CN105036108B - A kind of method that utilization maize leaves prepare sodium-ion battery electrode material with carbon element - Google Patents
A kind of method that utilization maize leaves prepare sodium-ion battery electrode material with carbon element Download PDFInfo
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- CN105036108B CN105036108B CN201510346139.6A CN201510346139A CN105036108B CN 105036108 B CN105036108 B CN 105036108B CN 201510346139 A CN201510346139 A CN 201510346139A CN 105036108 B CN105036108 B CN 105036108B
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- 240000008042 Zea mays Species 0.000 title claims abstract description 53
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 53
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 title claims abstract description 49
- 235000009973 maize Nutrition 0.000 title claims abstract description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 26
- 239000007772 electrode material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 44
- 238000010792 warming Methods 0.000 claims abstract description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007654 immersion Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims abstract description 7
- 238000001914 filtration 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 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000002033 PVDF binder Substances 0.000 description 4
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 4
- 235000005822 corn Nutrition 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- 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 3
- 239000006230 acetylene black Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000005518 electrochemistry Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000010977 jade Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-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
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 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 present invention relates to a kind of method that utilization maize leaves prepare sodium-ion battery electrode material with carbon element, it comprises the following steps：（a）Maize leaves are cut into small pieces, and ultrasonically treated, filtration is carried out in immersion alcohol, is dry for the first time；（b）Dried maize leaves will immerse in salpeter solution for the first time, and heat 1 ~ 5 hour at 50 ~ 100 DEG C, filter, dry for second；（c）Second dried maize leaves is placed in inert gas atmosphere, is warming up to 500 ~ 1100 DEG C and calcines 0.5 ~ 5 hour, grind into powder after cooling；（d）The powder is scattered in the concentrated sulfuric acid, potassium permanganate is added, carry out the reaction of low-temperature oxidation reaction, middle temperature oxidation reaction and high-temperature oxydation successively, subsequently it is added thereto to hydrogen peroxide solution to release to stirring nothing gas, suction filtration, washing, taking filter cake carries out drying for the third time.The space so enabled in sulfuric acid and potassium permanganate infiltration maize leaves is fully oxidized, and sloughs sulfur-containing group therein.
Description
Technical field
The invention belongs to battery electrode material field, is related to a kind of sodium-ion battery electrode material with carbon element, and in particular to a kind of
The method for sodium-ion battery electrode material with carbon element being prepared using maize leaves.
Background technology
Corn, original name：Maize, another name：Maize, big sorgo etc..The whole world torrid zone and Temperate Region in China are extensively planted, and are one
Important cereal.Corn is to be distributed one of widest cereal crops in the world, and cultivated area is only second to wheat and paddy rice and occupies
Three.Planting range is from 58 ° of north latitude（Canadian and Russian）To 40 ° of south latitude（South America）, the whole year, there was jade every month in the world
Rice is ripe, therefore, has a large amount of maize leaves to produce, but people are only limitted to the aspects such as dietotherapy, fuel to the application of maize leaves, rarely
Application in terms of electrochemistry.
With electric automobile, the extensive application of intelligent electronic device, the demand of lithium will be greatly increased, and the reserves of lithium have
Limit, and skewness, so as to raise the price with lithium associated materials, increase battery cost, meanwhile, lithium ion battery is also present
The problems such as security, cycle life, this restrict the development of lithium.Therefore, the energy storage of development excellent combination property of future generation is needed badly
Battery system.Sodium and lithium belong to same main group in the periodic table of elements, with similar physicochemical properties, and sodium aboundresources,
With low cost, it is the battery system for having very much development potentiality, receives the extensive concern of domestic and international researcher in recent years.If
Can will can substantially reduce the preparation cost of Graphene using discarded object maize leaves preparing Graphene, so as to be conducive to sodium from
The popularization of sub- battery.
Content of the invention
The invention aims to overcoming the deficiencies in the prior art and providing one kind and prepare sodium-ion battery using maize leaves
The method of electrode material with carbon element.
