CN108975302A - A kind of preparation method and application of the low graphitized carbon material of asphaltic base - Google Patents
A kind of preparation method and application of the low graphitized carbon material of asphaltic base Download PDFInfo
- Publication number
- CN108975302A CN108975302A CN201810731460.XA CN201810731460A CN108975302A CN 108975302 A CN108975302 A CN 108975302A CN 201810731460 A CN201810731460 A CN 201810731460A CN 108975302 A CN108975302 A CN 108975302A
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- Prior art keywords
- coal tar
- tar pitch
- carbon material
- graphitized carbon
- asphaltic base
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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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
- C01B32/20—Graphite
- C01B32/205—Preparation
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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
-
- 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
-
- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 preparation method and applications of the low graphitized carbon material of asphaltic base, and coal tar pitch is heated to 400~430 DEG C, and after reacting 1~3h under normal pressure, 0.5~1h, the coal tar pitch melted is evaporated in vacuo;Epoxy resin is added in the coal tar pitch of melting under agitation, obtains the mixture of coal tar pitch and epoxy resin, the mass ratio of epoxy resin and coal tar pitch is 0.1~2:1;After being cooled to room temperature, mixture is crushed;Mix powder obtained is put into retort, 700~1000 DEG C are heated under inert atmosphere, obtains the low graphitized carbon material of asphaltic base after cooling.Preparation method technical process of the present invention is simple, and raw material sources are abundant, and the low graphitized carbon material of prepared asphaltic base, which is used as negative electrode of lithium ion battery, has many advantages, such as that high specific capacity, good rate capability and cycle performance are excellent.
Description
Technical field
The present invention relates to carbon material preparation technical field more particularly to a kind of preparation sides of the low graphitized carbon material of asphaltic base
Method and application.
Background technique
The development of human society is faced with many stern challenges, one of them is exactly to meet growing energy need
It asks.The mankind cause ecological problem more and more prominent the uncontrolled use of natural resources, and future will inevitably can
Source shortage problem.In order to solve this problem, it is necessary to greatly develop new energy.Leave energy storage device, renewable energy such as wind energy,
The utilization of tide energy, solar energy is all limited, therefore is of great significance to the research of energy storage material of new generation and equipment.
Lithium ion secondary battery because its energy density is high, with stable charge and discharge platform, operating temperature section is wide, puts certainly
Electric rate is low, the advantages that having extended cycle life and is environmentally friendly, becomes the primary study object in new energy field.
As the negative electrode material being commercialized earliest, graphite is current most widely used lithium ion battery negative material.But
It is to have the characteristics that interlamellar spacing is small, defective bit is few due to graphite, it is limited to lithium ion storage capacity.And low graphitized carbon has surely
Fixed structure, and have extended cycle life, intercalation potential is high, highly-safe, and there is the microstructure passed in and out for lithium ion, so
It is effective to the increase of cell output.The present invention is using coal tar pitch as raw material, after blending epoxy, prepares a kind of with excellent
The low graphitized carbon material of asphaltic base of different storage lithium performance.
Summary of the invention
The present invention provides a kind of preparation method and application of the low graphitized carbon material of asphaltic base, the preparation method technique
Process is simple, and raw material sources are abundant, and the low graphitized carbon material of prepared asphaltic base, which is used as negative electrode of lithium ion battery, has specific volume
The advantages that amount is high, good rate capability and cycle performance are excellent.
In order to achieve the above object, the present invention is implemented with the following technical solutions:
A kind of preparation method of the low graphitized carbon material of asphaltic base, comprising the following steps:
Coal tar pitch is heated to 400~430 DEG C by step 1, after reacting 1~3h under normal pressure, 0.5~1h is evaporated in vacuo, obtains
The coal tar pitch of melting;
Epoxy resin is added in the coal tar pitch of melting by step 2 under agitation, obtains coal tar pitch and epoxy resin
Mixture, the mass ratio of epoxy resin and coal tar pitch is 0.1~2:1;After being cooled to room temperature, mixture is crushed;
Mix powder made from step 2) is put into retort by step 3, it is heated to 700 under inert atmosphere~
1000 DEG C, the low graphitized carbon material of asphaltic base is obtained after cooling.
A kind of low graphitized carbon material of asphaltic base, is used as negative electrode of lithium ion battery.
