CN108862276A - A kind of preparation method and product of lithium ion battery biomass carbon negative electrode material - Google Patents
A kind of preparation method and product of lithium ion battery biomass carbon negative electrode material Download PDFInfo
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- CN108862276A CN108862276A CN201810699912.0A CN201810699912A CN108862276A CN 108862276 A CN108862276 A CN 108862276A CN 201810699912 A CN201810699912 A CN 201810699912A CN 108862276 A CN108862276 A CN 108862276A
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- negative electrode
- lithium ion
- ion battery
- electrode material
- biomass carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- 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 discloses the preparation method and product of a kind of lithium ion battery biomass carbon negative electrode material, wherein method is using biomass green gram spermoderm as presoma, prepare the method with the lithium ion battery biomass carbon negative electrode material of layering aperture structure, it first uses green gram spermoderm that carbon matrix precursor is made, carbon matrix precursor is activated again to obtain activation presoma, activation presoma further activates up to target product.The present invention also provides lithium ion battery biomass carbon negative electrode materials made from the above method, and the negative electrode slurry comprising lithium ion battery biomass carbon negative electrode material obtained.Biomass carbon negative electrode material produced by the present invention, aperture structure is abundant, can be shortened lithium ion diffusion length, accelerates lithium ion diffusion rate, to improve capacity of lithium ion battery, high rate performance, cycle performance.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material and products, and in particular to a kind of lithium-ion electric
The preparation method and product of pond biomass carbon negative electrode material, belong to biomass carbon technical field.
Technical background
Due to economic fast development, demand of the people to the energy is also growing day by day, but withered with traditional fossil energy
It exhausts, it is extremely urgent to cause to develop a kind of new sustainable clean energy resource.Wherein lithium ion battery is exactly that a kind of good energy is close
One of degree height, energy of sustainable development.
Current commercialized lithium ion battery negative material is mainly graphite, and the source of graphite be mainly natural crystal,
Coal tar, it is all related with fossil energy.Additionally as lithium ion battery negative material, graphite is needed through broken, granulation, graphite
Change, sieve four big processes and many small processes, and is granulated and is graphitized and is required with high content of technology；The theoretical capacity of its schungite is low
Only 372mAh/g, poor circulation.Increasingly depleted with the energy, renewable resource is widely paid close attention to, wherein naturally
Biological material have many characteristics, such as it is from a wealth of sources, environmental-friendly, there is unique pattern and carbonaceous structure, before being a kind of good carbon
Drive body.Green gram spermoderm is as the waste in mung bean sprouts growth course, containing 60% or so cellulose, wherein cellulose carbon content
Up to 44.44%, oxygen content can provide more active site as carbon matrix precursor material up to 49.39%.In addition, green gram spermoderm is fine
The retention ability of dimension, expansive force hold that oily power is higher, and therefore, during carbonization-activation, green gram spermoderm is easy to be activated agent etching,
Form porous structure.
It is quite a few using biomass as the relevant report of raw material production biomass carbon material both at home and abroad：
CN108128773A discloses a kind of method for preparing electrode for electrochemical capacitor carbon material using peanut shell, adopts
The porous carbon materials made from hydro-thermal-fused salt combination technique.
CN108033447A discloses preparation method, multiporous biological matter carbon and the application of a kind of multiporous biological matter carbon, main
It is to prepare multiporous biological matter carbon by raw material of stalk.
CN107974672A fills the hole of porous plate using sugar juice, and the sugar in hole is obtained by the carbonization that heats up
Biomass carbon material.
CN107689445A is that material prepares multiporous biological matter carbon material using bracteal leaf of corn biomass.
But be showed no the relevant report that biomass carbon material is prepared using green gram spermoderm as raw material, the present invention is quasi- provide it is a kind of with
Biomass green gram spermoderm is biomass carbon lithium ion battery negative material and its preparation side that raw material preparation has layering aperture structure
Method.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation methods of lithium ion battery biomass carbon negative electrode material
And product, solve the defects of existing carbon material capacity is low, production technology is complicated, at high cost.
In order to solve the above-mentioned technical problem, the present invention uses following technical scheme：
A kind of preparation method of lithium ion battery biomass carbon negative electrode material is provided, before being specifically with biomass green gram spermoderm
Body is driven, the method with the lithium ion battery biomass carbon negative electrode material of layering aperture structure is prepared.
