CN110642237A - Preparation method of carbon-coated graphite negative electrode material - Google Patents

Preparation method of carbon-coated graphite negative electrode material Download PDF

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CN110642237A
CN110642237A CN201910940368.9A CN201910940368A CN110642237A CN 110642237 A CN110642237 A CN 110642237A CN 201910940368 A CN201910940368 A CN 201910940368A CN 110642237 A CN110642237 A CN 110642237A
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carbon
graphite
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仰永军
彭飞
仰韻霖
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Guangdong Kaijin New Energy Technology Co Ltd
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
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    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a preparation method of a carbon-coated graphite cathode material, which comprises the following steps: the catalyst comprises graphite, graphene, ionic liquid, epoxy resin, polyvinylidene fluoride, ethanol, acid pickling mixed liquor, benzenediol, a catalyst and an initiator, wherein the mass percentage of each component is as follows: 15-25% of graphite, 20-30% of graphene, 15-25% of ionic liquid, 10-20% of epoxy resin, 2-4% of polyvinylidene fluoride, 10-20% of ethanol, 1-3% of acid washing mixed solution, 5-10% of styrene, 0.5-1% of catalyst and 0.5-1% of initiator; the preparation method comprises the following steps of firstly, selecting raw materials; step two, oxidizing graphite; step three, coating graphite with carbon; step four, carbonizing graphite; step five, cleaning and drying; and step six, checking and storing, the process is simple and precise, can replace other expensive carbon-coated graphite cathode material preparation processes, has an obvious effect, is cheap in raw materials and low in cost, is convenient to process, greatly saves the production cost, and is beneficial to processing and production.

Description

Preparation method of carbon-coated graphite negative electrode material
Technical Field
The invention relates to the technical field of graphite cathode materials, in particular to a preparation method of a carbon-coated graphite cathode material.
Background
The negative electrode is the lower potential end of the power supply, and in the primary battery, the electrode plays an oxidation role, and the electrode is written on the left side in the battery reaction and is the electrode from which electrons flow out in the circuit from a physical point of view. The cathode material refers to a raw material for forming a cathode in the battery, and the common cathode materials at present comprise a carbon cathode material, a tin-based cathode material and a graphite cathode; the traditional carbon-coated graphite cathode material is complex to prepare and troublesome to operate, defects and impurities on the surface of graphite cannot be eliminated during preparation, subsequent processing and production of graphite are not facilitated, graphite is singly adopted as a carbon source, the electrochemical performance of graphite cannot be remarkably improved, and the traditional carbon-coated graphite cathode material is high in raw materials and not beneficial to saving of production cost; in view of these defects, it is necessary to design a method for preparing a carbon-coated graphite negative electrode material.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon-coated graphite negative electrode material, which aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a carbon-coated graphite negative electrode material comprises the following components in percentage by weight: the catalyst comprises graphite, graphene, ionic liquid, epoxy resin, polyvinylidene fluoride, ethanol, acid pickling mixed liquor, benzenediol, a catalyst and an initiator, wherein the mass percentage of each component is as follows: 15-25% of graphite, 20-30% of graphene, 15-25% of ionic liquid, 10-20% of epoxy resin, 2-4% of polyvinylidene fluoride, 10-20% of ethanol, 1-3% of acid washing mixed liquor, 5-10% of styrene, 0.5-1% of catalyst and 0.5-1% of initiator.