For reaching above-mentioned purpose, the technical solution used in the present invention is：One kind prepares sodium-ion battery electricity using maize leaves
The method of pole material with carbon element, it comprises the following steps：
（a）Maize leaves are cut into small pieces, and ultrasonically treated, filtration is carried out in immersion alcohol, is dry for the first time；
（b）Dried maize leaves will immerse in salpeter solution for the first time, and heat 1 ~ 5 hour at 50 ~ 100 DEG C, filter, the
Redrying；
（c）Second dried maize leaves is placed in inert gas atmosphere, is warming up to 500 ~ 1100 DEG C of calcinings 0.5 ~ 5
Hour, grind into powder after cooling；
（d）The powder is scattered in the concentrated sulfuric acid, potassium permanganate is added, carries out low-temperature oxidation reaction, middle temperature oxygen successively
Change and react and high-temperature oxydation reaction, hydrogen peroxide solution is subsequently added thereto to stirring nothing gas releasing, suction filtration, washing, takes filter
Cake carries out third time and dries；The low-temperature oxidation reaction is reacted 15 ~ 40 minutes at 0 ~ 4 DEG C for elder generation, then is warming up to 5 ~ 9 DEG C instead
Answer 1 ~ 3 hour, be then warming up to 10 ~ 14 DEG C and react 1 ~ 3 hour, be then warming up to 15 ~ 19 DEG C and react 1 ~ 3 hour, then heat up
React 1 ~ 3 hour to 20 ~ 30 DEG C；The middle temperature oxidation reaction is to react 15 ~ 60 minutes at 35 ~ 50 DEG C；The high-temperature oxydation is anti-
Should be and react 15 ~ 60 minutes at 80 ~ 100 DEG C after being added thereto to deionized water.
Optimally, step（b）In, the concentration of the salpeter solution is 1 ~ 5mol/L.
Optimally, step（c）In, the programming rate is 10 ~ 15 DEG C/min.
Further, step（c）In, when calcining heat is more than 900 DEG C, second dried maize leaves is existed respectively
400 DEG C, 700 DEG C, 900 DEG C of holdings be warming up to maximum temperature again within 1 ~ 2 hour.
Optimally, step（d）In, the concentrated sulfuric acid mass fraction is 95 ~ 98%, the powder, the concentrated sulfuric acid and described
The ratio of potassium permanganate is 5 ~ 10g：100~150ml：10 ~ 20g, in the hydrogen peroxide solution volume fraction of hydrogen peroxide be 1 ~
5%, the concentrated sulfuric acid is 5 ~ 10 with the volume ratio of the deionized water：1.
As technique scheme is used, the present invention has following advantages compared with prior art：The present invention utilizes corn
The method that leaf prepares sodium-ion battery electrode material with carbon element, is on the one hand carried out ultrasonically treated with alcohol, and is carried out using salpeter solution
Soak, the impurity such as the agricultural chemicals of residual, dust in maize leaves can be so removed, and which can be pre-oxidized；On the other hand
Powder after calcining is carried out low-temperature oxidation reaction, middle temperature oxidation reaction and high-temperature oxydation reaction successively, so enables to sulphur
The space that acid and potassium permanganate are penetrated in maize leaves is fully oxidized, and sloughs sulfur-containing group therein.
Description of the drawings
Accompanying drawing 1 is the scanning electron microscope (SEM) photograph of sodium-ion battery electrode material with carbon element obtained in embodiment 1；
Accompanying drawing 2 is the electricity that obtained sodium-ion battery electrode material with carbon element is measured after being assembled into sodium-ion battery in embodiment 1
Chemical property figure；
Accompanying drawing 3 is the electricity that obtained sodium-ion battery electrode material with carbon element is measured after being assembled into sodium-ion battery in embodiment 2
Chemical property figure；
Accompanying drawing 4 is the electricity that obtained sodium-ion battery electrode material with carbon element is measured after being assembled into sodium-ion battery in embodiment 3
Chemical property figure.
Specific embodiment
The method that the present invention prepares sodium-ion battery electrode material with carbon element using maize leaves, it comprises the following steps：（a）By jade
Meter Ye is cut into small pieces, and carries out ultrasonically treated, filtration, dry in immersion alcohol for the first time；（b）By dried for first time maize leaves
In immersion salpeter solution, heat 1 ~ 5 hour at 50 ~ 100 DEG C, filter, dry for second；（c）Will second dried corn
Leaf is placed in inert gas atmosphere, is warming up to 500 ~ 1100 DEG C and is calcined 0.5 ~ 5 hour, grind into powder after cooling；（d）Will be described
Powder is scattered in the concentrated sulfuric acid, is added potassium permanganate, is carried out low-temperature oxidation reaction, middle temperature oxidation reaction and high-temperature oxydation successively anti-
Answering, hydrogen peroxide solution being subsequently added thereto to stirring nothing gas releasing, suction filtration, washing, taking filter cake carries out drying for the third time i.e.