Further,
The above method specifically comprises the following steps：
S1, pretreatment of raw material
Green gram spermoderm is cleaned, dries simultaneously grind into powder；
S2, carbon matrix precursor is prepared
It is liquid phase using the resulting green gram spermoderm powder of step S1 as solid phase, deionized water, is mixed by liquid/solid ratio for 5~30
Merge 25~35min of stirring, be transferred to hydrothermal reaction kettle after mixing evenly and seal, hydrothermal temperature is 120~200 DEG C, water
It is heat-treated 3~8h, product is washed to neutral, drying with deionized water, obtains carbon matrix precursor by cooled to room temperature；
S3, preparation activation presoma
By the sylvite or sodium salt solution of carbon matrix precursor and 0.1~2mol/L obtained by step S2, by carbon matrix precursor：Potassium carbonate=
(0.1~5)：1 mass ratio is uniformly mixed, and drying to constant weight, obtains activation presoma；
S4, biomass carbon material is prepared
Activation presoma made from step S3 is put into tube furnace, is activated in 600~800 DEG C of inert atmosphere
1~3h to get.
Further,
It in step S3, is put into baking oven and dries, drying temperature is 80~120 DEG C.
Further,
Potassium salt soln in step S3 is K2CO3、KHCO3, KOH solution.
Further,
Sodium salt solution in step S3 is Na2CO3、NaHCO3, NaOH solution.
Further,
Inert atmosphere in step S4 is nitrogen atmosphere or argon atmosphere.
The present invention also provides lithium ion battery green gram spermoderm biomass carbon negative electrode materials made from above-mentioned preparation method.
The present invention also provides the cathode for including lithium ion battery green gram spermoderm biomass carbon negative electrode material made from the above method
Slurry.
It further, include above-mentioned lithium ion battery green gram spermoderm biomass carbon negative electrode material, conduction in the negative electrode slurry
Agent, binder, lithium ion battery green gram spermoderm biomass carbon negative electrode material：Conductive agent：The mass ratio of binder is (80~95):(3
~10):(2~10).
Beneficial effects of the present invention：
1, using green gram spermoderm as the biomass carbon negative electrode material of precursor preparation, aperture structure is abundant, can be shortened lithium ion
Diffusion length accelerates lithium ion diffusion rate, to improve capacity of lithium ion battery, high rate performance, cycle performance.
2, using green bio matter as carbon source abundance, environmental-friendly, simple process is easily-controllable, be suitble to large-scale production.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1~4 are respectively 1~4 green gram spermoderm based biomass carbon SEM of embodiment of the present invention figure；
Fig. 5 is 1 green gram spermoderm based biomass carbon cycle performance map of the embodiment of the present invention.
Specific embodiment
In order to preferably illustrate the content of the invention, below by specific embodiment to further verifying of the invention.It is special
Illustrate herein, embodiment is only that more directly description is of the invention, they are a part of the invention, cannot be to structure of the present invention
At any restrictions.
Embodiment 1
S1, green gram spermoderm is carried out to clean clear water, drying and grind into powder；
S2, using green gram spermoderm powder obtained by step S1 as solid phase, water be liquid phase, be 10 by liquid/solid ratio, by green gram spermoderm powder with
Water is stirred 30min, is transferred to hydrothermal reaction kettle after mixing evenly, hydrothermal temperature is 200 DEG C, hydro-thermal process 3h, natural
It is cooled to room temperature, product is washed to neutral, drying with deionized water, obtains carbon matrix precursor.
S3, by the potassium carbonate of carbon matrix precursor and 0.5mol/L obtained by step S2, by presoma：The mass ratio of potassium carbonate=2
It is uniformly mixed, is put into 100 DEG C of baking ovens that drying to constant weight, obtain activation presoma.
S4, activation presoma is put into high temperature furnace, is activated 1h in 800 DEG C of nitrogen atmosphere, prepares layering
The lithium ion battery biomass carbon negative electrode material of aperture structure, is denoted as number D1.
Embodiment 2
S1, green gram spermoderm is carried out to clean clear water, drying and grind into powder；
S2, by solid phase, water of green gram spermoderm powder it is liquid phase, is 20 by liquid/solid ratio, green gram spermoderm powder and water are stirred
30min is transferred to hydrothermal reaction kettle after mixing evenly, and hydrothermal temperature is 120 DEG C, hydro-thermal process 8h, cooled to room temperature,
Product is washed to neutral, drying with deionized water, obtains carbon matrix precursor；
S3, by the saleratus (KHCO of carbon matrix precursor and 1mol/L3), by presoma：The mass ratio of saleratus=0.5
It is uniformly mixed, is put into 90 DEG C of baking ovens that drying to constant weight, obtain activation presoma；
S4, activation presoma is put into high temperature furnace, is activated 1h in 700 DEG C of nitrogen atmosphere, prepares layering
The lithium ion battery biomass carbon negative electrode material of aperture structure, is denoted as number D2.