A preparation method of a carbon-coated graphite cathode material comprises the following steps of selecting raw materials; step two, oxidizing graphite; step three, coating graphite with carbon; step four, carbonizing graphite; step five, cleaning and drying; step six, checking and storing;
in the first step, the components in percentage by mass are as follows: selecting 15-25% of graphite, 20-30% of graphene, 15-25% of ionic liquid, 10-20% of epoxy resin, 2-4% of polyvinylidene fluoride, 10-20% of ethanol, 1-3% of acid washing mixed liquor, 5-10% of benzenediol, 0.5-1% of catalyst and 0.5-1% of initiator, and weighing according to the weight percentage sum of 1;
in the second step, the graphite oxidation comprises the following steps:
1) cleaning a reaction kettle, adding graphite and graphene, and slowly shaking for 1-2 h;
2) adding the acid washing mixed solution into the reaction kettle, slowly stirring uniformly while adding, and raising the temperature to 30-40 ℃;
3) keeping the temperature of the material, and slowly pouring the catalyst into the reaction kettle while stirring;
4) finally, adding benzenediol, reducing the material temperature, keeping the temperature at 20-30 ℃, and sealing the reaction kettle for reaction for 1-2 hours to obtain oxidized graphite;
in the third step, the carbon-coated graphite comprises the following steps:
1) manually cleaning the reaction kettle, adding ethanol and ionic liquid, and slowly stirring for 20 min;
2) adding the graphite oxidized in the step two 4), raising the temperature of the material to 35-45 ℃, then adding epoxy resin and polyvinylidene fluoride, introducing inert gas into a stirring kettle, and reacting for 1-2 hours;
3) pouring the mixture in the reaction kettle into a stirrer, and continuously stirring for 1-4h to obtain a carbon-coated graphite prototype;
in the fourth step, the graphite carbide comprises the following steps:
1) putting the carbon-coated graphite prototype obtained in the third step into an ultrasonic machine, and drying for 20min by using the ultrasonic machine;
2) then placing the dried carbon-coated graphite prototype into a calcining furnace, heating to 600-800 ℃, calcining for 2-4h, and keeping the temperature for 1-2h after calcining is finished;
3) after the heat preservation is finished, flowing protective gas is introduced into the calcining furnace, and the temperature is reduced at room temperature to obtain carbon-coated graphite;
in the fifth step, the cleaning and drying comprises the following steps:
1) soaking the carbon-coated graphite obtained in the step four 3) in deionized water, and slowly stirring for 1-2 h;
2) taking out the soaked carbon-coated graphite, putting the carbon-coated graphite into a centrifugal machine, and performing rotary centrifugation for 1-2 hours until the surface is dried;
3) taking out the carbon-coated graphite in the centrifuge, and blowing and drying by using protective gas to obtain dry carbon-coated graphite;
and in the sixth step, the carbon-coated graphite obtained in the fifth step is subjected to surface damage and scratch inspection, then plastic packaging is carried out, and finally the carbon-coated graphite subjected to plastic packaging is subjected to box separation and integral packaging storage.
According to the technical scheme, the components are as follows by mass percent: 16% of graphite, 25% of graphene, 20% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed solution, 10% of benzenediol, 1% of catalyst and 1% of initiator.
According to the technical scheme, the pickling mixed liquid is a mixed liquid of concentrated hydrochloric acid and concentrated sulfuric acid.
According to the technical scheme, the ionic liquid is one or more of trimethylpropanediamine bistrifluoromethanesulfonimide salt, methylbutylpyrrolidine bistrifluoromethanesulfonimide salt and methylimidazolium tetrafluoroborate.
According to the technical scheme, deionized water added in the step five 1) overflows the top of the carbon-coated graphite.
According to the technical scheme, the protective gas in the step four 3) and the protective gas in the step five 3) are argon.
Compared with the prior art, the invention has the following beneficial effects: the method is safe and reliable, adopts graphite and graphene as raw materials, uses acid washing mixed liquor to oxidize the graphite, eliminates defects and impurities on the surface of the graphite, is beneficial to subsequent processing and production of the graphite, adopts epoxy resin and polyvinylidene fluoride as carbon sources, and utilizes ionic liquid to coat the carbon source on the outer side of the graphite cathode material, thereby greatly improving the electrochemical performance of the graphite and being beneficial to use of the carbon-coated graphite cathode material.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a carbon-coated graphite negative electrode material comprises the following steps:
example 1:
a carbon-coated graphite negative electrode material comprises the following components in percentage by weight: the catalyst comprises graphite, graphene, ionic liquid, epoxy resin, polyvinylidene fluoride, ethanol, acid pickling mixed liquor, benzenediol, a catalyst and an initiator, wherein the mass percentage of each component is as follows: 16% of graphite, 20% of graphene, 25% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed solution, 10% of benzenediol, 1% of catalyst and 1% of initiator.
