CN109888181A - A kind of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material and preparation method thereof and anode plate for lithium ionic cell and lithium ion battery - Google Patents
A kind of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material and preparation method thereof and anode plate for lithium ionic cell and lithium ion battery Download PDFInfo
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- CN109888181A CN109888181A CN201910160616.8A CN201910160616A CN109888181A CN 109888181 A CN109888181 A CN 109888181A CN 201910160616 A CN201910160616 A CN 201910160616A CN 109888181 A CN109888181 A CN 109888181A
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- 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 discloses a kind of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material and preparation method thereof and anode plate for lithium ionic cell and lithium ion battery, halogenated choline type eutectic solvent is obtained mixing with lignocellulosic after eutectic solvent in proportion after evenly mixing, first pre-processed, then high temperature cabonization obtains the carbon material of doping nitrogen elemental lithium, can be applied to lithium ion battery negative material.Presoma employed in the present invention is that halogenated lithium is uniformly mixed with halogenated choline and its derivative, and presoma is environmentally protective, from a wealth of sources, cheap, can be obtained from industrial high-volume；The preparation process that the method for the present invention uses is succinct, and yield is high, and purity is good；Reaction system ingredient involved in the method for the present invention is simple, and configuration is convenient, easy to operate, low for equipment requirements and without geographical restrictions, is suitble to large-scale industrial production.
Description
Technical field
The invention belongs to material and technical field of chemical power, and in particular to a kind of carbon nitrogen lithium multiphase doped lithium ion battery
Negative electrode material and preparation method thereof and anode plate for lithium ionic cell and lithium ion battery.
Background technique
With the fast development of chemical cell with rapid changepl. never-ending changes and improvements, to battery material, there has also been increasingly higher demands.It is adjoint
The rapid advances of anode material for lithium-ion batteries, cell negative electrode material is also had higher requirement.Quotient on Vehicles Collected from Market
The most important negative electrode material of industryization is worked as and belongs to carbon material, such as graphite, hard carbon, carbonaceous mesophase spherules.But the theory of carbon material
Specific capacity only has 372mAh/g, at the same time since the carbon material in first time charge and discharge process and carbonate electrolyte generate admittedly
State electrolyte interface film (SEI), further limits the promotion of lithium battery capacity.
In carbon material, in order to meet requirement of the power battery for high magnification, high capacity, high circulation, hard carbon becomes
Newest focus.Different from other carbon materials, hard carbon specific capacity with higher, good cycle performance, high rate capability, system
The advantages that standby of less demanding, low in cost.
Traditional hard carbon material preparation method is complex, needs to carry out hard carbon pattern improvement, such as pore-creating, modification change
Property processing.Simultaneously as hard carbon is formed by polymer carbonization, most polymer has safety issue.Therefore, from production work
From the aspect of skill control and energy conservation and environmental protection, seek the simple and easy to do controllable synthetic method of one kind to prepare lithium ion batteries anodes
Material is of great significance.
Summary of the invention
The present invention, which is put into, has been designed to provide a kind of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material and its preparation
Method and anode plate for lithium ionic cell and lithium ion battery, this method precursors are from a wealth of sources to be easy to get, and reaction condition is simple
Controllably, simple to operation.
The technical scheme adopted by the invention is as follows:
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, the preparation method includes following step
It is rapid:
(1) by halogenated choline and halogenated lithium salts, heating stirring obtains eutectic solvent；
(2) lignocellulosic and step (1) are obtained into eutectic solvent heating stirring, obtained mixture by carbonization,
Carbon nitrogen lithium multiphase, which is obtained, after cleaning filtering, ball milling sieving adulterates miscellaneous lithium ion battery negative material.
In step (1), the halogenated choline is choline chloride or derivatives thereof, choline bromide or derivatives thereof, iodate gallbladder
Any one or more in alkali or derivatives thereof；The halogenated lithium salts is lithium chloride, lithium bromide, any one in lithium iodide
Or it is a variety of.
In step (1), the molar ratio of the halogenated choline and halogenated lithium salts is 1~3:2~8.
In step (1) and step (2), what the heating stirring referred to is in 60~100 DEG C of 1~4h of stirring.
In step (2), the mass ratio of the lignocellulosic and eutectic solvent is 1~2:1~5.
