CN111732098A - Preparation method of asphalt-based carbon microspheres for lithium battery negative electrode material - Google Patents
Preparation method of asphalt-based carbon microspheres for lithium battery negative electrode material Download PDFInfo
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- 239000010426 asphalt Substances 0.000 title claims abstract description 98
- 239000004005 microsphere Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 12
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 12
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000005087 graphitization Methods 0.000 claims abstract description 25
- 238000003763 carbonization Methods 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 17
- 239000007800 oxidant agent Substances 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000839 emulsion Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 4
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000010309 melting process Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000003575 carbonaceous material Substances 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract description 2
- 239000003995 emulsifying agent Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Classifications
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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
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- 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
-
- 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
- H01M2004/026—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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of preparation of spherical carbon materials, and particularly relates to a preparation method of an asphalt-based carbon microsphere used as a lithium battery negative electrode material, wherein the simple preparation steps of the small-particle-size porous asphalt microsphere are as follows: the method comprises the following steps: firstly, crushing raw material asphalt, screening and grading, taking 325-500 meshes, and then placing asphalt particles in an oven at 30 ℃ for drying for later use; the invention takes the dipping asphalt as the raw material, glycerol or glycerin and surfactant as the emulsifier, reduces unnecessary addition of organic reagent, the balling of the asphalt ball is carried out in the air, the preparation method is simple and convenient, the energy consumption is low, the preparation of the green ball does not need higher temperature and high pressure reaction kettle, the ball diameter after balling is 20-40 microns, the preparation method does not need complex process equipment, does not need to modify the asphalt, can prepare the small-particle-size asphalt microsphere at lower temperature, and finally prepare the graphitized asphalt microsphere through oxidation without melting, carbonization and graphitization.
Description
Technical Field
The invention belongs to the technical field of preparation of spherical carbon materials, and particularly relates to a preparation method of an asphalt-based carbon microsphere used as a lithium battery negative electrode material.
Background
The preparation of asphalt balls by using asphalt as a raw material, and then carbonization and graphitization to obtain graphitized asphalt microspheres is one of the effective methods for high added value of asphalt at present, however, the problems of the preparation of asphalt microspheres that the preparation of raw material asphalt needs to be modified, the preparation method is complicated, the requirement for required equipment is high, and the like exist, for example, the industrial preparation method for melting and balling asphalt of the patent CN201811242596.0 needs to modify the asphalt before preparation, and needs to use balling kettle equipment to heat to a higher temperature in the preparation process of the asphalt balls, the patent CN109399632A adds the medium-low temperature asphalt and the modifier into a reaction kettle after being mixed uniformly, heats and modifies for 0.5-4h, the obtained modified asphalt particles are balling by an emulsification method, and then are oxidized without melting to be balling, the patent CN103695019A adopts a "one-step low-energy asphalt ball preparation technology", the high softening point asphalt, naphthalene, the dispersant and water are directly added into a normal pressure reaction kettle to be balling, the solid-liquid separation can be directly carried out without cooling, and the solvent removes naphthalene to obtain the asphalt ball, so that the asphalt needs to be modified or heated to a higher temperature or needs harsher equipment in the process of preparing the asphalt microsphere, the processes either prolong the time for preparing the asphalt microsphere or need multiple sets of equipment to prolong the process, further increase the production cost and inevitably produce environmental pollution.
Disclosure of Invention
To solve the problems set forth in the background art described above. The invention provides a preparation method of asphalt-based carbon microspheres for a lithium battery negative electrode material, which has the characteristics of short preparation time and simple and convenient process flow.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of asphalt-based carbon microspheres used as negative electrode materials of lithium batteries comprises the following simple preparation steps of small-particle-size asphalt microspheres:
the method comprises the following steps: firstly, crushing raw material asphalt, screening and grading, taking 325-500 meshes, and then placing asphalt particles in an oven at 30 ℃ for drying for later use;
step two: weighing a certain amount of surfactant and a certain amount of glycerol, pouring into a beaker, and stirring and mixing uniformly for later use;
step three: weighing a certain amount of asphalt particles, pouring the asphalt particles into the solution obtained in the second step, uniformly stirring, and placing the mixture into an oil bath pan;
step four: setting the final temperature of the oil bath kettle to be 110 ℃, adding a strong oxidant substance when the temperature reaches the final temperature, and continuously stirring in the air in the whole process;
step five: cooling the pelletized asphalt ball emulsion to room temperature, then centrifugally separating, washing and drying to obtain asphalt microspheres;
step six: and (3) placing the asphalt microspheres in an oven, heating the asphalt microspheres to 220-300 ℃ from room temperature for 3-4 hours for oxidation, placing the oxidized asphalt spheres in a high-temperature furnace for carbonization, and then placing the carbonized asphalt spheres in a graphitization furnace for graphitization at 3000 ℃ to obtain the graphitized asphalt microspheres.