A preparation method of a carbon-coated graphite cathode material comprises the following steps of selecting raw materials; step two, oxidizing graphite; step three, coating graphite with carbon; step four, carbonizing graphite; step five, cleaning and drying; step six, checking and storing;
in the first step, the components in percentage by mass are as follows: selecting 16% of graphite, 20% of graphene, 25% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed liquor, 10% of benzenediol, 1% of catalyst and 1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the graphite oxidation comprises the following steps:
1) cleaning a reaction kettle, adding graphite and graphene, and slowly shaking for 1-2 h;
2) adding the acid washing mixed solution into the reaction kettle, slowly stirring uniformly while adding, and raising the temperature to 30-40 ℃;
3) keeping the temperature of the material, and slowly pouring the catalyst into the reaction kettle while stirring;
4) finally, adding benzenediol, reducing the material temperature, keeping the temperature at 20-30 ℃, and sealing the reaction kettle for reaction for 1-2 hours to obtain oxidized graphite;
in the third step, the carbon-coated graphite comprises the following steps:
1) manually cleaning the reaction kettle, adding ethanol and ionic liquid, and slowly stirring for 20 min;
2) adding the graphite oxidized in the step two 4), raising the temperature of the material to 35-45 ℃, then adding epoxy resin and polyvinylidene fluoride, introducing inert gas into a stirring kettle, and reacting for 1-2 hours;
3) pouring the mixture in the reaction kettle into a stirrer, and continuously stirring for 1-4h to obtain a carbon-coated graphite prototype;
in the fourth step, the graphite carbide comprises the following steps:
1) putting the carbon-coated graphite prototype obtained in the third step into an ultrasonic machine, and drying for 20min by using the ultrasonic machine;
2) then placing the dried carbon-coated graphite prototype into a calcining furnace, heating to 600-800 ℃, calcining for 2-4h, and keeping the temperature for 1-2h after calcining is finished;
3) after the heat preservation is finished, flowing protective gas is introduced into the calcining furnace, and the temperature is reduced at room temperature to obtain carbon-coated graphite;
in the fifth step, the cleaning and drying comprises the following steps:
1) soaking the carbon-coated graphite obtained in the step four 3) in deionized water, allowing the added deionized water to overflow the top of the carbon-coated graphite, and slowly stirring for 1-2 h;
2) taking out the soaked carbon-coated graphite, putting the carbon-coated graphite into a centrifugal machine, and performing rotary centrifugation for 1-2 hours until the surface is dried;
3) taking out the carbon-coated graphite in the centrifuge, and blowing and drying by using protective gas to obtain dry carbon-coated graphite;
and in the sixth step, the carbon-coated graphite obtained in the fifth step is subjected to surface damage and scratch inspection, then plastic packaging is carried out, and finally the carbon-coated graphite subjected to plastic packaging is subjected to box separation and integral packaging storage.
Wherein the pickling mixed solution is a mixed solution of concentrated hydrochloric acid and concentrated sulfuric acid; the ionic liquid is one or more of trimethylpropanediyl bistrifluoromethanesulfonimide salt, methylbutylpyrrolidine bistrifluoromethanesulfonimide salt and methylimidazole tetrafluoroborate; the protective gas in the fourth step 3) and the protective gas in the fifth step 3) are argon.
Example 2:
a carbon-coated graphite negative electrode material comprises the following components in percentage by weight: the catalyst comprises graphite, graphene, ionic liquid, epoxy resin, polyvinylidene fluoride, ethanol, acid pickling mixed liquor, benzenediol, a catalyst and an initiator, wherein the mass percentage of each component is as follows: 16% of graphite, 25% of graphene, 20% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed solution, 10% of benzenediol, 1% of catalyst and 1% of initiator.
