CN106531476A - Preparation method of metal oxide/ carbon composite material - Google Patents
Preparation method of metal oxide/ carbon composite material Download PDFInfo
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- CN106531476A CN106531476A CN201611246093.1A CN201611246093A CN106531476A CN 106531476 A CN106531476 A CN 106531476A CN 201611246093 A CN201611246093 A CN 201611246093A CN 106531476 A CN106531476 A CN 106531476A
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- biomass
- metal oxide
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- carbon composite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 27
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 27
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002028 Biomass Substances 0.000 claims abstract description 58
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 150000003839 salts Chemical class 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 14
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000006260 foam Substances 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 22
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000007654 immersion Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 3
- 235000018262 Arachis monticola Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 235000020232 peanut Nutrition 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 241000609240 Ambelania acida Species 0.000 claims description 2
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000010905 bagasse Substances 0.000 claims description 2
- 229910052571 earthenware Inorganic materials 0.000 claims description 2
- 239000010903 husk Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000010257 thawing Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000002791 soaking Methods 0.000 abstract description 5
- 239000003575 carbonaceous material Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract description 2
- 230000008901 benefit Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000002322 conducting polymer Substances 0.000 description 3
- 229920001940 conductive polymer Polymers 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacturing & Machinery (AREA)
Abstract
The invention discloses a preparation method of a metal oxide/ carbon composite material, and belongs to the technical fields of material science and electrochemical science. The preparation method of the metal oxide/ carbon composite material is mainly characterized by comprising the steps of: (1) washing, drying and crushing biomass, then soaking the biomass into a metal salt solution, performing centrifugal vacuum freeze drying, and repeating 2-5 times till the mass of the dried biomass is increased by 0.1-15%; (2) putting solid salt into a crucible, continuously introducing inert gas, and heating to 450-900 DEG C so that the solid salt in the crucible is melted; and (3) wrapping the biomass with nickel foam, immersing into the melted solid salt, preserving the heat for 0.25-2h, cooling to room temperature, taking the product out, washing, centrifuging, and performing vacuum freeze drying. The preparation method is short in process flow, simple in equipment, wide in material source and low in cost, and the metal oxide in the prepared metal oxide/ carbon composite material can be uniformly loaded on the carbon material.
Description
Technical field
The invention belongs to material science and electrochemistry science and technology field, and in particular to a kind of to be used for electric chemical super electric capacity
The preparation method of the metal oxide/carbon composite of device.
Background technology
As fossil energy is exhausted and global warming makes utilization pay attention to day by day of the people to regenerative resource, send out energetically
Exhibition clean energy vehicle becomes irreversible trend.With the commercialized development of electric automobile, hybrid vehicle etc., efficiently
Energy storage and switch technology be faced with increasing challenge.Ultracapacitor is one kind between battery and physical capacitors
Energy storage device between device.Because of its high-energy-density, can obtain the features such as instantaneous large-current fast charging and discharging, long circulation life
People more and more pay close attention to.
According to the difference of energy storage mechnism, ultracapacitor can be divided into two kinds：One kind is that electric charge is stored in carbon electrode/electrolysis
In electric double layer at matter solution interface；Second is Faraday pseudo-capacitance or pseudo-capacitance, is in metal oxide or conducting polymer
Quick Oxidation reduction reaction in thing surface or body phase and energy storage.The main electrode material of the first capacitor is with high-ratio surface
Long-pending material with carbon element, its advantage are that material is cheap and easy to get, good cycle, and Technical comparing is ripe, has the disadvantage that energy density is not high.
Second main material of capacitor is metal oxide and conducting polymer, and its advantage is that specific capacity is higher than material with carbon element, but gold
Category oxide high cost, poorly conductive or toxic, conducting polymer volume in charge and discharge process can change, cause
The cycle performance of capacitor is unstable.Therefore can be by preparing metal oxide and carbon composite, by the double-layer electric of carbon
The combination of the pseudo-capacitance of the metal oxide for holding and being filled in carbon pores gap, plays respective advantage, obtains high performance electrode
Material.