Embodiment 3
S1, green gram spermoderm is carried out to clean clear water, drying and grind into powder；
S2, by solid phase, water of green gram spermoderm powder it is liquid phase, is 30 by liquid/solid ratio, green gram spermoderm powder and water are stirred
25min is transferred to hydrothermal reaction kettle after mixing evenly, and hydrothermal temperature is 150 DEG C, hydro-thermal process 5h, cooled to room temperature,
Product is washed to neutral, drying with deionized water, obtains carbon matrix precursor；
S3, by the potassium hydroxide of carbon matrix precursor and 0.1mol/L, by presoma：The mass ratio mixing of potassium hydroxide=5 is equal
It is even, it is put into 120 DEG C of baking ovens that drying to constant weight, obtains activation presoma；
S4, activation presoma is put into high temperature furnace, is activated 2h in 600 DEG C of nitrogen atmosphere, prepares layering
The lithium ion battery biomass carbon negative electrode material of aperture structure, is denoted as number D3.
Embodiment 4
S1, green gram spermoderm is carried out to clean clear water, drying and grind into powder；
S2, by solid phase, water of green gram spermoderm powder it is liquid phase, is 5 by liquid/solid ratio, green gram spermoderm powder and water are stirred
35min is transferred to hydrothermal reaction kettle after mixing evenly, and hydrothermal temperature is 150 DEG C, hydro-thermal process 5h, cooled to room temperature,
Product is washed to neutral, drying with deionized water, obtains carbon matrix precursor；
S3, by the sodium carbonate of carbon matrix precursor and 1.0mol/L, by presoma：The mass ratio of sodium carbonate=3 is uniformly mixed, and is put
Enter in 120 DEG C of baking ovens that drying to constant weight, obtains activation presoma；
S4, activation presoma is put into high temperature furnace, is activated 2h in 650 DEG C of nitrogen atmosphere, prepares layering
The lithium ion battery biomass carbon negative electrode material of aperture structure, is denoted as number D4.
By the lithium ion battery biomass carbon negative electrode material scanning electron microscopy of number D1-D4 made from above-described embodiment
Mirror tests it, and the SEM photograph difference of sample D1-D4 is as shown in figures 1-4.From Fig. 1~4 as can be seen that according to this hair
The hole of biomass carbon negative electrode material made from bright method is very rich.
By the lithium ion battery biomass carbon negative electrode material of number D1-D4 prepared in the above embodiments, conductive agent, binder
95 are pressed respectively:3:2；80:10:10；80:10:10；95:3:2 mass ratio prepares lithium ion battery anode slurry, is coated in 8
On μm copper foil, electrode slice is made as working electrode, it is electrolyte that lithium metal, which is to electrode, 1M LiFP6, is assembled into battery, is remembered
For battery number DC1-DC4, cycle life survey is carried out under the conditions of current density is 100mAh/g, voltage window is -3.0~0V
Examination, test result is as follows table 1：
The cycle performance Comparative result of 1 sample DC1-DC4 of table
Fig. 5 furthermore presents the performance curve of battery DC1 made of D1 sample made from embodiment, can from figure
Out：Its first discharge specific capacity is 1058mAh/g, and much larger than the theoretical value 372mAh/g of graphite, after 100 weeks, capacity is circulation
747mAh/g, conservation rate 70.6%.
It is above-mentioned the experimental results showed that：A green gram spermoderm is lithium ion battery biomass carbon made from raw material by the method for the invention
Negative electrode material cycle performance is good, and carbon material stable structure has wide practical use.
The above is a specific embodiment of the invention, but any restrictions cannot be constituted to the present invention, therefore need special
It points out, it is all based on the present invention, it is made any modification and is all fallen within the scope of the present invention with improvement.
Claims (8)
1. a kind of preparation method of lithium ion battery biomass carbon negative electrode material, which is characterized in that be specifically with biomass mung bean
Skin is presoma, prepares the method with the lithium ion battery biomass carbon negative electrode material of layering aperture structure.
