CN105036108A - Method for preparing sodium-ion battery electrode carbon material from corn leaves - Google Patents
Method for preparing sodium-ion battery electrode carbon material from corn leaves Download PDFInfo
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- CN105036108A CN105036108A CN201510346139.6A CN201510346139A CN105036108A CN 105036108 A CN105036108 A CN 105036108A CN 201510346139 A CN201510346139 A CN 201510346139A CN 105036108 A CN105036108 A CN 105036108A
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- Prior art keywords
- semen maydis
- leaf
- hour
- ion battery
- warming
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- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 25
- 240000008042 Zea mays Species 0.000 title abstract description 12
- 235000002017 Zea mays subsp mays Nutrition 0.000 title abstract description 11
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title abstract description 10
- 235000005822 corn Nutrition 0.000 title abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000012065 filter cake Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 44
- 210000000582 semen Anatomy 0.000 claims description 44
- 238000010792 warming Methods 0.000 claims description 35
- 230000001590 oxidative effect Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000012423 maintenance Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 239000012466 permeate Substances 0.000 abstract 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 239000006230 acetylene black Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 235000007244 Zea mays Nutrition 0.000 description 1
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 235000009973 maize Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a method for preparing sodium-ion battery electrode carbon material from corn leaves. The method comprises the following steps: (a) cutting the corn leaves into chips, immersing the chips into alcohol for ultra-sounding treatment, filtering, and carrying out primary drying; (b) immersing the primarily dried corn leaf chips into a nitric acid solution, heating at 50 to 100CDEG C for 1 to 5 hours, filtering, and carrying out secondary drying; (c) placing the secondarily dried corn leaf chips at an inert gas atmosphere, heating to 500 to 1100 DEG C, carrying out calcination for 0.5 to 5 hours, cooling down, and grinding the cooled chips into powder; (d) dispersing the powder in a concentrated sulfuric acid solution, adding potassium permanganate, carrying out a low-temperature oxidation reaction, a moderate-temperature oxidation reaction and a high-temperature oxidation reaction in sequence, adding a hydrogen peroxide solution, stirring till no gas can be emitted, carrying out suction filtration and washing, taking filter cake, and conducting tertiary drying on the filter cake. According to the method, sulfuric acid and potassium permanganate can permeate gaps in the corn leaves for sufficient oxidization, and sulfur-containing groups in the corn leaves are removed.
Description
Technical field
The invention belongs to battery electrode material field, relate to a kind of sodium-ion battery electrode carbon material, be specifically related to a kind of method utilizing leaf of Semen Maydis to prepare sodium-ion battery electrode carbon material.
Background technology
Corn, original name: Zea mays, another name: maize, large sorgo etc.The torrid zone, the whole world and Temperate Region in China are extensively planted, and are an important cereal.Corn is one of the food crop the most widely that distribute in the world, and cultivated area is only second to wheat and paddy rice and occupies the 3rd.Planting range is from north latitude 58 ° (Canada and Russia) to 40 °, south latitude (South America), there is every month in the whole year corn ripe in the world, therefore, have a large amount of leaf of Semen Maydis to produce, but the application of people to leaf of Semen Maydis is only limitted to the aspect such as dietotherapy, fuel, the application rarely in electrochemistry.
Along with the widespread use of electromobile, intelligent electronic device, the demand of lithium will increase greatly, and the reserves of lithium are limited, and skewness, thus raised the price with lithium associated materials, increase battery cost, simultaneously, also there is the problem such as security, cycle life in lithium ion battery, this restrict the development of lithium.Therefore, the energy-storage battery system developing excellent combination property of future generation is needed badly.Sodium and lithium belong to same main group in the periodic table of elements, have similar physicochemical property, and sodium aboundresources, with low cost, be the battery system having very much development potentiality, receive the extensive concern of domestic and international researchist in recent years.If waste leaf of Semen Maydis can be utilized to prepare Graphene, greatly can reduce the preparation cost of Graphene, thus be conducive to the popularization of sodium-ion battery.
Summary of the invention
The present invention seeks to provide a kind of method utilizing leaf of Semen Maydis to prepare sodium-ion battery electrode carbon material to overcome the deficiencies in the prior art.