Compared with prior art, the beneficial effects of the present invention are:
1) preparation method of the low graphitized carbon material of asphaltic base provided by the present invention have simple and easy, operating procedure compared with
Few feature;
2) raw materials used cheap, abundance, it is easy to accomplish large-scale production;
3) the low graphitized carbon material of asphaltic base prepared by the present invention is used as lithium ion battery negative material, shows higher
Reversible lithium storage capacity, preferable high rate performance and excellent cycle performance.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of the low graphitized carbon material of asphaltic base prepared in the embodiment of the present invention 1.
Specific embodiment
A kind of preparation method of the low graphitized carbon material of asphaltic base of the present invention, comprising the following steps:
Coal tar pitch is heated to 400~430 DEG C by step 1, after reacting 1~3h under normal pressure, 0.5~1h is evaporated in vacuo, obtains
The coal tar pitch of melting;
Epoxy resin is added in the coal tar pitch of melting by step 2 under agitation, obtains coal tar pitch and epoxy resin
Mixture, the mass ratio of epoxy resin and coal tar pitch is 0.1~2:1;After being cooled to room temperature, mixture is crushed;
Mix powder made from step 2) is put into retort by step 3, it is heated to 700 under inert atmosphere~
1000 DEG C, the low graphitized carbon material of asphaltic base is obtained after cooling.
A kind of low graphitized carbon material of asphaltic base, is used as negative electrode of lithium ion battery.
Following embodiment is implemented under the premise of the technical scheme of the present invention, gives detailed embodiment and tool
The operating process of body, but protection scope of the present invention is not limited to following embodiments.Method therefor is such as without spy in following embodiments
Not mentionleting alone bright is conventional method.
[embodiment 1]
In the present embodiment, the process for preparing the low graphitized carbon material of asphaltic base is as follows:
1) coal tar pitch that 50g softening point is 65 DEG C is heated to 400 DEG C, reacts 3h under normal pressure, 0.5h is evaporated in vacuo, obtains
To the coal tar pitch of melting;
2) 20g epoxy resin is added in the coal tar pitch of above-mentioned melting and is stirred, after mixing, is cooled to room temperature simultaneously
Mixture is crushed;
3) obtained mix powder is carbonized, is warming up to 700 under inert gas shielding in tube furnace with 5 DEG C/min
DEG C and maintain 2h, taken out after cooling, obtain the low graphitized carbon material of asphaltic base.
The stereoscan photograph of the low graphitized carbon material of prepared asphaltic base is as shown in Figure 1.
By the low graphitized carbon material of the asphaltic base being prepared and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1
Mass ratio prepare negative electrode material, collector is copper foil, and lithium ion battery is assembled in glove box.
The chemical property of assembled lithium ion battery is tested on battery test system, charging/discharging voltage range is
0.01~3V measures the low graphitized carbon material of asphaltic base in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity be
613.2mAhg-1。
[embodiment 2]
In the present embodiment, the process for preparing the low graphitized carbon material of asphaltic base is as follows:
1) coal tar pitch that 30g softening point is 65 DEG C is heated to 430 DEG C, reacts 1h under normal pressure, 1h is evaporated in vacuo, obtains
The coal tar pitch of melting;
2) 30g epoxy resin is added in the coal tar pitch of above-mentioned melting and stirs, is uniformly mixed, after being cooled to room temperature,
Mixture is crushed;
3) obtained mix powder is carbonized, is warming up to 800 under inert gas shielding in tube furnace with 3 DEG C/min
DEG C and maintain 1h, taken out after cooling, obtain the low graphitized carbon material of asphaltic base.
By the low graphitized carbon material of the asphaltic base being prepared and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1
Mass ratio prepare negative electrode material, collector is copper foil, and lithium ion battery is assembled in glove box.