Can；The low-temperature oxidation reaction is reacted 15 ~ 40 minutes at 0 ~ 4 DEG C for elder generation, then is warming up to 5 ~ 9 DEG C of reactions 1 ~ 3 hour, then heats up
React 1 ~ 3 hour to 10 ~ 14 DEG C, be then warming up to 15 ~ 19 DEG C and react 1 ~ 3 hour, be then warming up to 20 ~ 30 DEG C of reactions 1 ~ 3 little
When；The middle temperature oxidation reaction is to react 15 ~ 60 minutes at 35 ~ 50 DEG C；High-temperature oxydation reaction for be added thereto to from
React 15 ~ 60 minutes at 80 ~ 100 DEG C after sub- water.On the one hand carried out with alcohol ultrasonically treated, and soaked using salpeter solution
Bubble, can so remove the impurity such as the agricultural chemicals of residual, dust in maize leaves, and which can be pre-oxidized；On the other hand will
Powder after calcining carries out the reaction of low-temperature oxidation reaction, middle temperature oxidation reaction and high-temperature oxydation successively, so enables to sulfuric acid
Fully oxidized with the space in potassium permanganate infiltration maize leaves, and slough sulfur-containing group therein.
Step（b）In, the concentration of the salpeter solution is preferably 1 ~ 5mol/L.Step（c）In, the programming rate is preferred
For 10 ~ 15 DEG C/min；When calcining heat is more than 900 DEG C, will second dried maize leaves respectively 400 DEG C, 700 DEG C,
900 DEG C of holdings are warming up to maximum temperature in 1 ~ 2 hour again, partly in order to the moisture in maize leaves is thoroughly removed, on the other hand
Be in order to by thorough for maize leaves carbonization.Step（d）In, the concentrated sulfuric acid mass fraction is preferably 95 ~ 98%, the powder, described
The ratio of the concentrated sulfuric acid and the potassium permanganate is preferably 5 ~ 10g：100~150ml：10 ~ 20g, hydrogen peroxide in the hydrogen peroxide solution
Volume fraction be preferably 1 ~ 5%, the volume ratio of the concentrated sulfuric acid and the deionized water is preferably 5 ~ 10：1, so as to further
Improve obtained material with carbon element quality.
The present invention is further described below in conjunction with accompanying drawing embodiment.
Embodiment 1
The present embodiment provides a kind of method that utilization maize leaves prepare sodium-ion battery electrode material with carbon element, and it includes following step
Suddenly：
（a）Maize leaves are cut into small pieces, and ultrasonically treated, filtration is carried out in immersion alcohol, is dry for the first time；
（b）By in the salpeter solution of dried maize leaves immersion 1mol/L for the first time, heat 5 hours at 50 DEG C, filter,
Dry for second；
（c）Second dried maize leaves is placed in inert gas atmosphere, is warming up to 10 DEG C/min of speed
500 DEG C are calcined 5 hours, grind into powder after cooling；
（d）5g powder is scattered in the 100ml concentrated sulfuric acid（The conventional concentrated sulfuric acid, sulfuric acid mass fraction are 95 ~ 98%）In, plus
Enter 10g potassium permanganate, carry out the reaction of low-temperature oxidation reaction, middle temperature oxidation reaction and high-temperature oxydation successively, be subsequently added thereto to
Volume fraction is that 1% hydrogen peroxide solution is released to stirring nothing gas, suction filtration, washing, and taking filter cake carries out drying for the third time,
Its scanning electron microscope (SEM) photograph is as shown in Figure 1；The low-temperature oxidation reaction is reacted 40 minutes at 0 DEG C for elder generation, then it is little to be warming up to 5 DEG C of reactions 3
When, then it is warming up to 10 DEG C and reacts 3 hours, be then warming up to 15 DEG C and react 3 hours, is then warming up to 20 DEG C and reacts 3 hours；Institute
It is to react 60 minutes at 35 DEG C to state middle temperature oxidation reaction；The high-temperature oxydation reaction is for being added thereto to after 20ml deionized water
80 DEG C are reacted 60 minutes.Subsequently by the material with carbon element for obtaining and acetylene black, PVDF（Kynoar）In mass ratio 7:2:1 mixing is all
Even, electrode is prepared into according to prior art and assembles sodium-ion battery, test its chemical property, as shown in Figure 2.
