CN108172832A - A kind of graphite material of stabilization and its preparation method and application - Google Patents
A kind of graphite material of stabilization and its preparation method and application Download PDFInfo
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- CN108172832A CN108172832A CN201711409803.2A CN201711409803A CN108172832A CN 108172832 A CN108172832 A CN 108172832A CN 201711409803 A CN201711409803 A CN 201711409803A CN 108172832 A CN108172832 A CN 108172832A
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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
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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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- 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
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Abstract
The invention discloses a kind of graphite material of stabilization and its preparation method and application, which includes according to the raw material of parts by weight：35 45 parts of blocky graphite, 18 26 parts of dichloroacetic acid, 7 15 parts of ethanol amine, 13 parts of methyl acetate.Blocky graphite is crushed, seals stir process with di-chloroacetic acid solution Hybrid Heating；Then ethanolamine solutions heating sealing stirring is added in, then through filtering, washing, drying obtained mixture A；Mixture A with methyl acetate is uniformly mixed, is then calcined in protective atmosphere to obtain the final product.The present invention has good chemical property, can greatly improve electronic conductivity, can improve reversible specific capacity, charging and discharging capacity, stable cycle performance and the high rate capability of lithium ion battery；The utilization rate of blocky graphite can be improved, and effect is extremely notable, preparation process is simple, easy to operate, and graphitization calcination time shortens, and raw material sources are extensive, at low cost, is suitble to large-scale industrial production.
Description
Technical field
The present invention relates to battery technology field, graphite material of specifically a kind of stabilization and its preparation method and application.
Background technology
Compared with traditional plumbic acid, ni-Cd secondary cell, lithium ion battery have operating voltage it is high, it is higher than energy, work
The advantages that temperature range is wide, electric discharge is steady, have extended cycle life, memory-less effect, therefore it is wide as a kind of novel energy-storing power supply
It is general to be applied to the fields such as communication equipment, electric tool, aerospace.
With being constantly progressive for technology, people propose lithium ion battery higher requirement, have high-energy density, height
The lithium ion battery of the performances such as high rate performance, long circulation life, high safety factor is increasingly becoming the research hotspot of people.Stone at present
Ink is the carbon negative electrode material of lithium ion cell of main commercialization.And blocky graphite grade is very high, crystal arrangement is disorderly and unsystematic, is in
Compact massive constructs.At present, researcher has mainly carried out numerous studies to crystalline flake graphite as lithium ion battery negative material,
And blocky graphite then rarely has research, and uses negative material made from blocky graphite in the prior art, large current density is electrical
The improvement of energy is not notable, and performance is unstable, makes its application limited.
Invention content
The purpose of the present invention is to provide a kind of graphite material of stabilization and its preparation method and application, to solve the above-mentioned back of the body
The problem of being proposed in scape technology.
To achieve the above object, the present invention provides following technical solution：
A kind of graphite material of stabilization, includes according to the raw material of parts by weight：35-45 parts of blocky graphite, 18-26 parts of dichloroacetic acid,
7-15 parts of ethanol amine, 1-3 parts of methyl acetate.
As further embodiment of the present invention：The graphite material of the stabilization includes according to the raw material of parts by weight：Blocky stone
38-42 parts black, 20-24 parts of dichloroacetic acid, 9-13 parts of ethanol amine, 1.5-2.5 parts of methyl acetate.
As further embodiment of the present invention：The graphite material of the stabilization includes according to the raw material of parts by weight：Blocky stone
40 parts of ink, 22 parts of dichloroacetic acid, 11 parts of ethanol amine, 2 parts of methyl acetate.