Preferably, the balling temperature in the fourth to fifth steps is 110-: surfactant (b): glycerol/glycerin =1g/300ml, and the ratio of the asphalt to the emulsion is 5-10 g: 100 ml. The surfactant is one of sodium dodecyl benzene sulfonate or sodium dodecyl sulfate.
Preferably, in the fourth step, after adding the strong oxidant into the balled solution, continuously stirring for 2-5min, taking out the beaker, placing the beaker in cooling water, and rapidly cooling to room temperature, wherein the strong oxidant can be one or more of potassium permanganate, ozone and hypochlorous acid.
Preferably, the treatment process of non-melting, carbonization and graphitization of the asphalt microsphere in the sixth step comprises the following steps: the non-melting process comprises the following steps: raising the temperature from room temperature to 220-300 ℃ at the speed of 3-4h, wherein the carbonization process comprises the following steps: the carbonization temperature is 800-1200 ℃, the heating speed is 3-4 ℃/min, the carbonization time is 2-6h, wherein protective gas is required to be used for protection, the protective gas can be nitrogen or argon, and the graphitization process comprises the following steps: placing the mixture in a graphitization furnace for graphitization treatment at 3000 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes the dipping asphalt as the raw material, glycerol or glycerol and surfactant as the emulsifier, reduces unnecessary addition of organic reagent, the balling of the asphalt ball is directly carried out in the air, the preparation method is simple and convenient, the energy consumption is low, the preparation of the green ball does not need higher temperature and high pressure reaction kettle, the ball diameter after balling is 20-40 microns, the preparation method does not need complex process equipment, does not need to modify the asphalt, can prepare the small-particle-size asphalt microsphere at lower temperature, and finally prepare the graphitized asphalt microsphere through oxidation, infusibility, carbonization and graphitization, the preparation time is short, and the process is simple.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
The invention provides the following technical scheme: a preparation method of asphalt-based carbon microspheres used as negative electrode materials of lithium batteries comprises the following simple preparation steps of small-particle-size asphalt microspheres:
the method comprises the following steps: firstly, crushing raw material asphalt, screening and grading, taking 325-500 meshes, and then drying asphalt particles in a drying oven at 30 ℃ for later use;
step two: weighing a certain amount of surfactant and a certain amount of glycerol, pouring into a beaker, and stirring and mixing uniformly for later use;
step three: weighing a certain amount of asphalt particles, pouring the asphalt particles into a beaker of glycerol, uniformly stirring, and placing the mixture into an oil bath pan;
step four: setting the final temperature of the oil bath kettle to be 110 ℃, adding a strong oxidant substance when the temperature reaches the final temperature, and continuously stirring in the air in the whole process;
step five: cooling the pelletized asphalt ball emulsion to room temperature, then centrifugally separating, washing and drying to obtain asphalt microspheres;
step six: and (3) placing the asphalt microspheres in an oven, heating the asphalt microspheres to 220-300 ℃ from room temperature for 3-4 hours for oxidation, placing the oxidized asphalt spheres in a high-temperature furnace for carbonization, and then placing the carbonized asphalt spheres in a graphitization furnace for graphitization at 3000 ℃ to obtain the graphitized asphalt microspheres.
Specifically, the balling temperature in the fourth to fifth steps is 110-: the ratio of asphalt to the emulsion is 5-10 g: 100 ml.
Specifically, in the fourth step, after adding the strong oxidant into the balled solution, continuously stirring for 2-5min, taking out the beaker, placing the beaker in cooling water, and rapidly cooling to room temperature, wherein the strong oxidant can be one or more of potassium permanganate, ozone and hypochlorous acid.
Specifically, the treatment process of non-melting, carbonization and graphitization of the asphalt microspheres in the sixth step comprises the following steps: the non-melting process comprises the following steps: raising the temperature from room temperature to 220-300 ℃ at the speed of 3-4h, wherein the carbonization process comprises the following steps: the carbonization temperature is 800-1200 ℃, the heating speed is 3-4 ℃/min, the carbonization time is 2-6h, wherein protective gas is required to be used for protection, the protective gas can be nitrogen or argon, and the graphitization process comprises the following steps: placing the mixture in a graphitization furnace for graphitization treatment at 3000 ℃.