The chemical property of assembled lithium ion battery is tested on battery test system, charging/discharging voltage range is
0.01~3V measures the low graphitized carbon material of asphaltic base in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity be
576.9mAhg-1。
[embodiment 3]
In the present embodiment, the process for preparing the low graphitized carbon material of asphaltic base is as follows:
1) coal tar pitch that 40g softening point is 65 DEG C is heated to 420 DEG C, reacts 3h under normal pressure, 0.5h is evaporated in vacuo, obtains
To the coal tar pitch of melting;
2) 50g epoxy resin is added in the coal tar pitch of above-mentioned melting and stirs, is uniformly mixed, after being cooled to room temperature,
Mixture is crushed;
3) obtained mix powder is carbonized, is warming up to 900 under inert gas shielding in tube furnace with 5 DEG C/min
DEG C and maintain 1h, taken out after cooling, obtain the low graphitized carbon material of asphaltic base.
By the low graphitized carbon material of the asphaltic base being prepared and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1
Mass ratio prepare negative electrode material, collector is copper foil, and lithium ion battery is assembled in glove box.
The chemical property of assembled lithium ion battery is tested on battery test system, charging/discharging voltage range is
0.01~3V measures the low graphitized carbon material of asphaltic base in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity be
524.7mAhg-1。
[embodiment 4]
In the present embodiment, the process for preparing the low graphitized carbon material of asphaltic base is as follows:
1) coal tar pitch that 60g softening point is 65 DEG C is heated to 410 DEG C, reacts 3h under normal pressure, 0.5h is evaporated in vacuo, obtains
To the coal tar pitch of melting;
2) 10g epoxy resin is added in the coal tar pitch of above-mentioned melting and stirs, is uniformly mixed, after being cooled to room temperature,
Mixture is crushed;
3) obtained mix powder is carbonized, is warming up in tube furnace under inert gas shielding with 10 DEG C/min
700 DEG C and 2h is maintained, is taken out after cooling, obtain the low graphitized carbon material of asphaltic base.
By the low graphitized carbon material of the asphaltic base being prepared and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1
Mass ratio prepare negative electrode material, collector is copper foil, and lithium ion battery is assembled in glove box.
The chemical property of assembled lithium ion battery is tested on battery test system, charging/discharging voltage range is
0.01~3V measures the low graphitized carbon material of asphaltic base in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity be
488.3mAhg-1。
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (2)
1. a kind of preparation method of the low graphitized carbon material of asphaltic base, which comprises the following steps:
Coal tar pitch is heated to 400~430 DEG C by step 1, after reacting 1~3h under normal pressure, 0.5~1h is evaporated in vacuo, is melted
Coal tar pitch;
Epoxy resin is added in the coal tar pitch of melting by step 2 under agitation, obtains the mixed of coal tar pitch and epoxy resin
Close object;The mass ratio of epoxy resin and coal tar pitch is 0.1~2:1, and after being cooled to room temperature, mixture is crushed;
Mix powder made from step 2) is put into retort by step 3, and 700~1000 DEG C are heated under inert atmosphere,
The low graphitized carbon material of asphaltic base is obtained after cooling.
2. a kind of low graphitized carbon material of asphaltic base, which is characterized in that be used as negative electrode of lithium ion battery.
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Cited By (3)
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CN111217368A (en) * | 2020-02-17 | 2020-06-02 | 中钢集团鞍山热能研究院有限公司 | Production process and device of hard carbon negative electrode material |
CN115159503A (en) * | 2022-08-19 | 2022-10-11 | 中国科学技术大学 | Preparation method and application of carbon material with adjustable degree of order |
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CN110317622A (en) * | 2019-08-08 | 2019-10-11 | 平顶山东晟高科实业有限公司 | A kind of preparation method of the dedicated high softening point bitumen of negative electrode material |
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CN115159503A (en) * | 2022-08-19 | 2022-10-11 | 中国科学技术大学 | Preparation method and application of carbon material with adjustable degree of order |
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Application publication date: 20181211 |