A kind of preparation method of the graphite material of stabilization, includes the following steps：
1）4.5-5 times of deionized water of dichloroacetic acid and its quality is mixed, di-chloroacetic acid solution is made；By ethanol amine and its matter
The deionized water mixing of 3-3.5 times of amount, is made ethanolamine solutions；
2）Blocky graphite is crushed, crosses 200 mesh sieve, is then mixed with di-chloroacetic acid solution, is warming up to 150-155 DEG C and in the temperature
The lower sealing stir process 65-70min of degree, is then cooled to 88-92 DEG C and at such a temperature sealing stir process 30-35min；So
After add in ethanolamine solutions, and stir process 2.0-2.1h is sealed at a temperature of 118-120 DEG C, then through filtering, washing, drying
Mixture A is made；
3）Mixture A with methyl acetate is uniformly mixed, is then warming up in protective atmosphere, with the heating rate of 1 DEG C/min
And 4.5h is calcined at such a temperature, be then warming up to 1620 DEG C and at such a temperature in the heating rate of 0.5 DEG C/min again by 550 DEG C
It calcines 5h, be then warming up to 2850 DEG C with the heating rate of 1.5 DEG C/min and calcine 4h at such a temperature to obtain the final product.
As further embodiment of the present invention：Protective atmosphere is using one kind in helium, nitrogen, argon gas.
As further embodiment of the present invention：Step 2）In, it is 350r/ with the mixed mixing speed of di-chloroacetic acid solution
min。
As further embodiment of the present invention：Step 2）In, the mixing speed added in after ethanolamine solutions is 120r/min.
Another object of the present invention is to provide the application of the graphite material in the battery.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention is handled blocky graphite using dichloroacetic acid, ethanol amine, using graphite material made from other techniques
With good chemical property, electronic conductivity can be greatly improved, the reversible specific capacity of lithium ion battery can be improved, filled
Specific discharge capacity, stable cycle performance and high rate capability；The utilization rate of blocky graphite can be improved, and effect is extremely aobvious
It writes, preparation process is simple, easy to operate, and graphitization calcination time shortens, and raw material sources are extensive, at low cost, is suitble to extensive work
Industry metaplasia is produced, and can be applied to field of lithium ion battery as a kind of new graphite material.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of graphite material of stabilization, including following raw material：Blocky graphite 35kg, dichloroacetic acid 18kg,
Ethanol amine 7kg, methyl acetate 1kg.
4.5 times of deionized water of dichloroacetic acid and its quality is mixed, di-chloroacetic acid solution is made；By ethanol amine and its matter
The deionized water mixing of 3 times of amount, is made ethanolamine solutions.Blocky graphite is crushed, crosses 200 mesh sieve, it is then molten with dichloroacetic acid
Liquid mixes, and is warming up to 150 DEG C and at such a temperature sealing stir process 65min, is then cooled to 88 DEG C and close at such a temperature
Seal stir process 30min；Mixing speed is 350r/min.Then ethanolamine solutions are added in, and seals and stirs at a temperature of 118 DEG C
Processing 2.0h is mixed, then through filtering, washing, drying obtained mixture A；Mixing speed is 120r/min.By mixture A and acetic acid first
Ester is uniformly mixed, and is then warming up to 550 DEG C in helium protective atmosphere, with the heating rate of 1 DEG C/min and is forged at such a temperature
Burn 4.5h, be then warming up to 1620 DEG C in the heating rate of 0.5 DEG C/min again and calcine 5h at such a temperature, then with 1.5 DEG C/
The heating rate of min is warming up to 2850 DEG C and calcines 4h at such a temperature to obtain the final product.
Conductivity made from the embodiment of the present invention is from l0-6 S/cm is increased to 10-2The S/cm orders of magnitude, with 0.2C multiplying power dischargings
When reversible specific capacity be up to 366mAh/g, close to the theoretical specific capacity of graphite.With its specific capacity when 1C, 5C and 10C multiplying power discharging
Respectively 363,361 and 360mAh/g.
Embodiment 2
In the embodiment of the present invention, a kind of graphite material of stabilization, including following raw material：Blocky graphite 45kg, dichloroacetic acid 26kg,
Ethanol amine 15kg, methyl acetate 3kg.