2. a kind of preparation method of lithium ion battery biomass carbon negative electrode material according to claim 1, which is characterized in that
The above method specifically comprises the following steps：
S1, pretreatment of raw material
Green gram spermoderm is cleaned, dries simultaneously grind into powder；
S2, carbon matrix precursor is prepared
It is liquid phase using the resulting green gram spermoderm powder of step S1 as solid phase, deionized water, is mixed simultaneously by liquid/solid ratio for 5~30
25~35min is stirred, hydrothermal reaction kettle is transferred to after mixing evenly and seals, hydrothermal temperature is 120~200 DEG C, at hydro-thermal
3~8h is managed, product is washed to neutral, drying with deionized water, obtains carbon matrix precursor by cooled to room temperature；
S3, preparation activation presoma
By the sylvite or sodium salt solution of carbon matrix precursor and 0.1~2mol/L obtained by step S2, by carbon matrix precursor：Potassium carbonate=(0.1
~5)：1 mass ratio is uniformly mixed, and drying to constant weight, obtains activation presoma；
S4, biomass carbon material is prepared
By made from step S3 activation presoma be put into tube furnace, in 600~800 DEG C of inert atmosphere be activated 1~
3h to get.
3. a kind of preparation method of lithium ion battery biomass carbon negative electrode material according to claim 1 or 2, feature exist
In,
It in step S3, is put into baking oven and dries, drying temperature is 80~120 DEG C.
4. a kind of preparation method of lithium ion battery biomass carbon negative electrode material according to claim 2, which is characterized in that
Potassium salt soln in step S3 is K2CO3、KHCO3, KOH solution.
5. a kind of preparation method of lithium ion battery biomass carbon negative electrode material according to claim 2, which is characterized in that
Sodium salt solution in step S3 is Na2CO3、NaHCO3, NaOH solution.
6. a kind of preparation method of lithium ion battery biomass carbon negative electrode material according to claim 2, which is characterized in that
Inert atmosphere in step S4 is nitrogen atmosphere or argon atmosphere.
7. using lithium ion battery green gram spermoderm biomass carbon negative electrode material made from preparation method as claimed in claim 1 or 2.
8. including the negative of lithium ion battery green gram spermoderm biomass carbon negative electrode material made from preparation method as claimed in claim 1 or 2
Pole slurry, which is characterized in that
In the negative electrode slurry include above-mentioned lithium ion battery green gram spermoderm biomass carbon negative electrode material, conductive agent, binder, lithium from
Sub- battery green gram spermoderm biomass carbon negative electrode material：Conductive agent：The mass ratio of binder is (80~95):(3~10):(2~10).
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Cited By (4)
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| CN109742384A (en) * | 2019-01-07 | 2019-05-10 | 中国矿业大学 | A kind of biomass porous carbon is used as the method for kalium ion battery cathode |
| CN112735857A (en) * | 2020-12-22 | 2021-04-30 | 上海卓笙环保科技有限公司 | Method for constructing composite material based on bean sprouts |
| CN113861946A (en) * | 2021-11-03 | 2021-12-31 | 东南大学 | Lotus root stalk biomass porous carbon composite phase change material and preparation method thereof |
| CN114620722A (en) * | 2022-03-17 | 2022-06-14 | 青岛华世洁环保科技有限公司 | Porous carbon negative electrode material, preparation method thereof, electrode, battery and capacitor prepared from porous carbon negative electrode material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109742384A (en) * | 2019-01-07 | 2019-05-10 | 中国矿业大学 | A kind of biomass porous carbon is used as the method for kalium ion battery cathode |
| CN112735857A (en) * | 2020-12-22 | 2021-04-30 | 上海卓笙环保科技有限公司 | Method for constructing composite material based on bean sprouts |
| CN113861946A (en) * | 2021-11-03 | 2021-12-31 | 东南大学 | Lotus root stalk biomass porous carbon composite phase change material and preparation method thereof |
| CN114620722A (en) * | 2022-03-17 | 2022-06-14 | 青岛华世洁环保科技有限公司 | Porous carbon negative electrode material, preparation method thereof, electrode, battery and capacitor prepared from porous carbon negative electrode material |
| CN114620722B (en) * | 2022-03-17 | 2023-09-19 | 青岛华世洁环保科技有限公司 | Porous carbon negative electrode material, preparation method thereof, electrode, battery and capacitor prepared from porous carbon negative electrode material |
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Application publication date: 20181123 |