Embodiment 2
The present embodiment provides a kind of method that utilization maize leaves prepare sodium-ion battery electrode material with carbon element, and it includes following step
Suddenly：
（a）Maize leaves are cut into small pieces, and ultrasonically treated, filtration is carried out in immersion alcohol, is dry for the first time；
（b）Dried maize leaves will immerse in 5mol/L salpeter solution for the first time, and heat 1 hour at 100 DEG C, filter,
Dry for second；
（c）Second dried maize leaves is placed in inert gas atmosphere, is warming up to 15 DEG C/min of speed
1100 DEG C are calcined 0.5 hour（Wherein, need to be risen after 400 DEG C, 700 DEG C, 900 DEG C are kept for 1 ~ 2 hour respectively again in temperature-rise period
Temperature is calcined 0.5 hour to 1100 DEG C）, grind into powder after cooling；
（d）10g powder is scattered in the 150ml concentrated sulfuric acid, add 20g potassium permanganate, carry out successively low-temperature oxidation reaction,
Middle temperature oxidation reaction and high-temperature oxydation reaction, are subsequently added thereto to the hydrogen peroxide solution that volume fraction is 5% and extremely stir nothing gas
Release, suction filtration, washing, taking filter cake carries out drying for the third time；The low-temperature oxidation reaction is reacted 15 minutes at 4 DEG C for elder generation,
It is warming up to 9 DEG C again to react 1 hour, is then warming up to 14 DEG C and reacts 1 hour, is then warming up to 19 DEG C and reacts 1 hour, then heat up
React 1 hour to 30 DEG C；The middle temperature oxidation reaction is to react 15 minutes at 50 DEG C；The high-temperature oxydation reaction is for adding thereto
React 15 minutes at 100 DEG C after entering 15ml ionized water.Subsequently by the material with carbon element for obtaining and acetylene black, PVDF（Kynoar）
In mass ratio 7:2:1 mixes, and is prepared into electrode according to prior art and assembles sodium-ion battery, tests its electrochemistry
Can, as shown in Figure 3.
Embodiment 3
The present embodiment provides a kind of method that utilization maize leaves prepare sodium-ion battery electrode material with carbon element, and it includes following step
Suddenly：
（a）Maize leaves are cut into small pieces, and ultrasonically treated, filtration is carried out in immersion alcohol, is dry for the first time；
（b）Dried maize leaves will immerse in 1.5mol/L salpeter solution for the first time, and heat 4 hours at 75 DEG C, filter,
Dry for second；
（c）Second dried maize leaves is placed in inert gas atmosphere, is warming up to 12 DEG C/min of speed
1000 DEG C are calcined 0.5 hour（Wherein, need to be risen after 400 DEG C, 700 DEG C, 900 DEG C are kept for 1 ~ 2 hour respectively again in temperature-rise period
Temperature is calcined 0.5 hour to 1000 DEG C）, grind into powder after cooling；
（d）The powder is scattered in the 120ml concentrated sulfuric acid, 15g potassium permanganate is added, carries out low-temperature oxidation successively anti-
Answer, middle temperature oxidation reaction and high-temperature oxydation are reacted, volume fraction is subsequently added thereto to for 3% hydrogen peroxide solution to stirring nothing gas
Body is released, suction filtration, washing, and taking filter cake carries out drying for the third time；The low-temperature oxidation reaction reacts 20 points for elder generation at 2 DEG C
Clock, then 8 DEG C of reactions 2 hours are warming up to, then it is warming up to 12 DEG C and reacts 2 hours, 16 DEG C of reactions 2 hours is then warming up to, then
It is warming up to 25 DEG C to react 2 hours；The middle temperature oxidation reaction is to react 20 minutes at 40 DEG C；High-temperature oxydation reaction be to which
React 30 minutes at 90 DEG C after middle addition 16ml deionized water.Subsequently by the material with carbon element for obtaining and acetylene black, PVDF（Polyvinylidene fluoride
Alkene）In mass ratio 7:2:1 mixes, and is prepared into electrode according to prior art and assembles sodium-ion battery, tests its electrochemistry
Performance, as shown in figure 4, its chemical property is optimum.