5 times of deionized water of dichloroacetic acid and its quality is mixed, di-chloroacetic acid solution is made；By ethanol amine and its quality
3.5 times of deionized water mixing, is made ethanolamine solutions.Blocky graphite is crushed, crosses 200 mesh sieve, it is then molten with dichloroacetic acid
Liquid mixes, and is warming up to 155 DEG C and at such a temperature sealing stir process 70min, is then cooled to 92 DEG C and close at such a temperature
Seal stir process 35min；Mixing speed is 350r/min.Then ethanolamine solutions are added in, and seals and stirs at a temperature of 120 DEG C
Processing 2.1h is mixed, then through filtering, washing, drying obtained mixture A；Mixing speed is 120r/min.By mixture A and acetic acid first
Ester is uniformly mixed, and is then warming up to 550 DEG C in argon atmosphere, with the heating rate of 1 DEG C/min and is forged at such a temperature
Burn 4.5h, be then warming up to 1620 DEG C in the heating rate of 0.5 DEG C/min again and calcine 5h at such a temperature, then with 1.5 DEG C/
The heating rate of min is warming up to 2850 DEG C and calcines 4h at such a temperature to obtain the final product.
Conductivity made from the embodiment of the present invention is from l0-6 S/cm is increased to 10-2The S/cm orders of magnitude, with 0.2C multiplying power dischargings
When reversible specific capacity be up to 367mAh/g, close to the theoretical specific capacity of graphite.With its specific capacity when 1C, 5C and 10C multiplying power discharging
Respectively 365,362 and 360mAh/g.
Embodiment 3
In the embodiment of the present invention, a kind of graphite material of stabilization, including following raw material：Blocky graphite 38kg, dichloroacetic acid 20kg,
Ethanol amine 9kg, methyl acetate 1.5kg.
5 times of deionized water of dichloroacetic acid and its quality is mixed, di-chloroacetic acid solution is made；By ethanol amine and its quality
3.5 times of deionized water mixing, is made ethanolamine solutions.Blocky graphite is crushed, crosses 200 mesh sieve, it is then molten with dichloroacetic acid
Liquid mixes, and is warming up to 152 DEG C and at such a temperature sealing stir process 70min, is then cooled to 90 DEG C and close at such a temperature
Seal stir process 35min；Mixing speed is 350r/min.Then ethanolamine solutions are added in, and seals and stirs at a temperature of 119 DEG C
Processing 2.1h is mixed, then through filtering, washing, drying obtained mixture A；Mixing speed is 120r/min.By mixture A and acetic acid first
Ester is uniformly mixed, and is then warming up to 550 DEG C in nitrogen protection atmosphere, with the heating rate of 1 DEG C/min and is forged at such a temperature
Burn 4.5h, be then warming up to 1620 DEG C in the heating rate of 0.5 DEG C/min again and calcine 5h at such a temperature, then with 1.5 DEG C/
The heating rate of min is warming up to 2850 DEG C and calcines 4h at such a temperature to obtain the final product.
Conductivity made from the embodiment of the present invention is from l0-6 S/cm is increased to 10-2The S/cm orders of magnitude, with 0.2C multiplying power dischargings
When reversible specific capacity be up to 370mAh/g, close to the theoretical specific capacity of graphite.With its specific capacity when 1C, 5C and 10C multiplying power discharging
Respectively 366,365 and 365mAh/g.
Embodiment 4
In the embodiment of the present invention, a kind of graphite material of stabilization, including following raw material：Blocky graphite 42kg, dichloroacetic acid 24kg,
Ethanol amine 13kg, methyl acetate 2.5kg.
5 times of deionized water of dichloroacetic acid and its quality is mixed, di-chloroacetic acid solution is made；By ethanol amine and its quality
3.5 times of deionized water mixing, is made ethanolamine solutions.Blocky graphite is crushed, crosses 200 mesh sieve, it is then molten with dichloroacetic acid
Liquid mixes, and is warming up to 152 DEG C and at such a temperature sealing stir process 70min, is then cooled to 90 DEG C and close at such a temperature
Seal stir process 35min；Mixing speed is 350r/min.Then ethanolamine solutions are added in, and seals and stirs at a temperature of 119 DEG C
Processing 2.1h is mixed, then through filtering, washing, drying obtained mixture A；Mixing speed is 120r/min.By mixture A and acetic acid first
Ester is uniformly mixed, and is then warming up to 550 DEG C in nitrogen protection atmosphere, with the heating rate of 1 DEG C/min and is forged at such a temperature
Burn 4.5h, be then warming up to 1620 DEG C in the heating rate of 0.5 DEG C/min again and calcine 5h at such a temperature, then with 1.5 DEG C/
The heating rate of min is warming up to 2850 DEG C and calcines 4h at such a temperature to obtain the final product.