China is large agricultural country, the stalk such as the substantial amounts of paddy and wheat of annual output, corn, oil crop.According to investigations, China is every
Up to 800,000,000 tons or so of year stalk total amount, as stalk quantity is big, density is little, collecting and distributing accumulating is costly, economic worth is low, people
Mainly it is considered as waste to abandon or directly burn.Straw burning has not only had influence on daily life but also has caused pole
Big problem of environmental pollution, has become the public hazards of social concerns.Biomass contain a large amount of cellulose fibres, its be widely present and
It is renewable, select abandoned biomass not only reduce preparation cost problem as carbon source but also stalk can be solved processing difficult and resource wave
The problem taken.Therefore, research abandoned biomass is that carbon source has environmental protection and economic benefit double meaning.
The content of the invention
It is an object of the invention to provide a kind of preparation side of the metal oxide/carbon composite for ultracapacitor
Method.
The present invention technical solution be：A kind of method for preparing metal oxide/carbon composite, it is characterised in that
Comprise the steps：
1. by biomass washing, dry, crushing；Biomass after crushing are mixed into immersion with metal salt solution, is then centrifuged for true
Vacuum freecing-dry；Repeat 2-5 time, until dried biomass quality increases 0.1%-15%；
2. solid salt is put in crucible, and is continually fed into inert gas argon gas or nitrogen, being heated to 450 DEG C to 900 DEG C makes earthenware
Solid salt in crucible is melted；
1. 3. Jing the walked the biomass foam nickel coated of process, is immersed in the thawing solid salt in crucible, be incubated 0.25h
- 2h, is subsequently cooled to room temperature, product is taken out washing, centrifugation, vacuum freeze drying, metal oxide/carbon composite wood is obtained
Material.
The technical solution the of present invention biomass 1. described in step are that agro-ecology discarded object, industrial processes are discarded
One or more in biomass and forest abandoned biomass.
Agro-ecology discarded object described in the technical solution of the present invention is rice husk, peanut shell or stalk；Industry adds
Work abandoned biomass is bagasse, cocoanut shell, sesame-send cake or rape cake；Forest abandoned biomass is root, stem or the leaf of biomass.
Nitrate, sulphur of the technical solution the of the present invention metal salt solution 1. described in step for Co, Ni, Mn or Fe
The aqueous solution of one or more and/or alcoholic solution in hydrochlorate, chlorate or metallo-organic complex, its concentration are 0.3
3mol/L。
Alcoholic solution described in the technical solution of the present invention is methanol solution and/or ethanol solution.
Biomass of the technical solution the of the present invention 1. described in step mix immersion with metal salt solution, and its process is
Biomass after crushing are positioned in container, are vacuumized, it is 0.1-0.3Mpa to be depressurized to vacuum, adds metal salt solution,
Using the loose structure of biomass, solution is made to enter inside biomass along biomass itself duct, soak time is 15min-
180min；Repeat 2-5 time, until dried biomass quality increases 0.1%-15%.
The technical solution the of present invention solid salt 2. described in step is the one kind in NaCl, KCl, NaOH or KOH
Or various mixing.
The present invention soaks abandoned biomass by metal salt solution, allows slaine to enter biomass by biological itself duct
Inside, then again after freeze-drying, obtains this product by thermal cracking in molten salt at a certain temperature.The method is by by metal
Oxide and material with carbon element are compound, reach the requirement for improving electric conductivity and lifting specific capacity.
The present invention is had the advantage that compared with prior art：（1）The present invention is from abandoned biomass as carbon raw material, cost
Low and wide material sources；（2）At reduced pressure, biomass are soaked by metal salt solution, the hole of biomass itself can be utilized
Road is quickly entered inside biomass, is evenly distributed；（3）When cracking in fused salt, the structure that biomass energy keeps which special,
Slaine energy metal oxide particle formed in situ, such metal salt component are evenly distributed, and granularity is less, gives full play to
The synergy of carbon and metal oxide；（4）Can make the slaine in access aperture road will not be using Vacuum Freezing ＆ Drying Technology
The concentration aggregation of aperture end.