In step (2), the method for the carbonization are as follows:
Mixture is first warming up to 250~400 DEG C by (2-1) in air atmosphere, 2~4h is kept the temperature, so that in mixture
Moisture slow evaporation；
(2-2) carbon gasification is warming up to 600~1200 DEG C then under argon stream in order to prevent, keeps the temperature 2~4h.
Further, in step (2-1), the rate of the heating is 1~5 DEG C/min；
In step (2-2), the rate of the heating is 1~5 DEG C/min.
The present invention controls the heating rate of carbonation stage in 1~5 DEG C/min, and partial size can be obtained in this way at 5~10 μm
And the product of even size distribution；If the too fast meeting of heating rate influences the partial size of product so that halogenated choline fast decoupled
And the uniformity.
In step (2), cleaning filtering refers to through dehydrated alcohol, with standing, separation, suction filtration one or more of methods one
Secondary or multiple cleaning filter process.
In step (2), in the ball mill with 500~1000r/min, 4~6h of ball milling, then the ball milling sieving refers to
It is screened with 180~400 mesh screens.
Further, the preparation method of the carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material specifically includes following step
It is rapid:
1) 1~3:2~8 weigh halogenated choline and halogenated lithium salts in molar ratio, with 60~100 in constant temperature blender with magnetic force
DEG C stirring 1~4h, obtain eutectic solvent；
2) 1~2:1~5 weigh lignocellulosic and eutectic solvent in mass ratio, with 60 in constant temperature blender with magnetic force
~100 DEG C of 1~4h of stirring, obtain mixture；
3) mixture obtained by step 2) is first warming up to 250 in air atmosphere with the heating rate of 1~5 DEG C/min~
400 DEG C, keep the temperature 2~4h；Then under Ar air-flow, 600~1200 DEG C are warming up to the heating rate of 5 DEG C/min, heat preservation 2~
4h obtains carbide；
4) gained carbide is repeatedly filtered afterwards with washes of absolute alcohol；Then in the ball mill with 500~1000r/min
4~6h of ball milling adulterates miscellaneous lithium ion battery negative material with carbon nitrogen lithium multiphase is obtained after the screening of 180~400 mesh screens.
The present invention also provides a kind of anode plate for lithium ionic cell, the carbon nitrogen being prepared with the preparation method in the present invention
Lithium multiphase doped lithium ion battery negative electrode material is prepared for active material.
The present invention also provides a kind of lithium ion batteries, are assembled using the anode plate for lithium ionic cell as cathode.
In technical solution provided by the invention, it is molten that eutectic is mixed to form with halogenated choline and the heating of halogenated lithium salts first
Agent, lignocellulosic is not soluble in water, but can be swollen in eutectic solvent, forms homogeneous mixture, then will mixing
Object carries out high temperature cabonization, and during high temperature cabonization, the flue gas of choline carbonization, to generate corrosion pore-creating effect, is mentioned in alkalinity
Rise the specific surface area and storage lithium performance of biomass carbon cathode；The doping of lithium salts simultaneously is played in battery charge and discharge process and mends lithium
Effect promotes the formation of solid electrolyte interface film (SEI), greatly improves coulombic efficiency for the first time and cycle performance.
In preparation method disclosed by the invention, the raw material environmental protection of use is easy to get, the uniqueness that halogenated choline has, Ke Yifen
Staple in bulk element, while the important function of carbon source, nitrogen source and corrosive agent is had concurrently, it can be achieved that producing to carbonization during high temperature cabonization
The controllable preparation of object pattern and pore structure；The reaction system ingredient that the method for the present invention is related to is simple, and reaction condition is controllable, prepares work
Skill is simple and easy, has the advantages that environmental protection, low for equipment requirements and without geographical restrictions, is suitble to large-scale industrial production.
Compared with prior art, advantages of the present invention is specific as follows:
First, the hydroxyl of nitrogen-atoms and cellulose on oxygen atom and amino on carboxyl in eutectic solvent forms
New hydrogen bond destroys the crystal structure of cellulose, the dissolution of accelerating fibers element；
Second, unique lithium doping can reduce solid electrolyte interface film (SEI) formation in first time charge and discharge process
And in cyclic process in electrolyte irreversible lithium ion loss, significantly increase for the first time coulombic efficiency and circulation the longevity
Life；
Third, nitrogen doped can change the lattice structure of carbon in choline, operating voltage is reduced to increase full electricity
The voltage window in pond；
Fourth, choline, during high temperature cabonization, the flue gas of choline carbonization can generate corrosion pore-creating in alkalinity to carbon material
Effect, to promote the specific surface area and storage lithium performance of Carbon anode；
Fifth, due to using cellulose dissolution eutectic solvent mixture direct carbonization, being avoided usually in carbonisation
Reactant mixes non-uniform phenomenon in presoma in carbonisation, to promote carbonization efficiency and homogeneity, is suitable for industry
Metaplasia produces.