Conductivity made from the embodiment of the present invention is from l0-6 S/cm is increased to 5*10-2The S/cm orders of magnitude are put with 0.2C multiplying powers
Reversible specific capacity is up to 370mAh/g when electric, close to the theoretical specific capacity of graphite.With its specific volume when 1C, 5C and 10C multiplying power discharging
Amount is respectively 368,367 and 367mAh/g.
Embodiment 5
In the embodiment of the present invention, a kind of graphite material of stabilization, including following raw material：Blocky graphite 40kg, dichloroacetic acid 22kg,
Ethanol amine 11kg, methyl acetate 2kg.
5 times of deionized water of dichloroacetic acid and its quality is mixed, di-chloroacetic acid solution is made；By ethanol amine and its quality
3.5 times of deionized water mixing, is made ethanolamine solutions.Blocky graphite is crushed, crosses 200 mesh sieve, it is then molten with dichloroacetic acid
Liquid mixes, and is warming up to 152 DEG C and at such a temperature sealing stir process 70min, is then cooled to 90 DEG C and close at such a temperature
Seal stir process 35min；Mixing speed is 350r/min.Then ethanolamine solutions are added in, and seals and stirs at a temperature of 119 DEG C
Processing 2.1h is mixed, then through filtering, washing, drying obtained mixture A；Mixing speed is 120r/min.By mixture A and acetic acid first
Ester is uniformly mixed, and is then warming up to 550 DEG C in nitrogen protection atmosphere, with the heating rate of 1 DEG C/min and is forged at such a temperature
Burn 4.5h, be then warming up to 1620 DEG C in the heating rate of 0.5 DEG C/min again and calcine 5h at such a temperature, then with 1.5 DEG C/
The heating rate of min is warming up to 2850 DEG C and calcines 4h at such a temperature to obtain the final product.
Conductivity made from the embodiment of the present invention is from l0-6 S/cm is increased to 5*10-2The S/cm orders of magnitude are put with 0.2C multiplying powers
Reversible specific capacity is up to 371mAh/g when electric, close to the theoretical specific capacity of graphite.With its specific volume when 1C, 5C and 10C multiplying power discharging
Amount is respectively 369,368 and 368mAh/g.
Comparative example 1
In addition to dichloroacetic acid, ethanol amine is not contained, remaining raw material is consistent with embodiment 5 with technique.
Conductivity made from comparative example of the present invention is l0-6 S/cm, using reversible specific capacity during 0.2C multiplying power dischargings as
309mAh/g is respectively 307,303 and 300mAh/g with its specific capacity when 1C, 5C and 10C multiplying power discharging.
Comparative example 2
Each raw material is directly mixed, other raw materials in embodiment 5 are added in, then in nitrogen protection atmosphere, with the liter of 1 DEG C/min
Warm speed is warming up to 550 DEG C and calcines 4.5h at such a temperature, is then warming up to 1620 DEG C in the heating rate of 0.5 DEG C/min again
And 5h is calcined at such a temperature, be then warming up to 2850 DEG C with the heating rate of 1.5 DEG C/min and calcines 4h i.e. at such a temperature
.Its each raw material is consistent with the raw material and component that are used in embodiment 5.
Conductivity made from comparative example of the present invention is l0-5S/cm, using reversible specific capacity during 0.2C multiplying power dischargings as 321mAh/
G is respectively 313,307 and 305mAh/g with its specific capacity when 1C, 5C and 10C multiplying power discharging.
It is obvious to a person skilled in the art that the present invention is not limited to the details of above-mentioned exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requirement rather than above description limit, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in each embodiment can also be properly combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (8)
1. a kind of graphite material of stabilization, which is characterized in that include according to the raw material of parts by weight：35-45 parts of blocky graphite, dichloro
18-26 parts of acetic acid, 7-15 parts of ethanol amine, 1-3 parts of methyl acetate.