The technology of the present invention technological process is short, and equipment is simple, raw material sources extensively, low cost, prepared metal oxide/
In material with carbon element composite, metal oxide energy uniform load is on the carbon material.
Specific embodiment
Preparation method of the present invention is described further with reference to specific embodiment, but the protection of invention
Scope is not limited to this.
Embodiment 1：
10g stalks are washed, 150 m or so size particles is dry, pulverize into, is put in container with foam nickel coated, by container
It is 0.1Mpa to be evacuated down to vacuum, is rapidly added the 2mol/L Ni (NO of 500ml3)2Solution, keeps vacuum to be that 0.1Mpa is left
The right side, soak time are 30min, and after soaking, biomass take out drying, repeat immersion 1 time, biomass are taken out vacuum then
Freeze-drying, after weighing, quality is 11.24g.It is placed in reactor during crucible is put into after taking 480gNaCl, 20gNaOH mixing, holds
Continuous to be passed through inert gas argon gas, heating fused salt will be immersed in fused salt with the good biomass of foam nickel coated to 800 DEG C, is incubated
0.5h, product is taken out, and cooling, centrifugation, vacuum freeze drying obtain NiO/C composites.
Embodiment 2：
10g peanut shells are washed, 75 m or so size particles is dry, pulverize into, is put in container with foam nickel coated, will be held
It is 0.3Mpa that device is evacuated down to vacuum, is rapidly added the 0.4 mol/L MnSO of 500ml4Solution, keep vacuum be
0.3Mpa or so, soak time are 60min, and after soaking, biomass take out drying, repeat immersion 2 times, then by biomass
Vacuum freeze drying is taken out, quality is 10.58g after weighing.It is placed in during crucible is put into after taking 380g KCl, 120g KOH mixing anti-
In answering device, inert nitrogen gas are continually fed into, then heating fused salt cools to 700 DEG C to 800 DEG C, will be good with foam nickel coated
Biomass be immersed in fused salt, be incubated 2h, product is taken out, cool down, centrifugation, vacuum freeze drying, that is, obtain MnO/C be combined
Material.
Embodiment 3：
By 10g sesame-send cakes（Residue after oil expression）Washing, dry, pulverize into 40 m or so size particles, is put with foam nickel coated
Enter in container, be 0.2Mpa by container vacuum-pumping to vacuum, be rapidly added the 3 mol/L CoCl of 500ml2Ethanol solution, protects
It is 0.2Mpa or so to hold vacuum, and soak time is 90min, and after soaking, biomass take out drying, repeat immersion 1 time, take
Go out to be placed on low temperature on flat board drier and dry 60min, then by biomass vacuum freeze-drying, quality is 11.37g after weighing.Take
It is placed in reactor during crucible is put into after 240g KCl, 260g KOH mixing, is continually fed into inert gas argon gas, heating fused salt is extremely
800 DEG C, 570 DEG C are then cooled to, will be immersed in fused salt with the good biomass of foam nickel coated, be incubated 0.25h, product is taken
Go out, cool down, centrifugation, vacuum freeze drying obtain CoO/C composites.
Embodiment 4：
The 10g withered leaf of bamboo is washed, 50 m or so size particles is dry, pulverize into, is put in container with foam nickel coated, will be held
It is 0.1Mpa that device is evacuated down to vacuum, is rapidly added the 1 mol/L Fe (NO of 500ml3)3Solution, keep vacuum be
0.1Mpa or so, soak time are 160min, and after soaking, biomass take out drying, repeat immersion 4 times, then by biomass
Vacuum freeze drying, after weighing, quality is 10.96g.Reaction is placed in during crucible is put into after taking 245g NaCl, 255g NaOH mixing
In device, inert nitrogen gas are continually fed into, then heating fused salt cools to 470 DEG C to 820 DEG C, will be good with foam nickel coated
Biomass are immersed in fused salt, be incubated 1h, product is taken out, and are cooled down, and centrifugation, vacuum freeze drying obtain Fe2O3/ C is combined
Material.