Above-described embodiment technology design only to illustrate the invention and feature, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implement according to this, can not be limited the scope of the invention with this, all according to the present invention
Equivalence changes or modification that Spirit Essence is made, should all be included within the scope of the present invention.
Claims (5)
1. a kind of method that utilization maize leaves prepare sodium-ion battery electrode material with carbon element, it is characterised in that it comprises the following steps：
（a）Maize leaves are cut into small pieces, and ultrasonically treated, filtration is carried out in immersion alcohol, is dry for the first time；
（b）Dried maize leaves will immerse in salpeter solution for the first time, and heat 1 ~ 5 hour at 50 ~ 100 DEG C, filter, second
Dry；
（c）Second dried maize leaves is placed in inert gas atmosphere, is warming up to 500 ~ 1100 DEG C of calcinings 0.5 ~ 5 little
When, grind into powder after cooling；
（d）The powder is scattered in the concentrated sulfuric acid, potassium permanganate is added, carry out low-temperature oxidation reaction, the oxidation of middle temperature successively instead
Should react with high-temperature oxydation, hydrogen peroxide solution is subsequently added thereto to stirring nothing gas releasing, suction filtration, washing, takes filter cake and enter
Row third time dries；Low-temperature oxidation reaction is reacted 15 ~ 40 minutes at 0 ~ 4 DEG C for elder generation, then be warming up to 5 ~ 9 DEG C of reactions 1 ~
3 hours, then it is warming up to 10 ~ 14 DEG C and reacts 1 ~ 3 hour, is then warming up to 15 ~ 19 DEG C and reacts 1 ~ 3 hour, then it is warming up to 20 ~
30 DEG C are reacted 1 ~ 3 hour；The middle temperature oxidation reaction is to react 15 ~ 60 minutes at 35 ~ 50 DEG C；High-temperature oxydation reaction be to
React 15 ~ 60 minutes at 80 ~ 100 DEG C after wherein adding deionized water.
2. the method for preparing sodium-ion battery electrode material with carbon element using maize leaves according to claim 1, it is characterised in that：Step
Suddenly（b）In, the concentration of the salpeter solution is 1 ~ 5mol/L.
3. the method for preparing sodium-ion battery electrode material with carbon element using maize leaves according to claim 1, it is characterised in that：Step
Suddenly（c）In, the programming rate is 10 ~ 15 DEG C/min.
4. the method for preparing sodium-ion battery electrode material with carbon element using maize leaves according to claim 3, it is characterised in that：Step
Suddenly（c）In, when calcining heat is more than 900 DEG C, second dried maize leaves is protected in 400 DEG C, 700 DEG C, 900 DEG C respectively
Hold 1 ~ 2 hour and be warming up to maximum temperature again.
5. the method for preparing sodium-ion battery electrode material with carbon element using maize leaves according to claim 1, it is characterised in that：Step
Suddenly（d）In, the concentrated sulfuric acid mass fraction is 95 ~ 98%, and the ratio of the powder, the concentrated sulfuric acid and the potassium permanganate is 5
~10g：100~150ml：10 ~ 20g, in the hydrogen peroxide solution volume fraction of hydrogen peroxide be 1 ~ 5%, the concentrated sulfuric acid with described
The volume ratio of 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 |
| 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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| CN103382028A (en) * | 2013-08-17 | 2013-11-06 | 青岛中科昊泰新材料科技有限公司 | Preparation of graphene oxide and post-processing method for waste liquor |
| CN104051160A (en) * | 2014-05-30 | 2014-09-17 | 大英聚能科技发展有限公司 | Graphene for electrical double-layer capacitor and preparation method thereof |
| CN104016341A (en) * | 2014-07-01 | 2014-09-03 | 济南圣泉集团股份有限公司 | Preparation method of porous graphene |
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