For achieving the above object, the technical solution used in the present invention is: a kind of method utilizing leaf of Semen Maydis to prepare sodium-ion battery electrode carbon material, and it comprises the following steps:
A leaf of Semen Maydis is cut into small pieces by (), immerse in alcohol and carry out supersound process, filters, and first time is dry;
B dried for first time leaf of Semen Maydis immerses in salpeter solution by (), 50 ~ 100 DEG C of heating 1 ~ 5 hour, filter, second time is dry;
C the dried leaf of Semen Maydis of second time is placed in inert gas atmosphere by (), be warming up to 500 ~ 1100 DEG C of calcinings 0.5 ~ 5 hour, grind into powder after cooling;
D described powder dispersion in the vitriol oil, is added potassium permanganate by (), carry out low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction successively, release without gas to stirring subsequently to wherein adding hydrogen peroxide solution, suction filtration, washing, gets filter cake and carries out third time drying; Described low-temperature oxidation reaction for first reacting 15 ~ 40 minutes at 0 ~ 4 DEG C, then is warming up to 5 ~ 9 DEG C of reactions 1 ~ 3 hour, is then warming up to 10 ~ 14 DEG C of reactions 1 ~ 3 hour, is then warming up to 15 ~ 19 DEG C of reactions 1 ~ 3 hour, is then warming up to 20 ~ 30 DEG C of reactions 1 ~ 3 hour; Described middle temperature oxidizing reaction is 35 ~ 50 DEG C of reactions 15 ~ 60 minutes; Described high temperature oxidation reaction is reacted 15 ~ 60 minutes at 80 ~ 100 DEG C after adding deionized water wherein.
Optimally, in step (b), the concentration of described salpeter solution is 1 ~ 5mol/L.
Optimally, in step (c), described heat-up rate is 10 ~ 15 DEG C/min.
Further, in step (c), when calcining temperature is greater than 900 DEG C, the dried leaf of Semen Maydis of second time is warming up to top temperature in 1 ~ 2 hour again 400 DEG C, 700 DEG C, 900 DEG C maintenances respectively.
Optimally, in step (d), described vitriol oil massfraction is 95 ~ 98%, the ratio of described powder, the described vitriol oil and described potassium permanganate is 5 ~ 10g:100 ~ 150ml:10 ~ 20g, in described hydrogen peroxide solution, the volume fraction of hydrogen peroxide is 1 ~ 5%, and the volume ratio of the described vitriol oil and described deionized water is 5 ~ 10:1.
Because technique scheme is used, the present invention compared with prior art has following advantages: the present invention utilizes leaf of Semen Maydis to prepare the method for sodium-ion battery electrode carbon material, one side alcohol carries out supersound process, and use salpeter solution to soak, the impurity such as agricultural chemicals, dust residual in leaf of Semen Maydis can be removed like this, and preoxidation can be carried out to it; Powder after calcining is carried out successively low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction on the other hand, the space that sulfuric acid and potassium permanganate can be made like this to infiltrate in leaf of Semen Maydis is fully oxidized, and sloughs sulfur-containing group wherein.
Accompanying drawing explanation
Accompanying drawing 1 is the scanning electron microscope (SEM) photograph of the sodium-ion battery electrode carbon material that embodiment 1 obtains;
Accompanying drawing 2 is the chemical property figure recorded after sodium-ion battery electrode carbon material obtained in embodiment 1 is assembled into sodium-ion battery;
Accompanying drawing 3 is the chemical property figure recorded after sodium-ion battery electrode carbon material obtained in embodiment 2 is assembled into sodium-ion battery;
Accompanying drawing 4 is the chemical property figure recorded after sodium-ion battery electrode carbon material obtained in embodiment 3 is assembled into sodium-ion battery.
