum oven for vacuum drying for 24 hours to prepare a working electrode, and forming a three-electrode system by using an Ag/AgCl electrode as a reference electrode, a carbon rod as a counter electrode and KOH solution as electrolyte to test the electrochemical performance.
Example 2
2g of gelatin granules were weighed, added to a mixed solution of 10g of glacial acetic acid and 8g of deionized water, and magnetically stirred at room temperature for 3 hours. Subsequently, 20% wt sodium lignosulfonate (i.e. 5g sodium lignosulfonate) was added and stirred magnetically at room temperature for 8 hours to homogeneity. Subsequently, 0.25g of nickel nitrate hexahydrate was added, and stirring was continued until uniform. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground in a mortar and then placed in a vacuum oven at 80 ℃ for vacuum drying for 48 hours. And putting the dried product into a tubular furnace, calcining for 180 minutes at 1000 ℃ in an argon atmosphere, cooling and grinding to obtain the nano composite fiber.
Electrode preparation was consistent with the above examples.
Example 3
2g of gelatin granules were weighed, added to a mixed solution of 10g of glacial acetic acid and 4g of deionized water, and magnetically stirred at room temperature for 2.5 hours. Subsequently, 20% wt sodium lignosulfonate (i.e. 4g sodium lignosulfonate) was added and stirred magnetically at room temperature for 7 hours until homogeneous. Subsequently, 0.25g of nickel nitrate hexahydrate was added, and stirring was continued until uniform. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground with a mortar and then placed in a vacuum oven at 70 ℃ to be vacuum-dried for 24 hours. And putting the dried product into a tubular furnace, calcining for 120 minutes at 900 ℃ in an argon atmosphere, cooling and grinding to obtain the nano composite fiber.
Electrode preparation was consistent with the above examples.
Example 4
6g of gelatin granules were weighed, added to a mixed solution of 10g of glacial acetic acid and 6g of deionized water, and magnetically stirred at room temperature for 3 hours. Subsequently, 15% wt of calcium lignosulphonate (i.e. 3.88g of calcium lignosulphonate) was added and stirred magnetically at room temperature for 6 hours to homogeneity. Subsequently, 0.25g of nickel nitrate hexahydrate was added, and stirring was continued until uniform. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground with a mortar and then placed in a vacuum oven at 60 ℃ to be vacuum-dried for 24 hours. And putting the dried product into a tubular furnace, calcining for 120 minutes at 1000 ℃ in an argon atmosphere, cooling and grinding to obtain the nano composite fiber.
Electrode preparation was consistent with the above examples.
Example 5
2g of gelatin granules were weighed, added to a mixed solution of 5g of glacial acetic acid and 3g of deionized water, and magnetically stirred at room temperature for 2 hours. Subsequently, 3g of calcium lignosulfonate was added and stirred magnetically at room temperature for 6 hours to homogeneity. Subsequently, 0.5g of nickel nitrate hexahydrate was added, and stirring was continued until uniform. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground with a mortar and then placed in a vacuum oven at 60 ℃ to be vacuum-dried for 24 hours. And putting the dried product into a tubular furnace, calcining for 120 minutes at 900 ℃ in an argon atmosphere, cooling and grinding to obtain the nano composite fiber.
Electrode preparation was consistent with the above examples.
Example 5
4g of gelatin particles were weighed, added to a mixed solution of 6g of glacial acetic acid and 4g of deionized water, and magnetically stirred at room temperature for 2 hours. Subsequently, 10% wt of calcium lignosulphonate (i.e. 1.56g of calcium lignosulphonate) was added and stirred magnetically at room temperature for 6 hours to homogeneity. Subsequently, 0.5g of nickel nitrate hexahydrate was added, and stirring was continued until uniform. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground with a mortar and then placed in a vacuum oven at 60 ℃ to be vacuum-dried for 24 hours. And putting the dried product into a tubular furnace, calcining for 120 minutes at 1000 ℃ in a nitrogen atmosphere, cooling and grinding to obtain the nano composite fiber.
Electrode preparation was consistent with the above examples.