Example 2
The invention provides the following technical scheme: a preparation method of asphalt-based carbon microspheres used as negative electrode materials of lithium batteries comprises the following simple preparation steps of small-particle-size asphalt microspheres:
the method comprises the following steps: firstly, crushing raw material asphalt, screening and grading, taking 325-mesh and 500-mesh asphalt particles, and then placing the asphalt particles in an oven at 40 ℃ for drying treatment for 2 hours for later use;
step two: weighing 100ml of glycerol or glycerin, pouring into a beaker, weighing 1-5g of asphalt particles with 325 meshes and 400 meshes, pouring into the beaker, uniformly stirring, placing into an oil bath, and heating while stirring;
step three: setting the final temperature of an oil bath kettle to be 120 ℃, and immediately introducing cold water or adding an oxidant into the solution after the asphalt is pelletized when the asphalt is pelletized;
step four: pouring the pelletized asphalt microspheres into cold water and continuously stirring until the water temperature is reduced to room temperature, and performing suction filtration, washing and drying to obtain the asphalt microspheres;
step five: and (3) placing the asphalt microspheres in an oven, heating the asphalt microspheres to 220-300 ℃ from room temperature for 3-4 hours for oxidation, placing the oxidized asphalt spheres in a high-temperature furnace for carbonization, and then placing the carbonized asphalt spheres in a graphitization furnace for graphitization at 3000 ℃ to obtain the graphitized asphalt microspheres.
Specifically, the stirring speed in the fourth step is 300-400 r/min.
Specifically, in the third step, after the oxidizing agent is added into the balled solution, the solution needs to be continuously stirred for 2-5min, then the beaker is taken out and placed in cooling water to be rapidly cooled to room temperature, wherein the used oxidizing agent can be one or more of potassium permanganate, ozone and hypochlorous acid.
Specifically, the asphalt microspheres prepared in the fifth step are placed in an oven for 3-4h, the temperature is raised from room temperature to 220-300 ℃ for oxidation, the oxidized asphalt spheres are placed in a high-temperature furnace, the temperature is raised to 800-1200 ℃ at 3-4 ℃/min, carbonization is carried out for 2-6h, nitrogen or argon is introduced during carbonization, and the carbonized asphalt microspheres are placed in a graphitization furnace, the temperature is raised to 3000 ℃ for graphitization treatment.
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 (4)
1. A preparation method of asphalt-based carbon microspheres for a lithium battery negative electrode material is characterized by comprising the following steps of: the simple small-particle-size asphalt microsphere is prepared by the following steps:
the method comprises the following steps: firstly, crushing raw material asphalt, screening and grading, taking 325-500 meshes, and then placing asphalt particles in an oven at 30 ℃ for drying for later use;
step two: weighing a certain amount of surfactant and a certain amount of glycerol, pouring into a beaker, and stirring and mixing uniformly for later use;
step three: weighing a certain amount of asphalt particles, pouring the asphalt particles into a beaker of glycerol, uniformly stirring, and placing the mixture into an oil bath pan;
step four: setting the final temperature of the oil bath kettle to be 110 ℃, adding a strong oxidant substance when the temperature reaches the final temperature, and continuously stirring in the air in the whole process;
step five: cooling the pelletized asphalt ball emulsion to room temperature, then centrifugally separating, washing and drying to obtain asphalt microspheres;
step six: and (3) placing the asphalt microspheres in an oven, heating the asphalt microspheres to 220-300 ℃ from room temperature for 3-4 hours for oxidation, placing the oxidized asphalt spheres in a high-temperature furnace for carbonization, and then placing the carbonized asphalt spheres in a graphitization furnace for graphitization at 3000 ℃ to obtain the graphitized asphalt microspheres.
2. The preparation method of the pitch-based carbon microsphere as the negative electrode material of the lithium battery, according to claim 1, is characterized in that: the balling temperature in the fourth to fifth steps is 110-120 ℃, the stirring speed is 300-400r/min, and the mixture ratio of the emulsion is as follows: the ratio of asphalt to the emulsion is 5-10 g: 100 ml.
3. The preparation method of the pitch-based carbon microsphere as the negative electrode material of the lithium battery, according to claim 1, is characterized in that: and in the fourth step, adding a strong oxidant into the balled solution, continuously stirring for 2-5min, taking out the beaker, placing the beaker in cooling water, and quickly cooling to room temperature, wherein the strong oxidant can be one or more of potassium permanganate, ozone and hypochlorous acid.
4. The preparation method of the pitch-based carbon microsphere as the negative electrode material of the lithium battery, according to claim 1, is characterized in that: the treatment process of non-melting, carbonization and graphitization of the asphalt microspheres in the sixth step comprises the following steps: the non-melting process comprises the following steps: raising the temperature from room temperature to 220-300 ℃ at the speed of 3-4h, wherein the carbonization process comprises the following steps: the carbonization temperature is 800-1200 ℃, the heating speed is 3-4 ℃/min, the carbonization time is 2-6h, wherein protective gas is required to be used for protection, the protective gas can be nitrogen or argon, and the graphitization process comprises the following steps: placing the mixture in a graphitization furnace for graphitization treatment at 3000 ℃.
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