Embodiment
The present invention utilizes leaf of Semen Maydis to prepare the method for sodium-ion battery electrode carbon material, and it comprises the following steps: leaf of Semen Maydis is cut into small pieces by (a), immerses in alcohol and carries out supersound process, filters, and first time is dry; B dried for first time leaf of Semen Maydis immerses in salpeter solution by (), 50 ~ 100 DEG C of heating 1 ~ 5 hour, filter, second time is dry; C the dried leaf of Semen Maydis of second time is placed in inert gas atmosphere by (), be warming up to 500 ~ 1100 DEG C of calcinings 0.5 ~ 5 hour, grind into powder after cooling; D described powder dispersion in the vitriol oil, is added potassium permanganate by (), carry out low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction successively, release without gas to stirring subsequently to wherein adding hydrogen peroxide solution, suction filtration, washing, gets filter cake and carries out third time drying; Described low-temperature oxidation reaction for first reacting 15 ~ 40 minutes at 0 ~ 4 DEG C, then is warming up to 5 ~ 9 DEG C of reactions 1 ~ 3 hour, is then warming up to 10 ~ 14 DEG C of reactions 1 ~ 3 hour, is then warming up to 15 ~ 19 DEG C of reactions 1 ~ 3 hour, is then warming up to 20 ~ 30 DEG C of reactions 1 ~ 3 hour; Described middle temperature oxidizing reaction is 35 ~ 50 DEG C of reactions 15 ~ 60 minutes; Described high temperature oxidation reaction is reacted 15 ~ 60 minutes at 80 ~ 100 DEG C after adding deionized water wherein.One side alcohol carries out supersound process, and uses salpeter solution to soak, and can remove the impurity such as agricultural chemicals, dust residual in leaf of Semen Maydis like this, and can carry out preoxidation to it; Powder after calcining is carried out successively low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction on the other hand, the space that sulfuric acid and potassium permanganate can be made like this to infiltrate in leaf of Semen Maydis is fully oxidized, and sloughs sulfur-containing group wherein.
In step (b), the concentration of described salpeter solution is preferably 1 ~ 5mol/L.In step (c), described heat-up rate is preferably 10 ~ 15 DEG C/min; When calcining temperature is greater than 900 DEG C, the dried leaf of Semen Maydis of second time is warming up to top temperature for 1 ~ 2 hour again 400 DEG C, 700 DEG C, 900 DEG C maintenances respectively, being on the one hand the moisture in order to thoroughly remove in leaf of Semen Maydis, is in order to by thorough for leaf of Semen Maydis carbonization on the other hand.In step (d), described vitriol oil massfraction is preferably 95 ~ 98%, the ratio of described powder, the described vitriol oil and described potassium permanganate is preferably 5 ~ 10g:100 ~ 150ml:10 ~ 20g, in described hydrogen peroxide solution, the volume fraction of hydrogen peroxide is preferably 1 ~ 5%, the volume ratio of the described vitriol oil and described deionized water is preferably 5 ~ 10:1, thus improves obtained carbon material quality further.
Below in conjunction with accompanying drawing embodiment, the present invention is further described.
Embodiment 1
The present embodiment provides a kind of method utilizing leaf of Semen Maydis to prepare sodium-ion battery electrode carbon material, and it comprises the following steps:
A leaf of Semen Maydis is cut into small pieces by (), immerse in alcohol and carry out supersound process, filters, and first time is dry;
B dried for first time leaf of Semen Maydis immerses in the salpeter solution of 1mol/L by (), 50 DEG C of heating 5 hours, filter, second time is dry;
C the dried leaf of Semen Maydis of second time is placed in inert gas atmosphere by (), be warming up to 500 DEG C of calcinings 5 hours, grind into powder after cooling with the speed of 10 DEG C/min;
(d) by 5g powder dispersion in the 100ml vitriol oil (the conventional vitriol oil, sulfuric acid massfraction is 95 ~ 98%) in, add 10g potassium permanganate, carry out low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction successively, subsequently to wherein add volume fraction be 1% hydrogen peroxide solution to stir without gas release, suction filtration, wash, get filter cake and carry out third time drying, its scanning electron microscope (SEM) photograph as shown in Figure 1; Described low-temperature oxidation reaction for first reacting 40 minutes at 0 DEG C, then is warming up to 5 DEG C of reactions 3 hours, is then warming up to 10 DEG C of reactions 3 hours, is then warming up to 15 DEG C of reactions 3 hours, is then warming up to 20 DEG C of reactions 3 hours; Described middle temperature oxidizing reaction is 35 DEG C of reactions 60 minutes; Described high temperature oxidation reaction is reacted 60 minutes at 80 DEG C after adding 20ml deionized water wherein.Subsequently by the carbon material obtained and acetylene black, PVDF(polyvinylidene difluoride (PVDF)) in mass ratio 7:2:1 mix, be conventionally prepared into electrode and assemble sodium-ion battery, testing its chemical property, as shown in Figure 2.