Detailed description of the invention
Fig. 1 is the SEM figure of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material prepared by the embodiment of the present invention 3.
Specific embodiment
The following describes the present invention in detail with reference to examples.
It is involved in the present invention to each raw material directly can commercially obtain.
Embodiment 1
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, comprising the following steps:
1) 1:5 weighs choline chloride 13.96g and lithium chloride 21.20g in molar ratio, with 70 in constant temperature blender with magnetic force
DEG C stirring 2h, obtain eutectic solvent；
2) 1:2 in mass ratio weighs lignocellulosic 17.28g and eutectic solvent 34.56g, in constant temperature blender with magnetic force
In with 100 DEG C of stirring 2h, obtain mixture；
3) 2) gained mixture is first warming up to 300 DEG C in air atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h；
Then under Ar air-flow, 800 DEG C is warming up to the heating rate of 5 DEG C/min, 2h is kept the temperature, obtains carbide.
4) gained carbide is filtered with after washes of absolute alcohol 3 times；Then in the ball mill with 600r/min ball milling 4h,
With carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material is obtained after the screening of 200 mesh screens, SEM schemes as shown in Figure 1, from figure
The particle diameter distribution of hard carbon obtained by it can be seen that is at 8~9 μm, and the uniformity is higher.
Embodiment 2
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, comprising the following steps:
1) 2:5 weighs choline chloride 27.92g and lithium chloride 21.20g in molar ratio, with 70 in constant temperature blender with magnetic force
DEG C stirring 2h, obtain eutectic solvent；
2) 1:2 in mass ratio weighs lignocellulosic 17.28g and eutectic solvent 34.56g, in constant temperature blender with magnetic force
In with 100 DEG C of stirring 2h, obtain mixture；
3) 2) gained mixture is first warming up to 300 DEG C in air atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h；
Then under Ar air-flow, 800 DEG C is warming up to the heating rate of 5 DEG C/min, 2h is kept the temperature, obtains carbide.
Gained carbide is filtered with after washes of absolute alcohol 3 times；Then it is used in the ball mill with 600r/min ball milling 4h
Carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material is obtained after the screening of 200 mesh screens.
Embodiment 3
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, comprising the following steps:
1) 1:5 weighs choline chloride 13.96g and lithium chloride 21.20g in molar ratio, with 90 in constant temperature blender with magnetic force
DEG C stirring 2h, obtain eutectic solvent；
2) 1:3 in mass ratio weighs lignocellulosic 11.72g and eutectic solvent 35.16g, in constant temperature blender with magnetic force
In with 80 DEG C of stirring 2h, obtain mixture；
3) 2) gained mixture is first warming up to 300 DEG C in air atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h；
Then under Ar air-flow, 800 DEG C is warming up to the heating rate of 5 DEG C/min, 4h is kept the temperature, obtains carbide.
4) gained carbide is filtered with after washes of absolute alcohol 3 times；Then in the ball mill with 600r/min ball milling 4h,
With carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material is obtained after the screening of 300 mesh screens, SEM schemes as shown in Fig. 2, from figure
It can be seen that the particle diameter distribution of gained hard carbon material at 6~7 μm, illustrate compared to Figure 1 generation product the uniformity is higher, partial size
It is smaller, increase specific surface area so that for the first time coulombic efficiency decrease but high rate performance it is more preferable.
Embodiment 4
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, comprising the following steps:
1) 1:5 weighs choline chloride 13.96g and lithium chloride 21.20g in molar ratio, with 70 in constant temperature blender with magnetic force
DEG C stirring 2h, obtain eutectic solvent；
2) 1:2 in mass ratio weighs lignocellulosic 17.28g and eutectic solvent 34.56g, in constant temperature blender with magnetic force
In with 100 DEG C of stirring 2h, obtain mixture；
3) 2) gained mixture is first warming up to 300 DEG C in air atmosphere with the heating rate of 5 DEG C/min, keeps the temperature 2h；
Then under Ar air-flow, 1000 DEG C is warming up to the heating rate of 5 DEG C/min, 2h is kept the temperature, obtains carbide.