A preparation method of a carbon-coated graphite cathode material comprises the following steps of selecting raw materials; step two, oxidizing graphite; step three, coating graphite with carbon; step four, carbonizing graphite; step five, cleaning and drying; step six, checking and storing;
in the first step, the components in percentage by mass are as follows: selecting 16% of graphite, 25% of graphene, 20% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed liquor, 10% of benzenediol, 1% of catalyst and 1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the graphite oxidation comprises the following steps:
1) cleaning a reaction kettle, adding graphite and graphene, and slowly shaking for 1-2 h;
2) adding the acid washing mixed solution into the reaction kettle, slowly stirring uniformly while adding, and raising the temperature to 30-40 ℃;
3) keeping the temperature of the material, and slowly pouring the catalyst into the reaction kettle while stirring;
4) finally, adding benzenediol, reducing the material temperature, keeping the temperature at 20-30 ℃, and sealing the reaction kettle for reaction for 1-2 hours to obtain oxidized graphite;
in the third step, the carbon-coated graphite comprises the following steps:
1) manually cleaning the reaction kettle, adding ethanol and ionic liquid, and slowly stirring for 20 min;
2) adding the graphite oxidized in the step two 4), raising the temperature of the material to 35-45 ℃, then adding epoxy resin and polyvinylidene fluoride, introducing inert gas into a stirring kettle, and reacting for 1-2 hours;
3) pouring the mixture in the reaction kettle into a stirrer, and continuously stirring for 1-4h to obtain a carbon-coated graphite prototype;
in the fourth step, the graphite carbide comprises the following steps:
1) putting the carbon-coated graphite prototype obtained in the third step into an ultrasonic machine, and drying for 20min by using the ultrasonic machine;
2) then placing the dried carbon-coated graphite prototype into a calcining furnace, heating to 600-800 ℃, calcining for 2-4h, and keeping the temperature for 1-2h after calcining is finished;
3) after the heat preservation is finished, flowing protective gas is introduced into the calcining furnace, and the temperature is reduced at room temperature to obtain carbon-coated graphite;
in the fifth step, the cleaning and drying comprises the following steps:
1) soaking the carbon-coated graphite obtained in the step four 3) in deionized water, allowing the added deionized water to overflow the top of the carbon-coated graphite, and slowly stirring for 1-2 h;
2) taking out the soaked carbon-coated graphite, putting the carbon-coated graphite into a centrifugal machine, and performing rotary centrifugation for 1-2 hours until the surface is dried;
3) taking out the carbon-coated graphite in the centrifuge, and blowing and drying by using protective gas to obtain dry carbon-coated graphite;
and in the sixth step, the carbon-coated graphite obtained in the fifth step is subjected to surface damage and scratch inspection, then plastic packaging is carried out, and finally the carbon-coated graphite subjected to plastic packaging is subjected to box separation and integral packaging storage.
Wherein the pickling mixed solution is a mixed solution of concentrated hydrochloric acid and concentrated sulfuric acid; the ionic liquid is one or more of trimethylpropanediyl bistrifluoromethanesulfonimide salt, methylbutylpyrrolidine bistrifluoromethanesulfonimide salt and methylimidazole tetrafluoroborate; the protective gas in the fourth step 3) and the protective gas in the fifth step 3) are argon.
Example 3:
a carbon-coated graphite negative electrode material comprises the following components in percentage by weight: the catalyst comprises graphite, graphene, ionic liquid, epoxy resin, polyvinylidene fluoride, ethanol, acid pickling mixed liquor, benzenediol, a catalyst and an initiator, wherein the mass percentage of each component is as follows: 16% of graphite, 30% of graphene, 15% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed solution, 10% of benzenediol, 1% of catalyst and 1% of initiator.