2. the graphite material of stabilization according to claim 1, which is characterized in that include according to the raw material of parts by weight：It is blocky
38-42 parts of graphite, 20-24 parts of dichloroacetic acid, 9-13 parts of ethanol amine, 1.5-2.5 parts of methyl acetate.
3. the graphite material of stabilization according to claim 1, which is characterized in that include according to the raw material of parts by weight：It is blocky
40 parts of graphite, 22 parts of dichloroacetic acid, 11 parts of ethanol amine, 2 parts of methyl acetate.
4. a kind of preparation method of the graphite material of stabilization as described in any one of claims 1-3, which is characterized in that including following
Step：
1）4.5-5 times of deionized water of dichloroacetic acid and its quality is mixed, di-chloroacetic acid solution is made；By ethanol amine and its matter
The deionized water mixing of 3-3.5 times of amount, is made ethanolamine solutions；
2）Blocky graphite is crushed, crosses 200 mesh sieve, is then mixed with di-chloroacetic acid solution, is warming up to 150-155 DEG C and in the temperature
The lower sealing stir process 65-70min of degree, is then cooled to 88-92 DEG C and at such a temperature sealing stir process 30-35min；So
After add in ethanolamine solutions, and stir process 2.0-2.1h is sealed at a temperature of 118-120 DEG C, then through filtering, washing, drying
Mixture A is made；
3）Mixture A with methyl acetate is uniformly mixed, is then warming up in protective atmosphere, with the heating rate of 1 DEG C/min
And 4.5h is calcined at such a temperature, be then warming up to 1620 DEG C and at such a temperature in the heating rate of 0.5 DEG C/min again by 550 DEG C
It calcines 5h, be then warming up to 2850 DEG C with the heating rate of 1.5 DEG C/min and calcine 4h at such a temperature to obtain the final product.
5. the preparation method of the graphite material of stabilization according to claim 4, which is characterized in that protective atmosphere uses helium
One kind in gas, nitrogen, argon gas.
6. the preparation method of the graphite material of stabilization according to claim 4, which is characterized in that step 2）In, with dichloro
The mixed mixing speed of acetic acid solution is 350r/min.
7. the preparation method of the graphite material of stabilization according to claim 4, which is characterized in that step 2）In, add in second
Mixing speed after alkanolamine solution is 120r/min.
8. the application of graphite material as described in any one of claims 1-3 in the battery.
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| CN201711409803.2A CN108172832A (en) | 2017-12-23 | 2017-12-23 | A kind of graphite material of stabilization and its preparation method and application |
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| CN201711409803.2A CN108172832A (en) | 2017-12-23 | 2017-12-23 | A kind of graphite material of stabilization and its preparation method and application |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013020899A (en) * | 2011-07-14 | 2013-01-31 | Asahi Glass Co Ltd | Positive electrode active material for secondary battery, positive electrode for secondary battery, and method for manufacturing secondary battery |
| CN104393298A (en) * | 2014-10-20 | 2015-03-04 | 洛阳月星新能源科技有限公司 | Blocky graphite negative electrode material for lithium ion battery, preparation method of blocky graphite negative electrode material and lithium ion battery |
| CN106654300A (en) * | 2016-12-19 | 2017-05-10 | 中国科学院山西煤炭化学研究所 | Method for preparing monodisperse metal atom/graphene composite material employing electrochemical dissolved graphite |
-
2017
- 2017-12-23 CN CN201711409803.2A patent/CN108172832A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013020899A (en) * | 2011-07-14 | 2013-01-31 | Asahi Glass Co Ltd | Positive electrode active material for secondary battery, positive electrode for secondary battery, and method for manufacturing secondary battery |
| CN104393298A (en) * | 2014-10-20 | 2015-03-04 | 洛阳月星新能源科技有限公司 | Blocky graphite negative electrode material for lithium ion battery, preparation method of blocky graphite negative electrode material and lithium ion battery |
| CN106654300A (en) * | 2016-12-19 | 2017-05-10 | 中国科学院山西煤炭化学研究所 | Method for preparing monodisperse metal atom/graphene composite material employing electrochemical dissolved graphite |
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