4) gained carbide is filtered with after washes of absolute alcohol 3 times；Then in the ball mill with 600r/min ball milling 4h,
Carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material is obtained after being screened with 200 mesh screens.
Embodiment 5
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, comprising the following steps:
1) 1:5 weighs choline chloride 13.96g and lithium chloride 21.20g in molar ratio, with 70 in constant temperature blender with magnetic force
DEG C stirring 2h, obtain eutectic solvent；
2) 2:5 in mass ratio weighs lignocellulosic 14.06g and eutectic solvent 35.15g, in constant temperature blender with magnetic force
In with 70 DEG C of stirring 2h, obtain mixture；
3) 2) gained mixture is first warming up to 300 DEG C in air atmosphere with the heating rate of 1 DEG C/min, keeps the temperature 2h；
Then under Ar air-flow, 1000 DEG C is warming up to the heating rate of 1 DEG C/min, 2h is kept the temperature, obtains carbide；
4) gained carbide is filtered with after washes of absolute alcohol 3 times；Then in the ball mill with 600r/min ball milling 4h,
Carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material is obtained after being screened with 200 mesh screens.
Comparative example 1
A kind of preparation method of lithium ion battery negative material, comprising the following steps:
1) lignocellulosic 17.28g is weighed, is warming up to 300 DEG C in air atmosphere with the heating rate of 5 DEG C/min, is protected
Warm 2h is warming up to 800 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 2h, obtain carbide then under Ar air-flow；
2) gained carbide is filtered with after washes of absolute alcohol 3 times；Then in the ball mill with 600r/min ball milling 4h,
Lithium ion battery negative material is obtained after being screened with 200 mesh screens.
Comparative example 2
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, other are with embodiment 1, only step
3) in, it is that mixture obtained by step 2) is first warming up to 300 DEG C in air atmosphere with the heating rate of 8 DEG C/min, keeps the temperature 2h；
Then under Ar air-flow, 800 DEG C is warming up to the heating rate of 8 DEG C/min, 2h is kept the temperature, obtains carbide.
Comparative example 3
A kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, other are with embodiment 1, only step
It 3) is to be warming up to 800 DEG C by mixture obtained by step 2) and then under Ar air-flow with the heating rate of 8 DEG C/min, heat preservation in
3h obtains carbide.
It is poly- inclined using negative electrode material made from embodiment 1-5 and comparative example 1-3 as electrode active material and adhesive
Difluoroethylene (PVDF) and the black mass ratio by 80:5:15 of conductive acetylene mix, and 1-Methyl-2-Pyrrolidone is added
(NMP) it is stirred into slurry, is coated uniformly on copper foil surface, pole piece is then dried into 12h at 80C.By electrode slice through roller
Be placed in vacuum drying oven again after press compacting in the dry 8h of 90C, cutting be made lithium ion battery negative electrode tab I, II, III, IV, V,
VI、Ⅶ、Ⅷ。
Manufactured electrode slice is assembled into lithium ion half-cell and carries out performance detection, metal Li piece is as nitrating battery cathode
Material to electrode.Electrolyte is LiPF containing 1mol/L6DEC (diethyl carbonate)+EC (ethylene carbonate) (volume ratio
DEC:EC=7:3), diaphragm polypropylene Celgard2300.Battery assembling process is lower than 1% drying gloves in relative humidity
It is completed in case.
The battery assembled carries out constant current charge-discharge test after placing 12h, and charging/discharging voltage is 0.1V~3.0V, 25
DEG C, carry out constant current charge-discharge loop test in 2 DEG C of environment at 50mA/g and 100mA/g respectively and (rate of charge and corresponding put
Electric multiplying power is identical), the reversible capacity and charge-discharge performance of nitrating cell negative electrode material negative electrode of lithium ion battery are measured, is obtained
The test result of nitrating cell negative electrode material is as shown in table 1.
Table 1
Above-mentioned reference embodiment is to a kind of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material and preparation method thereof and lithium
The detailed description that ion battery negative electrode tab and lithium ion battery carry out, is illustrative without being restrictive, can be according to being limited
Determine range and enumerate several embodiments, therefore the change and modification in the case where not departing from present general inventive concept, the present invention should be belonged to
Protection scope within.