A preparation method of a carbon-coated graphite cathode material comprises the following steps of selecting raw materials; step two, oxidizing graphite; step three, coating graphite with carbon; step four, carbonizing graphite; step five, cleaning and drying; step six, checking and storing;
in the first step, the components in percentage by mass are as follows: selecting 16% of graphite, 30% of graphene, 15% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed solution, 10% of benzenediol, 1% of catalyst and 1% of initiator, and weighing according to the sum of the weight percentages of 1;
in the second step, the graphite oxidation comprises the following steps:
1) cleaning a reaction kettle, adding graphite and graphene, and slowly shaking for 1-2 h;
2) adding the acid washing mixed solution into the reaction kettle, slowly stirring uniformly while adding, and raising the temperature to 30-40 ℃;
3) keeping the temperature of the material, and slowly pouring the catalyst into the reaction kettle while stirring;
4) finally, adding benzenediol, reducing the material temperature, keeping the temperature at 20-30 ℃, and sealing the reaction kettle for reaction for 1-2 hours to obtain oxidized graphite;
in the third step, the carbon-coated graphite comprises the following steps:
1) manually cleaning the reaction kettle, adding ethanol and ionic liquid, and slowly stirring for 20 min;
2) adding the graphite oxidized in the step two 4), raising the temperature of the material to 35-45 ℃, then adding epoxy resin and polyvinylidene fluoride, introducing inert gas into a stirring kettle, and reacting for 1-2 hours;
3) pouring the mixture in the reaction kettle into a stirrer, and continuously stirring for 1-4h to obtain a carbon-coated graphite prototype;
in the fourth step, the graphite carbide comprises the following steps:
1) putting the carbon-coated graphite prototype obtained in the third step into an ultrasonic machine, and drying for 20min by using the ultrasonic machine;
2) then placing the dried carbon-coated graphite prototype into a calcining furnace, heating to 600-800 ℃, calcining for 2-4h, and keeping the temperature for 1-2h after calcining is finished;
3) after the heat preservation is finished, flowing protective gas is introduced into the calcining furnace, and the temperature is reduced at room temperature to obtain carbon-coated graphite;
in the fifth step, the cleaning and drying comprises the following steps:
1) soaking the carbon-coated graphite obtained in the step four 3) in deionized water, allowing the added deionized water to overflow the top of the carbon-coated graphite, and slowly stirring for 1-2 h;
2) taking out the soaked carbon-coated graphite, putting the carbon-coated graphite into a centrifugal machine, and performing rotary centrifugation for 1-2 hours until the surface is dried;
3) taking out the carbon-coated graphite in the centrifuge, and blowing and drying by using protective gas to obtain dry carbon-coated graphite;
and in the sixth step, the carbon-coated graphite obtained in the fifth step is subjected to surface damage and scratch inspection, then plastic packaging is carried out, and finally the carbon-coated graphite subjected to plastic packaging is subjected to box separation and integral packaging storage.
Wherein the pickling mixed solution is a mixed solution of concentrated hydrochloric acid and concentrated sulfuric acid; the ionic liquid is one or more of trimethylpropanediyl bistrifluoromethanesulfonimide salt, methylbutylpyrrolidine bistrifluoromethanesulfonimide salt and methylimidazole tetrafluoroborate; the protective gas in the fourth step 3) and the protective gas in the fifth step 3) are argon.
The properties of the examples are compared in the following table:
Figure BDA0002222691890000081
based on the above, the method has the advantages that the method is safe and reliable, graphite and graphene are used as raw materials, acid washing mixed liquor is used for oxidizing the graphite and the graphene to eliminate defects and impurities on the surface of the graphite, meanwhile, epoxy resin and polyvinylidene fluoride are used as carbon sources, the carbon sources are coated on the outer side of the graphite cathode material by using ionic liquid, the electrochemical performance of the graphite is greatly improved, the method is simple and rigorous in process, the method can replace other expensive carbon-coated graphite cathode material preparation processes, the effect is obvious, the raw materials are cheap and low in cost, the processing is convenient, and the production cost is greatly saved.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A carbon-coated graphite negative electrode material is characterized in that: the formula comprises the following components: the catalyst comprises graphite, graphene, ionic liquid, epoxy resin, polyvinylidene fluoride, ethanol, acid pickling mixed liquor, benzenediol, a catalyst and an initiator, wherein the mass percentage of each component is as follows: 15-25% of graphite, 20-30% of graphene, 15-25% of ionic liquid, 10-20% of epoxy resin, 2-4% of polyvinylidene fluoride, 10-20% of ethanol, 1-3% of acid washing mixed liquor, 5-10% of styrene, 0.5-1% of catalyst and 0.5-1% of initiator.