Claims (7)
1. a kind of preparation method of metal oxide/carbon composite, it is characterised in that comprise the steps：
1. by biomass washing, dry, crushing；Biomass after crushing are mixed into immersion with metal salt solution, is then centrifuged for true
Vacuum freecing-dry；Repeat 2-5 time, until dried biomass quality increases 0.1%-15%；
2. solid salt is put in crucible, and is continually fed into inert gas argon gas or nitrogen, being heated to 450 DEG C to 900 DEG C makes earthenware
Solid salt in crucible is melted；
1. 3. Jing the walked the biomass foam nickel coated of process, is immersed in the thawing solid salt in crucible, be incubated 0.25h
- 2h, is subsequently cooled to room temperature, product is taken out washing, centrifugation, vacuum freeze drying, metal oxide/activated carbon is obtained multiple
Condensation material.
2. the preparation method of a kind of metal oxide/carbon composite according to claim 1, it is characterised in that：It is described
The biomass 1. described in step be agro-ecology discarded object, industrial processes abandoned biomass and forest abandoned biomass
One or more.
3. the preparation method of a kind of metal oxide/carbon composite according to claim 2, described agro-ecology are given up
Gurry is rice husk, peanut shell or stalk；Industrial processes abandoned biomass is bagasse, cocoanut shell, sesame-send cake or rape cake；Forest
Abandoned biomass is root, stem or the leaf of biomass.
4. the preparation method of a kind of metal oxide/carbon composite according to claim 1 and 2, it is characterised in that：The
1. during the metal salt solution described in step is nitrate, sulfate, chlorate or the metallo-organic complex of Co, Ni, Mn or Fe
The aqueous solution of one or more and/or alcoholic solution, its concentration be 0.3 3mol/L.
5. the preparation method of a kind of metal oxide/carbon composite according to claim 4, it is characterised in that：It is described
Alcoholic solution be methanol solution and/or ethanol solution.
6. the preparation method of a kind of metal oxide/carbon composite according to claim 1 and 2, it is characterised in that：The
1. the biomass described in step mix immersion with metal salt solution, and its process is that the biomass after crushing are positioned in container,
Vacuumize, it is 0.1-0.3Mpa to be depressurized to vacuum, adds metal salt solution, using the loose structure of biomass, makes solution suitable
Biomass itself duct to enter inside biomass；Soak time is 15min-180min；Repeat 2-5 time, until dried
Biomass quality increases 0.1%-15%.
7. the preparation method of a kind of metal oxide/carbon composite according to claim 1 and 2, it is characterised in that：The
2. the solid salt described in step is one or more mixing in NaCl, KCl, NaOH or KOH.
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| CN201611246093.1A CN106531476B (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of metal oxide/carbon composite |
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| CN201611246093.1A CN106531476B (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of metal oxide/carbon composite |
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| CN106531476B CN106531476B (en) | 2018-10-02 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107093529A (en) * | 2017-05-08 | 2017-08-25 | 华东理工大学 | A kind of method that utilization solar energy prepares transition metal oxide/carbon composite |
| CN109465001A (en) * | 2018-10-16 | 2019-03-15 | 江苏理工学院 | A kind of preparation method and application of carried metal carbon micron chip |
| CN110104630A (en) * | 2019-05-16 | 2019-08-09 | 华南师范大学 | A kind of porous carbon composite and its preparation method and application for battery diaphragm |
| CN110416516A (en) * | 2019-07-25 | 2019-11-05 | 东北大学 | A kind of preparation method of the anode material of lithium-ion battery of coal and manganese monoxide |
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| CN110624551A (en) * | 2019-10-10 | 2019-12-31 | 湖北文理学院 | Preparation method of lotus seedpod-based carbon-supported nickel catalyst |
| CN110624551B (en) * | 2019-10-10 | 2022-05-31 | 湖北文理学院 | Preparation method of lotus seedpod-based carbon-supported nickel catalyst |
| CN113249142A (en) * | 2021-05-21 | 2021-08-13 | 西北大学 | Preparation method of biomass charcoal-metal oxide composite electrode material |
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