Claims (10)
1. a kind of preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material, which is characterized in that the preparation method
The following steps are included:
(1) by halogenated choline and halogenated lithium salts, heating stirring obtains eutectic solvent；
(2) lignocellulosic and step (1) are obtained into eutectic solvent heating stirring, obtained mixture is by carbonization, cleaning
Carbon nitrogen lithium multiphase, which is obtained, after filtering, ball milling sieving adulterates miscellaneous lithium ion battery negative material.
2. the preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material according to claim 1, feature exist
In, in step (1), the halogenated choline be choline chloride or derivatives thereof, choline bromide or derivatives thereof, choline iodide or its
Any one or more in derivative；The halogenated lithium salts be lithium chloride, lithium bromide, in lithium iodide any one or it is more
Kind.
3. the preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material according to claim 1 or 2, feature
It is, in step (1), the molar ratio of the halogenated choline and halogenated lithium salts is 1~3:2~8.
4. the preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material according to claim 1 or 2, feature
It is, in step (1) and step (2), what the heating stirring referred to is in 60~100 DEG C of 1~4h of stirring.
5. the preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material according to claim 1, feature exist
In in step (2), the mass ratio of the lignocellulosic and eutectic solvent is 1~2:1~5.
6. the preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material according to claim 1, feature exist
In, in step (2), the method for the carbonization are as follows:
Mixture is first warming up to 250~400 DEG C by (2-1) in air atmosphere, keeps the temperature 2~4h；
(2-2) then under argon stream, is warming up to 600~1200 DEG C, keeps the temperature 2~4h.
7. the preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material according to claim 6, feature exist
In in step (2-1), the rate of the heating is 1~5 DEG C/min；In step (2-2), the rate of the heating is 1~5 DEG C/
min。
8. the preparation method of carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material according to claim 1, feature exist
In in step (2), the ball milling sieving refers in the ball mill with 500~1000r/min, 4~6h of ball milling, then with 180
The screening of~400 mesh screens.
9. a kind of anode plate for lithium ionic cell, which is characterized in that be prepared into preparation method described in claim 1-8 any one
To carbon nitrogen lithium multiphase doped lithium ion battery negative electrode material be prepared for active material.
10. a kind of lithium ion battery, which is characterized in that assembled by cathode of anode plate for lithium ionic cell as claimed in claim 9
It forms.
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| CN114604850A (en) * | 2022-03-30 | 2022-06-10 | 广东邦普循环科技有限公司 | Preparation method and application of porous microsphere carbon negative electrode material |
| CN114883528A (en) * | 2022-06-16 | 2022-08-09 | 雅迪科技集团有限公司 | Carbon fiber negative electrode material, preparation method thereof and lithium ion battery |
| CN115058794A (en) * | 2022-06-16 | 2022-09-16 | 雅迪科技集团有限公司 | Carbon fiber material, preparation method thereof and lithium ion battery |
| CN116632233A (en) * | 2023-07-19 | 2023-08-22 | 成都锂能科技有限公司 | High-performance sodium ion battery doped hard carbon negative electrode material and preparation method thereof |
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| CN106753514A (en) * | 2016-12-27 | 2017-05-31 | 江苏大学 | A kind of method of choline eutectic solvent abstraction desulfurization |
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| CN109019590A (en) * | 2018-07-23 | 2018-12-18 | 北京林业大学 | Lignin-base multi-stage porous carbon material and preparation method thereof |
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| CN106753514A (en) * | 2016-12-27 | 2017-05-31 | 江苏大学 | A kind of method of choline eutectic solvent abstraction desulfurization |
| CN109019590A (en) * | 2018-07-23 | 2018-12-18 | 北京林业大学 | Lignin-base multi-stage porous carbon material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114604850A (en) * | 2022-03-30 | 2022-06-10 | 广东邦普循环科技有限公司 | Preparation method and application of porous microsphere carbon negative electrode material |
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| CN115058794A (en) * | 2022-06-16 | 2022-09-16 | 雅迪科技集团有限公司 | Carbon fiber material, preparation method thereof and lithium ion battery |
| CN116632233A (en) * | 2023-07-19 | 2023-08-22 | 成都锂能科技有限公司 | High-performance sodium ion battery doped hard carbon negative electrode material and preparation method thereof |
| CN116632233B (en) * | 2023-07-19 | 2023-09-29 | 成都锂能科技有限公司 | High-performance sodium ion battery doped hard carbon negative electrode material and preparation method thereof |
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