Embodiment 2
The present embodiment provides a kind of method utilizing leaf of Semen Maydis to prepare sodium-ion battery electrode carbon material, and it comprises the following steps:
A leaf of Semen Maydis is cut into small pieces by (), immerse in alcohol and carry out supersound process, filters, and first time is dry;
B dried for first time leaf of Semen Maydis immerses in 5mol/L salpeter solution by (), 100 DEG C of heating 1 hour, filter, second time is dry;
C the dried leaf of Semen Maydis of second time is placed in inert gas atmosphere by (), be warming up to 1100 DEG C with the speed of 15 DEG C/min and calcine 0.5 hour (wherein, 1100 DEG C are warming up to again after needing to keep 1 ~ 2 hour respectively at 400 DEG C, 700 DEG C, 900 DEG C in temperature-rise period, calcine 0.5 hour), grind into powder after cooling;
(d) by 10g powder dispersion in the 150ml vitriol oil, add 20g potassium permanganate, carry out low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction successively, subsequently to wherein add volume fraction be 5% hydrogen peroxide solution to stir release without gas, suction filtration, washing, gets filter cake and carries out third time drying; Described low-temperature oxidation reaction for first reacting 15 minutes at 4 DEG C, then is warming up to 9 DEG C of reactions 1 hour, is then warming up to 14 DEG C of reactions 1 hour, is then warming up to 19 DEG C of reactions 1 hour, is then warming up to 30 DEG C of reactions 1 hour; Described middle temperature oxidizing reaction is 50 DEG C of reactions 15 minutes; Described high temperature oxidation reaction is reacted 15 minutes at 100 DEG C after adding 15ml ionized water wherein.Subsequently by the carbon material obtained and acetylene black, PVDF(polyvinylidene difluoride (PVDF)) in mass ratio 7:2:1 mix, be conventionally prepared into electrode and assemble sodium-ion battery, testing its chemical property, as shown in Figure 3.
Embodiment 3
The present embodiment provides a kind of method utilizing leaf of Semen Maydis to prepare sodium-ion battery electrode carbon material, and it comprises the following steps:
A leaf of Semen Maydis is cut into small pieces by (), immerse in alcohol and carry out supersound process, filters, and first time is dry;
B dried for first time leaf of Semen Maydis immerses in 1.5mol/L salpeter solution by (), 75 DEG C of heating 4 hours, filter, second time is dry;
C the dried leaf of Semen Maydis of second time is placed in inert gas atmosphere by (), be warming up to 1000 DEG C with the speed of 12 DEG C/min and calcine 0.5 hour (wherein, 1000 DEG C are warming up to again after needing to keep 1 ~ 2 hour respectively at 400 DEG C, 700 DEG C, 900 DEG C in temperature-rise period, calcine 0.5 hour), grind into powder after cooling;
(d) by described powder dispersion in the 120ml vitriol oil, add 15g potassium permanganate, carry out low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction successively, release without gas to stirring subsequently to wherein to add volume fraction be 3% hydrogen peroxide solution, suction filtration, washing, gets filter cake and carries out third time drying; Described low-temperature oxidation reaction for first reacting 20 minutes at 2 DEG C, then is warming up to 8 DEG C of reactions 2 hours, is then warming up to 12 DEG C of reactions 2 hours, is then warming up to 16 DEG C of reactions 2 hours, is then warming up to 25 DEG C of reactions 2 hours; Described middle temperature oxidizing reaction is 40 DEG C of reactions 20 minutes; Described high temperature oxidation reaction is reacted 30 minutes at 90 DEG C after adding 16ml deionized water wherein.Subsequently by the carbon material obtained and acetylene black, PVDF(polyvinylidene difluoride (PVDF)) in mass ratio 7:2:1 mix, be conventionally prepared into electrode and assemble sodium-ion battery, testing its chemical property, as shown in Figure 4, its chemical property is optimum.