2. A preparation method of a carbon-coated graphite cathode material comprises the following steps of selecting raw materials; step two, oxidizing graphite; step three, coating graphite with carbon; step four, carbonizing graphite; step five, cleaning and drying; step six, checking and storing; the method is characterized in that:
in the first step, the components in percentage by mass are as follows: selecting 15-25% of graphite, 20-30% of graphene, 15-25% of ionic liquid, 10-20% of epoxy resin, 2-4% of polyvinylidene fluoride, 10-20% of ethanol, 1-3% of acid washing mixed liquor, 5-10% of benzenediol, 0.5-1% of catalyst and 0.5-1% of initiator, and weighing according to the weight percentage sum of 1;
in the second step, the graphite oxidation comprises the following steps:
1) cleaning a reaction kettle, adding graphite and graphene, and slowly shaking for 1-2 h;
2) adding the acid washing mixed solution into the reaction kettle, slowly stirring uniformly while adding, and raising the temperature to 30-40 ℃;
3) keeping the temperature of the material, and slowly pouring the catalyst into the reaction kettle while stirring;
4) finally, adding benzenediol, reducing the material temperature, keeping the temperature at 20-30 ℃, and sealing the reaction kettle for reaction for 1-2 hours to obtain oxidized graphite;
in the third step, the carbon-coated graphite comprises the following steps:
1) manually cleaning the reaction kettle, adding ethanol and ionic liquid, and slowly stirring for 20 min;
2) adding the graphite oxidized in the step two 4), raising the temperature of the material to 35-45 ℃, then adding epoxy resin and polyvinylidene fluoride, introducing inert gas into a stirring kettle, and reacting for 1-2 hours;
3) pouring the mixture in the reaction kettle into a stirrer, and continuously stirring for 1-4h to obtain a carbon-coated graphite prototype;
in the fourth step, the graphite carbide comprises the following steps:
1) putting the carbon-coated graphite prototype obtained in the third step into an ultrasonic machine, and drying for 20min by using the ultrasonic machine;
2) then placing the dried carbon-coated graphite prototype into a calcining furnace, heating to 600-800 ℃, calcining for 2-4h, and keeping the temperature for 1-2h after calcining is finished;
3) after the heat preservation is finished, flowing protective gas is introduced into the calcining furnace, and the temperature is reduced at room temperature to obtain carbon-coated graphite;
in the fifth step, the cleaning and drying comprises the following steps:
1) soaking the carbon-coated graphite obtained in the step four 3) in deionized water, and slowly stirring for 1-2 h;
2) taking out the soaked carbon-coated graphite, putting the carbon-coated graphite into a centrifugal machine, and performing rotary centrifugation for 1-2 hours until the surface is dried;
3) taking out the carbon-coated graphite in the centrifuge, and blowing and drying by using protective gas to obtain dry carbon-coated graphite;
and in the sixth step, the carbon-coated graphite obtained in the fifth step is subjected to surface damage and scratch inspection, then plastic packaging is carried out, and finally the carbon-coated graphite subjected to plastic packaging is subjected to box separation and integral packaging storage.
3. The carbon-coated graphite anode material according to claim 1, characterized in that: the components are as follows by mass percent: 16% of graphite, 25% of graphene, 20% of ionic liquid, 10% of epoxy resin, 4% of polyvinylidene fluoride, 10% of ethanol, 3% of acid washing mixed solution, 10% of benzenediol, 1% of catalyst and 1% of initiator.
4. The carbon-coated graphite anode material according to claim 1, characterized in that: the pickling mixed liquid is a mixed liquid of concentrated hydrochloric acid and concentrated sulfuric acid.
5. The carbon-coated graphite anode material according to claim 1, characterized in that: the ionic liquid is one or more of trimethylpropanediamine bistrifluoromethanesulfonimide salt, methylbutylpyrrolidine bistrifluoromethanesulfonimide salt and methylimidazolium tetrafluoroborate.
6. The method for preparing the carbon-coated graphite anode material according to claim 2, wherein the method comprises the following steps: and D) enabling the deionized water added in the step five 1) to flow over the top of the carbon-coated graphite.
7. The method for preparing the carbon-coated graphite anode material according to claim 2, wherein the method comprises the following steps: and the protective gas in the fourth step 3) and the protective gas in the fifth step 3) are argon.
CN201910940368.9A 2019-09-30 2019-09-30 Preparation method of carbon-coated graphite negative electrode material Pending CN110642237A (en)

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