Example 6
6g of gelatin granules were weighed, added to a mixed solution of 10g of glacial acetic acid and 4g of deionized water, and magnetically stirred at room temperature for 2 hours. Subsequently, 5g of sodium lignin sulfonate was added and stirred magnetically at room temperature for 6 hours until homogeneous. Subsequently, 0.5g of nickel chloride was added and stirring was continued until homogeneous. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground with a mortar and then placed in a vacuum oven at 60 ℃ to be vacuum-dried for 24 hours. And putting the dried product into a tubular furnace, calcining for 90 minutes at 1000 ℃ in a nitrogen atmosphere, cooling and grinding to obtain the nano composite fiber.
Electrode preparation was consistent with the above examples. .
Example 7
4g of gelatin particles were weighed, added to a mixed solution of 8g of glacial acetic acid and 3g of deionized water, and magnetically stirred at room temperature for 3 hours. Subsequently, 2g of calcium lignosulphonate was added and stirred magnetically at room temperature for 6 hours until homogeneous. Subsequently, 1g of nickel sulfate was added, and the mixture was stirred until uniform. The homogeneous solution was then poured into a disposable syringe for electrospinning. The obtained spinning product was ground with a mortar and then placed in a vacuum oven at 60 ℃ to be vacuum-dried for 24 hours. And putting the dried product into a tubular furnace, calcining for 12 minutes at 1000 ℃ in an argon atmosphere, cooling and grinding to obtain the nano composite fiber.
Electrode preparation was consistent with the above examples.
The embodiments described in this specification are merely illustrative of implementations of the inventive concepts, which are intended for purposes of illustration only. The scope of the present invention should not be construed as being limited to the particular forms set forth in the examples, but rather as being defined by the claims and the equivalents thereof which can occur to those skilled in the art upon consideration of the present inventive concept.
Claims (7)
1. A preparation method of a nickel oxide and lignin carbon composite electrochemical catalytic material is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) adding 2g-6g of gelatin into a glacial acetic acid/water mixed solution, wherein the mass of glacial acetic acid/water in the glacial acetic acid/water mixed solution is 5-10g and 3-8g respectively, and magnetically stirring for 2-3 hours at room temperature;
(2) adding 10-20 wt% of lignosulfonate into the solution, uniformly stirring, adding a nickel source, and magnetically stirring at room temperature for 6-8 hours to obtain a brown viscous solution;
(3) preparing the obtained brown viscous liquid into nano fibers by an electrostatic spinning technology;
(4) vacuum drying the obtained fiber in a vacuum oven for 24-48h, and calcining at high temperature for 2-3 h in a tube furnace under the protection of inert gas;
(5) and taking out the carbonized product, grinding and drying in vacuum to obtain the required product.
2. The method for preparing the nickel oxide and lignin carbon composite electrochemical catalytic material according to claim 1, wherein: in the step (1), the mass ratio of the glacial acetic acid/water mixed solution is 5:2-5: 4.
3. The method for preparing the nickel oxide and lignin carbon composite electrochemical catalytic material according to claim 1 or 2, characterized in that: in the step (2), the lignosulfonate is sodium lignosulfonate calcium lignosulfonate.
4. The method for preparing the nickel oxide and lignin carbon composite electrochemical catalytic material according to claim 1 or 2, characterized in that: in the step (2), the nickel source is one or a mixture of two or more of nickel nitrate, nickel sulfate and nickel chloride.
5. The method for preparing the nickel oxide and lignin carbon composite electrochemical catalytic material according to claim 1 or 2, characterized in that: in the step (4), the drying temperature is 60-80 ℃.
6. The method for preparing the nickel oxide and lignin carbon composite electrochemical catalytic material according to claim 1 or 2, characterized in that: in the step (4), the inert gas is one or a mixture of two or more of dried nitrogen, argon and helium.
7. The method for preparing the nickel oxide and lignin carbon composite electrochemical catalytic material according to claim 1 or 2, characterized in that: in the step (4), the high-temperature calcination temperature is 800-1000 ℃.
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| CN202110360300.0A CN113278985A (en) | 2021-04-02 | 2021-04-02 | Preparation method of nickel oxide and lignin carbon electrochemical catalysis nano composite material |
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| CN202110360300.0A CN113278985A (en) | 2021-04-02 | 2021-04-02 | Preparation method of nickel oxide and lignin carbon electrochemical catalysis nano composite material |
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