Above-described embodiment is only for illustrating technical conceive of the present invention and feature; its object is to person skilled in the art can be understood content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. utilize leaf of Semen Maydis to prepare a method for sodium-ion battery electrode carbon material, it is characterized in that, it comprises the following steps:
A leaf of Semen Maydis is cut into small pieces by (), immerse in alcohol and carry out supersound process, filters, and first time is dry;
B dried for first time leaf of Semen Maydis immerses in salpeter solution by (), 50 ~ 100 DEG C of heating 1 ~ 5 hour, filter, second time is dry;
C the dried leaf of Semen Maydis of second time is placed in inert gas atmosphere by (), be warming up to 500 ~ 1100 DEG C of calcinings 0.5 ~ 5 hour, grind into powder after cooling;
D described powder dispersion in the vitriol oil, is added potassium permanganate by (), carry out low-temperature oxidation reaction, middle temperature oxidizing reaction and high temperature oxidation reaction successively, release without gas to stirring subsequently to wherein adding hydrogen peroxide solution, suction filtration, washing, gets filter cake and carries out third time drying; Described low-temperature oxidation reaction for first reacting 15 ~ 40 minutes at 0 ~ 4 DEG C, then is warming up to 5 ~ 9 DEG C of reactions 1 ~ 3 hour, is then warming up to 10 ~ 14 DEG C of reactions 1 ~ 3 hour, is then warming up to 15 ~ 19 DEG C of reactions 1 ~ 3 hour, is then warming up to 20 ~ 30 DEG C of reactions 1 ~ 3 hour; Described middle temperature oxidizing reaction is 35 ~ 50 DEG C of reactions 15 ~ 60 minutes; Described high temperature oxidation reaction is reacted 15 ~ 60 minutes at 80 ~ 100 DEG C after adding deionized water wherein.
2. utilize leaf of Semen Maydis to prepare the method for sodium-ion battery electrode carbon material according to claim 1, it is characterized in that: in step (b), the concentration of described salpeter solution is 1 ~ 5mol/L.
3. utilize leaf of Semen Maydis to prepare the method for sodium-ion battery electrode carbon material according to claim 1, it is characterized in that: in step (c), described heat-up rate is 10 ~ 15 DEG C/min.
4. utilize leaf of Semen Maydis to prepare the method for sodium-ion battery electrode carbon material according to claim 3, it is characterized in that: in step (c), when calcining temperature is greater than 900 DEG C, the dried leaf of Semen Maydis of second time is warming up to top temperature in 1 ~ 2 hour again 400 DEG C, 700 DEG C, 900 DEG C maintenances respectively.
5. utilize leaf of Semen Maydis to prepare the method for sodium-ion battery electrode carbon material according to claim 1, it is characterized in that: in step (d), described vitriol oil massfraction is 95 ~ 98%, the ratio of described powder, the described vitriol oil and described potassium permanganate is 5 ~ 10g:100 ~ 150ml:10 ~ 20g, in described hydrogen peroxide solution, the volume fraction of hydrogen peroxide is 1 ~ 5%, and the volume ratio of the described vitriol oil and described deionized water is 5 ~ 10:1.
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| CN110719891A (en) * | 2018-11-23 | 2020-01-21 | 辽宁星空钠电电池有限公司 | Biomass-based hard carbon negative electrode material of sodium ion battery and preparation method and application thereof |
| CN110571432A (en) * | 2019-08-15 | 2019-12-13 | 合肥国轩高科动力能源有限公司 | element-doped biomass hard carbon negative electrode material for sodium ion battery, preparation method and sodium ion battery |
| CN113511654A (en) * | 2021-04-16 | 2021-10-19 | 中国科学院山西煤炭化学研究所 | Capacitance carbon and preparation method thereof |
| CN113511654B (en) * | 2021-04-16 | 2022-11-15 | 中国科学院山西煤炭化学研究所 | Capacitance carbon and preparation method thereof |
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